fall issue 2012 news/cadnews_2012_3__… · colors, there is a noticeable crispness in the air, the...
TRANSCRIPT
Chairmanrsquo s message
Welcome to the Fall edition of your CAD News newsletter published byJamie Przybylski As I sit here writing this message the leaves are changingcolors there is a noticeable crispness in the air the World Series is on TV andit is a reminder that summer has ended It is also the time of year when we gettogether in some city conduct our annual CAD RETECreg technical confer-ence This year was quite special because we celebrated our 50th anniversaryand that is quite special
Congratulations to Sandra Davis and her committee for organizing this very special RETECreg inLouisville KY The conference was a tremendous success with approximately 480 attendeeswhich makes it one of the best-attended conferences in our 50 year history The conference wasanchored by a strong technical program an interesting panel discussion and it featured over 60tabletop exhibitors and plenty of professional and social interactions The conference organizersread the surveys that you fill out and submit and they try and listen to you and this is evident inthe cities that are chosen the length and format of the conference and some of both the traditionaland new features of the RETECreg Finally I want to say thank you to everyone who attended andfinancially supported the conference The proceeds from our RETECreg support scholarships and
continuing education for the professionals in ourindustry We are insuring the future success ofour industry by developing the people who willlead the next generation of color scientists
Our next technical forum will be at theANTECreg in Cincinnati Ohio on April 22-24Scott Heitzman is chairing this event and he isbusy putting together a full palette of technicalpapers for you Please visit specadorg for moreinformation and you can find a link to register toattend as well
Our group continues to grow and evolve andthere are a couple of changes Id like to sharewith you First George Rangos has taken overthe Endowment Committee from JohnnySuthers George has served on the board forquite a long time and he has served in virtuallyevery capacity including the five year rotationthroughout the chair positions He is very capa-ble of managing this very important function ofour Division We would like to thank Johnny forhis years of leadership during which time he notonly managed the funds but he worked directly
continued on page 2
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fall issue
20122012
Table of ConTenTs
CliCk on arTiCle or page number
To go To page
Chairmanrsquos Message 12Mission Statement 2BOD Election Nominee Request 2Sponsorships 3Councilorrsquos Report 4Minutes of Board Link 4Sponsorships 5Color Mischief 7 6RETECreg 2012 Wrap-up 7Invitation to Attend our Board Meetings 7Scholarship Endowment Program 8Your Company Our Division 8Call for Papers RETECreg2013 9Social Media- LinkedIn 9Plastic Courses at Terra Community College 10Sponsorships 11Technical Article 12-19Sponsorships 15CAD BOD Directors Listing 20Other Contact Info 20
with the students that CAD was nurturing Secondly Id like to welcome Mark Freshwater as the newest member toyour Board of Directors Mark received the highest number of votes in the spring election and he will fill an openingthat was created recently We look forward to working with Mark and we are confident that he will bring new energyand ideas to the CAD
Please check the website often and look for emails from SPE about ongoing events in general I look forward to seeingeveryone in Cincinnati in April
Best Regards
Jim FiganiakCAD Chairperson
Chairmanrsquo s message - ConTinued
SPE CAD NEWS Fall 2012 page 2 wwwspecadorg
DisclaimerThe information submitted in this publication is based on current knowledge and experience In view of the many factors that may affect processibil-ity and application this datainformation does not relieve processors from the responsibility of carrying out their own tests and experiments neitherdo they imply any legally binding assurance of certain properties or of suitability for a specific purpose It is the responsibility of those to whom thisinformation is supplied to ensure that any proprietary rights and existing laws and legislation are observed
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spe Color amp appearanCe division
mission sTaTemenT
The Color and Appearance Division of SPE
strives to educate train inform and to pro-
vide professional interaction opportunities
to the global community involved in visual
performance and aesthetics of plastics
annual board eleCTions
of Color amp appearanCe
divisionDeadline for Nomination Submissions
December 15 2012
The Color amp Appearance Division of the SPE will beconducting its annual board elections in February 2013The election is open to SPE members with CAD astheir primary division Time commitment is four meet-ings per year including those held at ANTECreg andRETECreg and participation in CAD activities and ini-tiatives If you are interested or would like to nominatea colleague please contact Ann Smeltzer at the notedemail address or phone before December 15th Nominate a Colleague by emailing Ann Smeltzer atannsmeltzerclariantcom or calling 412-298-4373
Submit you nomination now
ech haintL and PsrrsoloCou Y
he tsech hastgmeni and P
Needou
cetLinwww
Ad
tcatnCo Ch336
moclanoitanretnIh
stgmeniPampvesitidAd
nruChselraCh336-255-6673 nLinruChselraCh
moclanoitanretnIhcetn
HIGH PERFORMANCE COLORS FOR PLASTICS
Prompt deliveries from our warehouses across the county
Organic PigmentsPearlescent PigmentsFluorescent DyesSolvent amp Disperse Dyes for Plastics
SPECTRA DYESTUFFS INC363-E Cliffwood Park St
Brea CA 92821P 714-990-4300F 714-990-4302
wwwspectradyescom
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Pigments and Additives for the Plastics Industry
Clariant Corporation4000 Monroe Road Charlotte NC 28205Phone 8004414414wwwclariantcom
Leading Manufacturer of Complex Inorganic Color Pigments (CICP) bull Pigment Brown 24 Yellow 53 Blue 28 Green 50 Black 28 etcbull Environmentally Friendly Pigments Brown 48 etcbull Laser Marking Pigmentsbull Pigments for Biodegradable Plastics
Contact in Americas
73 Cavalier Blvd Suite 207 Florence KY 41042TEL (859) 746-0407 FAX (859) 746-0467tomatecamtomateccomWWWToMaTeCCoM
HIGH PERFORMANCE PIGMENTS FOR PLASTICS
Ferros Geodereg Complex Inorganic Color Pigments offer unsurpassed color quality and stability
The complete Geodereg line includes
Chrome Titanates l Cobalt Blues amp Greens l Nickel Titanates
Heat stable Blacks l Iron Free Browns l IR Reflecting Blacks
Ferro Corporation Performance Pigments amp Colors
251 West Wylie Avenue PO Box 519
Washington PA 15301
Phone 724-223-5900
Fax 724 223-2700 wwwferrocom
wwwshepherdcolorcom
Lintech has theColors and Pigments
You Need
SPE CAD NEWS Fall 2012 page 3 wwwspecadorg
The Color and Appearance Division (CAD) commits to the pub-lishing of at least three newsletters a year (four if there is sufficientmaterial to justify the extra issue) Each newsletter is electronical-ly distributed to our membership of nearly 1000) Each sponsorrsquosart directly links to the companyrsquos website
In addition we print one of these newsletters on 80gloss coatedstock All electronic versions are also posted on the SPE websitewhere it available for anyone to download
For the small donation of $300 per year we offer a business cardsized (2 x 35 inches) mention in our newsletter
We currently have the following slots available for sponsorship
(2) 2 x 35 inch or (1) 4 x 35 inch
If interested in learning more please contact
SHARYL REID Phone 8649682426
Email Sharyl_Reidusaschulmancom
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SPE CAD NEWS Fall 2012 page 4 wwwspecadorg
CounCilorrsquo s reporT
The Fall Council meeting was held on September 15 2012 in Dearborn MI The day before the Councilmeeting there were various committee meetings including Divisions Committee and ConferenceOversight Committee The Fall meeting is the election meeting at which time the next leaders of SPEare selected by the Councilors
MEMBERSHIP While membership has shown slow growth over the past couple years in the first halfof 2012 there has been 2 decrease in membership This has been attributed to reduced retention rates
and the scheduling of ANTECreg It is felt that the retention rates have been negatively impacted due to the difficulties asso-ciated with membership renewal using the website which are directly related to the management software being used bythe organization The scheduling of ANTECreg adversely impacted membership numbers because there were less than 12months between ANTECreg 2011 and ANTECreg 2012 therefore members who joined in order to attend ANTECreg 2011 atthe member rate were able to register for ANTECreg 2012 as a member without renewing their membership
FINANCIAL Despite budgeting more tightly for 2012 than 2011 the mid-year financial review has shown a $52000shortfall The second half is typically lower in revenue for the organization so there is little expectation of making up thisshortfall Additionally the impact of ANTECreg Mumbai is unknown The worst case scenario has a year-end shortfall of$350000 for the organization A revised budget is being prepared to minimize the shortfall
ELECTION Vijay Boolani was elected by the Councilors as the President-Elect Additionally Raed Al-Zubiwas elected as Senior Vice-President and Dick Cameron was elected Vice-President
Sincerely
Sandra DavisCAD Councilor
ediTorrsquo s noTe
Hopefully many of you had a chance to attend the past CAD RETECreg in Louisville this fall Itwas a historic event the 50th anniversary conference conducted by the Color and AppearanceDivision of the SPE Sandra Davis and her team should be commended for making it success-ful and memorable One thing that made it memorable for me was the attendance of one specialperson Robert Charvat Not only has Bob been a good friend and mentor to many of us on theboard he has the distinction of being one of the founding members of the CAD and not onlyattended the very first conference but also helped finance it Bob was recognized at the awardsreception and given a plaque listing all of the conferences to commemorate his involvement
throughout the years I have included a picture of Bob and his plaque Bob is no longer a board member but hestays involved and is always in our hearts One other thing I would like to mention is that I am the professor in TerraState Community Collegersquos Coloring of Plastics program which Bob was also instrumental in starting and nurturingFor those of you that might have not seen it in Plastics News in August there was a nice article about our programAs always I ask you to spread the word about Terra to your colleagues and contacts that may be in the need of colortraining If you have not had a chance to see the article click here to the linkHave a save and happy Holiday season
Jamie PrzybylskiCAD Editor
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Organic Pigments Inorganic Pigments
Pigment Preparations
Heucotech Ltd 99 Newbold Road Fairless Hills PA 19030
wwwheubachcolorcom 215-736-0712
Organic amp InorganicPigments and Preparations
(416) 253-4297 hkennedydominioncolourcomwwwdominioncolourcom
DOM 653 ProgramAd_retec09_v2_ 72209 217 PM Page 1
Quality Formulation oF
Color amp additive ConCentrates
wwwtechmerpmcom
18420 laurel Park road 1 Quality Circle
rancho dominguez Ca 90220 Clinton Tn 37716
(310) 632-9211
(865) 457-6700
ISHIHARA CORPORATION (USA)l TiO2 l Ultra-fine TiO2
l Nickel Titanates l Chrome Titanatesl Conductive Pigments
600 Montgomery Street Tel (415) 421shy8207
San Francisco California 94111 Fax (415) 397shy5403wwwishiharacom
page 5
SPE CAD NEWS Fall 2012 page 5 wwwspecadorg
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SPE CAD NEWS Fall 2012 page 6 wwwspecadorg
Color misChief 7Can sTorage of samples or sTandards
be a problem
The answer to the title question is ldquoOh my yes it canrdquo
Many organizations store their standards and samples in more ways thananyone wants to take the time to even think about And Many of them arejust plain wrong
However there is one storage method at the top of the list that defies any reasonable technical justification What is thatawful procedure Storing the standards or samples measurement data in a computer memory Then believe it or notusing that canned data for subsequent virtual judgments for things like quality control of production batches and other vitalissues In all coloring of plastics adventures one must try to reduce or eliminate as many variables as are known Or at leastreduce them to manageable values that can be compensated for Itrsquos the unknown variables that doom projects to failure
Now letrsquos address the chief subject of this article The total objective of standard and sample storage is to protect the piecesfrom any environment that might repeat might alter their visual and or measurement stability There are a number of caseswhere this problem occurs and is totally unknown to the participants These are the killers
Did you know the procedure used to cool a sample from a process such as injection molding as an example can affect itslong term color stability This can occur before andor during long term storage The environmental conditions of the stor-age environment can affect long term color stability
If the surface of the stored sample is not completely protected from scratches smudges and or other defacements the sample is no longer valid for visual andor measurement evaluations
A many laboratories store standards and samples in freezers This is OK so far But many do not temperature stabilize thesample before an evaluation This will bias any subsequent testing This includes removing any surface moisture that maydevelop as a sample warms to room temperature
One of the most insidious problems that many times go un-noticed is the wrapping or protection given samples as they gointo storage One very convenient method used by numerous operations is to put the sample in a manila folder then put thesample containing folder into a file drawer cabinet where the cabinet environment is not considered This may not be agood idea Is the folder used pH neutral The composition of folders andor papers can be highly acidic or alkaline Eithervariety may affect the stability of the standards andor samples stored in these papers The last one for this message is thatmany manila folders contain some form of sulfur in the paper Does any reader remember sulfide staining of polymers andtheir additives Maybe this is affecting your samples
This and many other possibilities may lead to changes in samples during storage The major puzzle for storage is be sureyou know and understand the storage parameters If the parameters are not understood stored samples may not be stableduring the storage cycle
Enough for this mischief for now As usual the guilty shall remain anonymous to protect them Look for the next ColorMischief 8 article soon
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SPE CAD NEWS Fall 2012 page 7 wwwspecadorg
The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry
In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly
The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)
Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years
reTeCreg 2012 Wrap-up
inviTaTion To aTTend our Cad board
meeTings
The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg
The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg
Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
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aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
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courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
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Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
DuPonttrade TishyPurereg titanium dioxide
duPont titanium technologies8004419485
wwwtitaniumdupontcom
The DuPont Oval DuPont trade The miracles of sciencereg and TishyPurereg
are trademarks or registered trademarks of EI du Pont de Nemours and Company
PoLYmers Light amp sCieNCe
Polymers Light and the Science of TiO2
Color Concentrates and
single Pigment dispersions
for all Thermoplastic Polymers
A World of Color Perfection since 1964
Corporate Offices
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Operations amp
Research Center
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(215) 997-2221
wwwpenncolorcom
BTitanium dioxide
Brutile amp anatase
Bhigh Performance organic Pigments
B dPP reds hP yellowsB PvC additives
B lubricants amp stabilizers
364 Johnny Mercer blvd b-7 294 - savannah ga 31410
Tel (912)507-8972 - lwaltersagrofertinccom
wwwagrofertinccom
World leader in effect
Pigments
one international Plazasuite 300Philadelphia Pa 19113(888) 367-3275
wwwemdchemicalscom
A Complete Line of DyestuffsInorganic Pigments and
Organic Pigments forPlastics amp Fibers
lanXeSS corporation
111 rIDc Park west Drive 1-800-526-9377
Pittsburgh Pa 15275-1112 wwwlanxesscom
World Leaders in Ultramarine Pigmentswultramarine blue wultramarine violet
wChrome oxide green wlead Chromate
wZinc ferrite wiron oxide
Phone 770-338-4990
6369 Peachtree street fax 770-338-8315
norcross ga 30071 Toll free 886-682-4652wwwnubiolacom
We create chemistry for plastics
effect and functional pigments
eate chemistry for plastics
basfcomplastic-additiveswww
your plastic applicationsovide solutions for all ofand other additives pr
tnadixoitnasrezilibatsthgilVUruOfect and functional pigments efneeds with colorneeds with color ef
nufdnaelytsruoyteemsplehFSAASB
e crWWe cr
eate chemistry for plastics
1 800 431-2360 NJarkFlorham P
100 Campus DrivetionBASF Corpora
ovide solutions for all ofs rotaelcunst
fect and functional pigmentsy tilanoitcn
Color Software Experts
Since 1986
Quality Control Formulation
amp Instrument Profiling
Visit our website and color blog
wwwcyberchromeusacom
CyberChrome Inc
3642 Main Street tStone Ridge NY 12484
PH 845shy687shy26718601 DunwooDy Place Blg 334 atlanta ga uSa 30350
7709935500 wwwcolorchemcom
AMAPLASTreg DYES
IR ABSORBERS
NEOLORTM PIGMENTS
UVAPLASTTM UV ABSORBERS
SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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Clariant Corporation
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Finance Chair
Betty Puckerin 812shy466shy9828
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Bettypuckerinxxxampacetcom
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Councilor
Sandra Davis 302shy999shy2540
DuPont
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Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
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Steve Esker 614shy679shy4677
Paramount Colors Inc
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Mark Freshwater
Lansco Colors
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Clariant Corp
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ComAssist
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DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
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SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
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AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
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Frank Lavieri 401shy461shy4100
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EMD Chemicals
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Doreen Becker 914shy772shy5580
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Uniform Color
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Tronox LLC
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BASF Corporation
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Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
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608shy246shy2600
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OTHER USEFUL CONTACTS
with the students that CAD was nurturing Secondly Id like to welcome Mark Freshwater as the newest member toyour Board of Directors Mark received the highest number of votes in the spring election and he will fill an openingthat was created recently We look forward to working with Mark and we are confident that he will bring new energyand ideas to the CAD
Please check the website often and look for emails from SPE about ongoing events in general I look forward to seeingeveryone in Cincinnati in April
Best Regards
Jim FiganiakCAD Chairperson
Chairmanrsquo s message - ConTinued
SPE CAD NEWS Fall 2012 page 2 wwwspecadorg
DisclaimerThe information submitted in this publication is based on current knowledge and experience In view of the many factors that may affect processibil-ity and application this datainformation does not relieve processors from the responsibility of carrying out their own tests and experiments neitherdo they imply any legally binding assurance of certain properties or of suitability for a specific purpose It is the responsibility of those to whom thisinformation is supplied to ensure that any proprietary rights and existing laws and legislation are observed
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spe Color amp appearanCe division
mission sTaTemenT
The Color and Appearance Division of SPE
strives to educate train inform and to pro-
vide professional interaction opportunities
to the global community involved in visual
performance and aesthetics of plastics
annual board eleCTions
of Color amp appearanCe
divisionDeadline for Nomination Submissions
December 15 2012
The Color amp Appearance Division of the SPE will beconducting its annual board elections in February 2013The election is open to SPE members with CAD astheir primary division Time commitment is four meet-ings per year including those held at ANTECreg andRETECreg and participation in CAD activities and ini-tiatives If you are interested or would like to nominatea colleague please contact Ann Smeltzer at the notedemail address or phone before December 15th Nominate a Colleague by emailing Ann Smeltzer atannsmeltzerclariantcom or calling 412-298-4373
Submit you nomination now
ech haintL and PsrrsoloCou Y
he tsech hastgmeni and P
Needou
cetLinwww
Ad
tcatnCo Ch336
moclanoitanretnIh
stgmeniPampvesitidAd
nruChselraCh336-255-6673 nLinruChselraCh
moclanoitanretnIhcetn
HIGH PERFORMANCE COLORS FOR PLASTICS
Prompt deliveries from our warehouses across the county
Organic PigmentsPearlescent PigmentsFluorescent DyesSolvent amp Disperse Dyes for Plastics
SPECTRA DYESTUFFS INC363-E Cliffwood Park St
Brea CA 92821P 714-990-4300F 714-990-4302
wwwspectradyescom
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Pigments and Additives for the Plastics Industry
Clariant Corporation4000 Monroe Road Charlotte NC 28205Phone 8004414414wwwclariantcom
Leading Manufacturer of Complex Inorganic Color Pigments (CICP) bull Pigment Brown 24 Yellow 53 Blue 28 Green 50 Black 28 etcbull Environmentally Friendly Pigments Brown 48 etcbull Laser Marking Pigmentsbull Pigments for Biodegradable Plastics
Contact in Americas
73 Cavalier Blvd Suite 207 Florence KY 41042TEL (859) 746-0407 FAX (859) 746-0467tomatecamtomateccomWWWToMaTeCCoM
HIGH PERFORMANCE PIGMENTS FOR PLASTICS
Ferros Geodereg Complex Inorganic Color Pigments offer unsurpassed color quality and stability
The complete Geodereg line includes
Chrome Titanates l Cobalt Blues amp Greens l Nickel Titanates
Heat stable Blacks l Iron Free Browns l IR Reflecting Blacks
Ferro Corporation Performance Pigments amp Colors
251 West Wylie Avenue PO Box 519
Washington PA 15301
Phone 724-223-5900
Fax 724 223-2700 wwwferrocom
wwwshepherdcolorcom
Lintech has theColors and Pigments
You Need
SPE CAD NEWS Fall 2012 page 3 wwwspecadorg
The Color and Appearance Division (CAD) commits to the pub-lishing of at least three newsletters a year (four if there is sufficientmaterial to justify the extra issue) Each newsletter is electronical-ly distributed to our membership of nearly 1000) Each sponsorrsquosart directly links to the companyrsquos website
In addition we print one of these newsletters on 80gloss coatedstock All electronic versions are also posted on the SPE websitewhere it available for anyone to download
For the small donation of $300 per year we offer a business cardsized (2 x 35 inches) mention in our newsletter
We currently have the following slots available for sponsorship
(2) 2 x 35 inch or (1) 4 x 35 inch
If interested in learning more please contact
SHARYL REID Phone 8649682426
Email Sharyl_Reidusaschulmancom
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SPE CAD NEWS Fall 2012 page 4 wwwspecadorg
CounCilorrsquo s reporT
The Fall Council meeting was held on September 15 2012 in Dearborn MI The day before the Councilmeeting there were various committee meetings including Divisions Committee and ConferenceOversight Committee The Fall meeting is the election meeting at which time the next leaders of SPEare selected by the Councilors
MEMBERSHIP While membership has shown slow growth over the past couple years in the first halfof 2012 there has been 2 decrease in membership This has been attributed to reduced retention rates
and the scheduling of ANTECreg It is felt that the retention rates have been negatively impacted due to the difficulties asso-ciated with membership renewal using the website which are directly related to the management software being used bythe organization The scheduling of ANTECreg adversely impacted membership numbers because there were less than 12months between ANTECreg 2011 and ANTECreg 2012 therefore members who joined in order to attend ANTECreg 2011 atthe member rate were able to register for ANTECreg 2012 as a member without renewing their membership
FINANCIAL Despite budgeting more tightly for 2012 than 2011 the mid-year financial review has shown a $52000shortfall The second half is typically lower in revenue for the organization so there is little expectation of making up thisshortfall Additionally the impact of ANTECreg Mumbai is unknown The worst case scenario has a year-end shortfall of$350000 for the organization A revised budget is being prepared to minimize the shortfall
ELECTION Vijay Boolani was elected by the Councilors as the President-Elect Additionally Raed Al-Zubiwas elected as Senior Vice-President and Dick Cameron was elected Vice-President
Sincerely
Sandra DavisCAD Councilor
ediTorrsquo s noTe
Hopefully many of you had a chance to attend the past CAD RETECreg in Louisville this fall Itwas a historic event the 50th anniversary conference conducted by the Color and AppearanceDivision of the SPE Sandra Davis and her team should be commended for making it success-ful and memorable One thing that made it memorable for me was the attendance of one specialperson Robert Charvat Not only has Bob been a good friend and mentor to many of us on theboard he has the distinction of being one of the founding members of the CAD and not onlyattended the very first conference but also helped finance it Bob was recognized at the awardsreception and given a plaque listing all of the conferences to commemorate his involvement
throughout the years I have included a picture of Bob and his plaque Bob is no longer a board member but hestays involved and is always in our hearts One other thing I would like to mention is that I am the professor in TerraState Community Collegersquos Coloring of Plastics program which Bob was also instrumental in starting and nurturingFor those of you that might have not seen it in Plastics News in August there was a nice article about our programAs always I ask you to spread the word about Terra to your colleagues and contacts that may be in the need of colortraining If you have not had a chance to see the article click here to the linkHave a save and happy Holiday season
Jamie PrzybylskiCAD Editor
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Organic Pigments Inorganic Pigments
Pigment Preparations
Heucotech Ltd 99 Newbold Road Fairless Hills PA 19030
wwwheubachcolorcom 215-736-0712
Organic amp InorganicPigments and Preparations
(416) 253-4297 hkennedydominioncolourcomwwwdominioncolourcom
DOM 653 ProgramAd_retec09_v2_ 72209 217 PM Page 1
Quality Formulation oF
Color amp additive ConCentrates
wwwtechmerpmcom
18420 laurel Park road 1 Quality Circle
rancho dominguez Ca 90220 Clinton Tn 37716
(310) 632-9211
(865) 457-6700
ISHIHARA CORPORATION (USA)l TiO2 l Ultra-fine TiO2
l Nickel Titanates l Chrome Titanatesl Conductive Pigments
600 Montgomery Street Tel (415) 421shy8207
San Francisco California 94111 Fax (415) 397shy5403wwwishiharacom
page 5
SPE CAD NEWS Fall 2012 page 5 wwwspecadorg
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SPE CAD NEWS Fall 2012 page 6 wwwspecadorg
Color misChief 7Can sTorage of samples or sTandards
be a problem
The answer to the title question is ldquoOh my yes it canrdquo
Many organizations store their standards and samples in more ways thananyone wants to take the time to even think about And Many of them arejust plain wrong
However there is one storage method at the top of the list that defies any reasonable technical justification What is thatawful procedure Storing the standards or samples measurement data in a computer memory Then believe it or notusing that canned data for subsequent virtual judgments for things like quality control of production batches and other vitalissues In all coloring of plastics adventures one must try to reduce or eliminate as many variables as are known Or at leastreduce them to manageable values that can be compensated for Itrsquos the unknown variables that doom projects to failure
Now letrsquos address the chief subject of this article The total objective of standard and sample storage is to protect the piecesfrom any environment that might repeat might alter their visual and or measurement stability There are a number of caseswhere this problem occurs and is totally unknown to the participants These are the killers
Did you know the procedure used to cool a sample from a process such as injection molding as an example can affect itslong term color stability This can occur before andor during long term storage The environmental conditions of the stor-age environment can affect long term color stability
If the surface of the stored sample is not completely protected from scratches smudges and or other defacements the sample is no longer valid for visual andor measurement evaluations
A many laboratories store standards and samples in freezers This is OK so far But many do not temperature stabilize thesample before an evaluation This will bias any subsequent testing This includes removing any surface moisture that maydevelop as a sample warms to room temperature
One of the most insidious problems that many times go un-noticed is the wrapping or protection given samples as they gointo storage One very convenient method used by numerous operations is to put the sample in a manila folder then put thesample containing folder into a file drawer cabinet where the cabinet environment is not considered This may not be agood idea Is the folder used pH neutral The composition of folders andor papers can be highly acidic or alkaline Eithervariety may affect the stability of the standards andor samples stored in these papers The last one for this message is thatmany manila folders contain some form of sulfur in the paper Does any reader remember sulfide staining of polymers andtheir additives Maybe this is affecting your samples
This and many other possibilities may lead to changes in samples during storage The major puzzle for storage is be sureyou know and understand the storage parameters If the parameters are not understood stored samples may not be stableduring the storage cycle
Enough for this mischief for now As usual the guilty shall remain anonymous to protect them Look for the next ColorMischief 8 article soon
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SPE CAD NEWS Fall 2012 page 7 wwwspecadorg
The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry
In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly
The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)
Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years
reTeCreg 2012 Wrap-up
inviTaTion To aTTend our Cad board
meeTings
The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg
The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg
Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesra plastics program is
LC
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EHHECSRUUROOUYYO
DNND
AAAN
UOY
EELLEUULDDUEED
y is this internet based three course cerindustr or undererer or undery of the newman
One aspect of Tspeak ofspeak of One aspect of T new hires etc) that havff new hires etc) that havsales staf
e all know people within the industrWWe all know people within the industr
earseral yseved students globallvy sersuccessfull
classroom activities This distance learning program hasOhio campus to parto students who may reside too f
tificatey is this internet based three course cer-educated members of our or under
s program that can benefitrarsquorarsquos program that can benefiter One aspect of T One aspect of Tere no color education to new hires etc) that hav
y (technicianse all know people within the industr
ell as locall as wyy as wed students globallclassroom activities This distance learning program has
eningticipate in full time day or evOhio campus to parremontar from the Fto students who may reside too fto students who may reside too far from the F
Section VLDistance Learning Courses Offer
4195592459at or more infF
tificate-educated members of our
s program that can benefite no color education to
y (technicians
or fyy fell as locallclassroom activities This distance learning program has
eningremont
Section VLDistance Learning Courses Offer
aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
aeduxt 2459TERRA e
essoram Profam Professorrram ProfProg ylski
courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
The threeyy The threesegments of the coloring of plastics industrorking in the manone wyor ane fbackground knowledg
on their schedule The three courses provide solidywhereee can complete anyprogram that the emplo
xibleel fley low cost no travelprogram It is a relativ
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
ered Spring 2013 (JfOfall 2012 (Aered FfOf
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Section VL
The threeyorking in the man
on their schedule The three courses provide solidywhere
xible
y 14mdashDecember 14)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
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y 14ndashMay 9)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14mdashDecember 14)ugust 20mdashDecember 14)
e-stat-state)stiderC3(
y 14ndashMay 9)ugust 20mdashDecember 14)
e-stat-state(3 Credits)
of plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
cellent opporxCourses are an e
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er coloror newtunity fcellent oppor
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VL Section
or people withtechnicians and others to learn more about the coloringmatchers quality control technicians production
er color
y 14mdashMay 9)anuarered Spring 2013 (Jy $150ximatelBooks appro
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y 14mdashMay 9)
e-stat-state(4 Credits)
tificate can ecompleting this cery behind what they do evthe theor
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or them to learntunity food opporon-the-job This is a ge learnedy of them havxperience since man
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xpect benefits including Students
or them to learne learned
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y the Office of Print Production of TSCProduced b
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Click here
Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
DuPonttrade TishyPurereg titanium dioxide
duPont titanium technologies8004419485
wwwtitaniumdupontcom
The DuPont Oval DuPont trade The miracles of sciencereg and TishyPurereg
are trademarks or registered trademarks of EI du Pont de Nemours and Company
PoLYmers Light amp sCieNCe
Polymers Light and the Science of TiO2
Color Concentrates and
single Pigment dispersions
for all Thermoplastic Polymers
A World of Color Perfection since 1964
Corporate Offices
400 old dublin Pike
doylestown Pa 18901
(215) 345-6550
Operations amp
Research Center
2755 bergey road
hatfield Pa 19440
(215) 997-2221
wwwpenncolorcom
BTitanium dioxide
Brutile amp anatase
Bhigh Performance organic Pigments
B dPP reds hP yellowsB PvC additives
B lubricants amp stabilizers
364 Johnny Mercer blvd b-7 294 - savannah ga 31410
Tel (912)507-8972 - lwaltersagrofertinccom
wwwagrofertinccom
World leader in effect
Pigments
one international Plazasuite 300Philadelphia Pa 19113(888) 367-3275
wwwemdchemicalscom
A Complete Line of DyestuffsInorganic Pigments and
Organic Pigments forPlastics amp Fibers
lanXeSS corporation
111 rIDc Park west Drive 1-800-526-9377
Pittsburgh Pa 15275-1112 wwwlanxesscom
World Leaders in Ultramarine Pigmentswultramarine blue wultramarine violet
wChrome oxide green wlead Chromate
wZinc ferrite wiron oxide
Phone 770-338-4990
6369 Peachtree street fax 770-338-8315
norcross ga 30071 Toll free 886-682-4652wwwnubiolacom
We create chemistry for plastics
effect and functional pigments
eate chemistry for plastics
basfcomplastic-additiveswww
your plastic applicationsovide solutions for all ofand other additives pr
tnadixoitnasrezilibatsthgilVUruOfect and functional pigments efneeds with colorneeds with color ef
nufdnaelytsruoyteemsplehFSAASB
e crWWe cr
eate chemistry for plastics
1 800 431-2360 NJarkFlorham P
100 Campus DrivetionBASF Corpora
ovide solutions for all ofs rotaelcunst
fect and functional pigmentsy tilanoitcn
Color Software Experts
Since 1986
Quality Control Formulation
amp Instrument Profiling
Visit our website and color blog
wwwcyberchromeusacom
CyberChrome Inc
3642 Main Street tStone Ridge NY 12484
PH 845shy687shy26718601 DunwooDy Place Blg 334 atlanta ga uSa 30350
7709935500 wwwcolorchemcom
AMAPLASTreg DYES
IR ABSORBERS
NEOLORTM PIGMENTS
UVAPLASTTM UV ABSORBERS
SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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LTL Color CompoundersInc
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Clariant Corporation
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Betty Puckerin 812shy466shy9828
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Ticona
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Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
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Lansco Colors
markxxxpigmentscom
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Clariant Corp
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DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
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AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
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brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
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A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
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WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
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ech haintL and PsrrsoloCou Y
he tsech hastgmeni and P
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tcatnCo Ch336
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wwwspectradyescom
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Pigments and Additives for the Plastics Industry
Clariant Corporation4000 Monroe Road Charlotte NC 28205Phone 8004414414wwwclariantcom
Leading Manufacturer of Complex Inorganic Color Pigments (CICP) bull Pigment Brown 24 Yellow 53 Blue 28 Green 50 Black 28 etcbull Environmentally Friendly Pigments Brown 48 etcbull Laser Marking Pigmentsbull Pigments for Biodegradable Plastics
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SPE CAD NEWS Fall 2012 page 3 wwwspecadorg
The Color and Appearance Division (CAD) commits to the pub-lishing of at least three newsletters a year (four if there is sufficientmaterial to justify the extra issue) Each newsletter is electronical-ly distributed to our membership of nearly 1000) Each sponsorrsquosart directly links to the companyrsquos website
In addition we print one of these newsletters on 80gloss coatedstock All electronic versions are also posted on the SPE websitewhere it available for anyone to download
For the small donation of $300 per year we offer a business cardsized (2 x 35 inches) mention in our newsletter
We currently have the following slots available for sponsorship
(2) 2 x 35 inch or (1) 4 x 35 inch
If interested in learning more please contact
SHARYL REID Phone 8649682426
Email Sharyl_Reidusaschulmancom
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SPE CAD NEWS Fall 2012 page 4 wwwspecadorg
CounCilorrsquo s reporT
The Fall Council meeting was held on September 15 2012 in Dearborn MI The day before the Councilmeeting there were various committee meetings including Divisions Committee and ConferenceOversight Committee The Fall meeting is the election meeting at which time the next leaders of SPEare selected by the Councilors
MEMBERSHIP While membership has shown slow growth over the past couple years in the first halfof 2012 there has been 2 decrease in membership This has been attributed to reduced retention rates
and the scheduling of ANTECreg It is felt that the retention rates have been negatively impacted due to the difficulties asso-ciated with membership renewal using the website which are directly related to the management software being used bythe organization The scheduling of ANTECreg adversely impacted membership numbers because there were less than 12months between ANTECreg 2011 and ANTECreg 2012 therefore members who joined in order to attend ANTECreg 2011 atthe member rate were able to register for ANTECreg 2012 as a member without renewing their membership
FINANCIAL Despite budgeting more tightly for 2012 than 2011 the mid-year financial review has shown a $52000shortfall The second half is typically lower in revenue for the organization so there is little expectation of making up thisshortfall Additionally the impact of ANTECreg Mumbai is unknown The worst case scenario has a year-end shortfall of$350000 for the organization A revised budget is being prepared to minimize the shortfall
ELECTION Vijay Boolani was elected by the Councilors as the President-Elect Additionally Raed Al-Zubiwas elected as Senior Vice-President and Dick Cameron was elected Vice-President
Sincerely
Sandra DavisCAD Councilor
ediTorrsquo s noTe
Hopefully many of you had a chance to attend the past CAD RETECreg in Louisville this fall Itwas a historic event the 50th anniversary conference conducted by the Color and AppearanceDivision of the SPE Sandra Davis and her team should be commended for making it success-ful and memorable One thing that made it memorable for me was the attendance of one specialperson Robert Charvat Not only has Bob been a good friend and mentor to many of us on theboard he has the distinction of being one of the founding members of the CAD and not onlyattended the very first conference but also helped finance it Bob was recognized at the awardsreception and given a plaque listing all of the conferences to commemorate his involvement
throughout the years I have included a picture of Bob and his plaque Bob is no longer a board member but hestays involved and is always in our hearts One other thing I would like to mention is that I am the professor in TerraState Community Collegersquos Coloring of Plastics program which Bob was also instrumental in starting and nurturingFor those of you that might have not seen it in Plastics News in August there was a nice article about our programAs always I ask you to spread the word about Terra to your colleagues and contacts that may be in the need of colortraining If you have not had a chance to see the article click here to the linkHave a save and happy Holiday season
Jamie PrzybylskiCAD Editor
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Organic Pigments Inorganic Pigments
Pigment Preparations
Heucotech Ltd 99 Newbold Road Fairless Hills PA 19030
wwwheubachcolorcom 215-736-0712
Organic amp InorganicPigments and Preparations
(416) 253-4297 hkennedydominioncolourcomwwwdominioncolourcom
DOM 653 ProgramAd_retec09_v2_ 72209 217 PM Page 1
Quality Formulation oF
Color amp additive ConCentrates
wwwtechmerpmcom
18420 laurel Park road 1 Quality Circle
rancho dominguez Ca 90220 Clinton Tn 37716
(310) 632-9211
(865) 457-6700
ISHIHARA CORPORATION (USA)l TiO2 l Ultra-fine TiO2
l Nickel Titanates l Chrome Titanatesl Conductive Pigments
600 Montgomery Street Tel (415) 421shy8207
San Francisco California 94111 Fax (415) 397shy5403wwwishiharacom
page 5
SPE CAD NEWS Fall 2012 page 5 wwwspecadorg
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SPE CAD NEWS Fall 2012 page 6 wwwspecadorg
Color misChief 7Can sTorage of samples or sTandards
be a problem
The answer to the title question is ldquoOh my yes it canrdquo
Many organizations store their standards and samples in more ways thananyone wants to take the time to even think about And Many of them arejust plain wrong
However there is one storage method at the top of the list that defies any reasonable technical justification What is thatawful procedure Storing the standards or samples measurement data in a computer memory Then believe it or notusing that canned data for subsequent virtual judgments for things like quality control of production batches and other vitalissues In all coloring of plastics adventures one must try to reduce or eliminate as many variables as are known Or at leastreduce them to manageable values that can be compensated for Itrsquos the unknown variables that doom projects to failure
Now letrsquos address the chief subject of this article The total objective of standard and sample storage is to protect the piecesfrom any environment that might repeat might alter their visual and or measurement stability There are a number of caseswhere this problem occurs and is totally unknown to the participants These are the killers
Did you know the procedure used to cool a sample from a process such as injection molding as an example can affect itslong term color stability This can occur before andor during long term storage The environmental conditions of the stor-age environment can affect long term color stability
If the surface of the stored sample is not completely protected from scratches smudges and or other defacements the sample is no longer valid for visual andor measurement evaluations
A many laboratories store standards and samples in freezers This is OK so far But many do not temperature stabilize thesample before an evaluation This will bias any subsequent testing This includes removing any surface moisture that maydevelop as a sample warms to room temperature
One of the most insidious problems that many times go un-noticed is the wrapping or protection given samples as they gointo storage One very convenient method used by numerous operations is to put the sample in a manila folder then put thesample containing folder into a file drawer cabinet where the cabinet environment is not considered This may not be agood idea Is the folder used pH neutral The composition of folders andor papers can be highly acidic or alkaline Eithervariety may affect the stability of the standards andor samples stored in these papers The last one for this message is thatmany manila folders contain some form of sulfur in the paper Does any reader remember sulfide staining of polymers andtheir additives Maybe this is affecting your samples
This and many other possibilities may lead to changes in samples during storage The major puzzle for storage is be sureyou know and understand the storage parameters If the parameters are not understood stored samples may not be stableduring the storage cycle
Enough for this mischief for now As usual the guilty shall remain anonymous to protect them Look for the next ColorMischief 8 article soon
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SPE CAD NEWS Fall 2012 page 7 wwwspecadorg
The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry
In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly
The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)
Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years
reTeCreg 2012 Wrap-up
inviTaTion To aTTend our Cad board
meeTings
The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg
The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg
Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesra plastics program is
LC
N
EHHECSRUUROOUYYO
DNND
AAAN
UOY
EELLEUULDDUEED
y is this internet based three course cerindustr or undererer or undery of the newman
One aspect of Tspeak ofspeak of One aspect of T new hires etc) that havff new hires etc) that havsales staf
e all know people within the industrWWe all know people within the industr
earseral yseved students globallvy sersuccessfull
classroom activities This distance learning program hasOhio campus to parto students who may reside too f
tificatey is this internet based three course cer-educated members of our or under
s program that can benefitrarsquorarsquos program that can benefiter One aspect of T One aspect of Tere no color education to new hires etc) that hav
y (technicianse all know people within the industr
ell as locall as wyy as wed students globallclassroom activities This distance learning program has
eningticipate in full time day or evOhio campus to parremontar from the Fto students who may reside too fto students who may reside too far from the F
Section VLDistance Learning Courses Offer
4195592459at or more infF
tificate-educated members of our
s program that can benefite no color education to
y (technicians
or fyy fell as locallclassroom activities This distance learning program has
eningremont
Section VLDistance Learning Courses Offer
aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
aeduxt 2459TERRA e
essoram Profam Professorrram ProfProg ylski
courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
The threeyy The threesegments of the coloring of plastics industrorking in the manone wyor ane fbackground knowledg
on their schedule The three courses provide solidywhereee can complete anyprogram that the emplo
xibleel fley low cost no travelprogram It is a relativ
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
The threeyorking in the man
on their schedule The three courses provide solidywhere
xible
y 14mdashDecember 14)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14ndashMay 9)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14mdashDecember 14)ugust 20mdashDecember 14)
e-stat-state)stiderC3(
y 14ndashMay 9)ugust 20mdashDecember 14)
e-stat-state(3 Credits)
of plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
cellent opporxCourses are an e
ood fof plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
er coloror newtunity fcellent oppor
ered Spring 2013 (JfOfBooks approees $500 Ohio studentsF
VL Section
or people withtechnicians and others to learn more about the coloringmatchers quality control technicians production
er color
y 14mdashMay 9)anuarered Spring 2013 (Jy $150ximatelBooks appro
-stat$790 out-of$790 out-of-statees $500 Ohio studentsVL
y 14mdashMay 9)
e-stat-state(4 Credits)
tificate can ecompleting this cery behind what they do evthe theor
on-the-job This is a gxperience since many eindustr
of plastics These courses are also g
xpect benefits includingtificate can e Studentsy dayy day Studentsery behind what they do ev
or them to learntunity food opporon-the-job This is a ge learnedy of them havxperience since man
or people withood fof plastics These courses are also g
xpect benefits including Students
or them to learne learned
or people with
y the Office of Print Production of TSCProduced b
aeduterrwwwwwwterrremont OHF
C 030112y the Office of Print Production of TSC
Click here
Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
DuPonttrade TishyPurereg titanium dioxide
duPont titanium technologies8004419485
wwwtitaniumdupontcom
The DuPont Oval DuPont trade The miracles of sciencereg and TishyPurereg
are trademarks or registered trademarks of EI du Pont de Nemours and Company
PoLYmers Light amp sCieNCe
Polymers Light and the Science of TiO2
Color Concentrates and
single Pigment dispersions
for all Thermoplastic Polymers
A World of Color Perfection since 1964
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400 old dublin Pike
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Operations amp
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(215) 997-2221
wwwpenncolorcom
BTitanium dioxide
Brutile amp anatase
Bhigh Performance organic Pigments
B dPP reds hP yellowsB PvC additives
B lubricants amp stabilizers
364 Johnny Mercer blvd b-7 294 - savannah ga 31410
Tel (912)507-8972 - lwaltersagrofertinccom
wwwagrofertinccom
World leader in effect
Pigments
one international Plazasuite 300Philadelphia Pa 19113(888) 367-3275
wwwemdchemicalscom
A Complete Line of DyestuffsInorganic Pigments and
Organic Pigments forPlastics amp Fibers
lanXeSS corporation
111 rIDc Park west Drive 1-800-526-9377
Pittsburgh Pa 15275-1112 wwwlanxesscom
World Leaders in Ultramarine Pigmentswultramarine blue wultramarine violet
wChrome oxide green wlead Chromate
wZinc ferrite wiron oxide
Phone 770-338-4990
6369 Peachtree street fax 770-338-8315
norcross ga 30071 Toll free 886-682-4652wwwnubiolacom
We create chemistry for plastics
effect and functional pigments
eate chemistry for plastics
basfcomplastic-additiveswww
your plastic applicationsovide solutions for all ofand other additives pr
tnadixoitnasrezilibatsthgilVUruOfect and functional pigments efneeds with colorneeds with color ef
nufdnaelytsruoyteemsplehFSAASB
e crWWe cr
eate chemistry for plastics
1 800 431-2360 NJarkFlorham P
100 Campus DrivetionBASF Corpora
ovide solutions for all ofs rotaelcunst
fect and functional pigmentsy tilanoitcn
Color Software Experts
Since 1986
Quality Control Formulation
amp Instrument Profiling
Visit our website and color blog
wwwcyberchromeusacom
CyberChrome Inc
3642 Main Street tStone Ridge NY 12484
PH 845shy687shy26718601 DunwooDy Place Blg 334 atlanta ga uSa 30350
7709935500 wwwcolorchemcom
AMAPLASTreg DYES
IR ABSORBERS
NEOLORTM PIGMENTS
UVAPLASTTM UV ABSORBERS
SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
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SPE CAD NEWS Fall 2012 page 4 wwwspecadorg
CounCilorrsquo s reporT
The Fall Council meeting was held on September 15 2012 in Dearborn MI The day before the Councilmeeting there were various committee meetings including Divisions Committee and ConferenceOversight Committee The Fall meeting is the election meeting at which time the next leaders of SPEare selected by the Councilors
MEMBERSHIP While membership has shown slow growth over the past couple years in the first halfof 2012 there has been 2 decrease in membership This has been attributed to reduced retention rates
and the scheduling of ANTECreg It is felt that the retention rates have been negatively impacted due to the difficulties asso-ciated with membership renewal using the website which are directly related to the management software being used bythe organization The scheduling of ANTECreg adversely impacted membership numbers because there were less than 12months between ANTECreg 2011 and ANTECreg 2012 therefore members who joined in order to attend ANTECreg 2011 atthe member rate were able to register for ANTECreg 2012 as a member without renewing their membership
FINANCIAL Despite budgeting more tightly for 2012 than 2011 the mid-year financial review has shown a $52000shortfall The second half is typically lower in revenue for the organization so there is little expectation of making up thisshortfall Additionally the impact of ANTECreg Mumbai is unknown The worst case scenario has a year-end shortfall of$350000 for the organization A revised budget is being prepared to minimize the shortfall
ELECTION Vijay Boolani was elected by the Councilors as the President-Elect Additionally Raed Al-Zubiwas elected as Senior Vice-President and Dick Cameron was elected Vice-President
Sincerely
Sandra DavisCAD Councilor
ediTorrsquo s noTe
Hopefully many of you had a chance to attend the past CAD RETECreg in Louisville this fall Itwas a historic event the 50th anniversary conference conducted by the Color and AppearanceDivision of the SPE Sandra Davis and her team should be commended for making it success-ful and memorable One thing that made it memorable for me was the attendance of one specialperson Robert Charvat Not only has Bob been a good friend and mentor to many of us on theboard he has the distinction of being one of the founding members of the CAD and not onlyattended the very first conference but also helped finance it Bob was recognized at the awardsreception and given a plaque listing all of the conferences to commemorate his involvement
throughout the years I have included a picture of Bob and his plaque Bob is no longer a board member but hestays involved and is always in our hearts One other thing I would like to mention is that I am the professor in TerraState Community Collegersquos Coloring of Plastics program which Bob was also instrumental in starting and nurturingFor those of you that might have not seen it in Plastics News in August there was a nice article about our programAs always I ask you to spread the word about Terra to your colleagues and contacts that may be in the need of colortraining If you have not had a chance to see the article click here to the linkHave a save and happy Holiday season
Jamie PrzybylskiCAD Editor
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Organic Pigments Inorganic Pigments
Pigment Preparations
Heucotech Ltd 99 Newbold Road Fairless Hills PA 19030
wwwheubachcolorcom 215-736-0712
Organic amp InorganicPigments and Preparations
(416) 253-4297 hkennedydominioncolourcomwwwdominioncolourcom
DOM 653 ProgramAd_retec09_v2_ 72209 217 PM Page 1
Quality Formulation oF
Color amp additive ConCentrates
wwwtechmerpmcom
18420 laurel Park road 1 Quality Circle
rancho dominguez Ca 90220 Clinton Tn 37716
(310) 632-9211
(865) 457-6700
ISHIHARA CORPORATION (USA)l TiO2 l Ultra-fine TiO2
l Nickel Titanates l Chrome Titanatesl Conductive Pigments
600 Montgomery Street Tel (415) 421shy8207
San Francisco California 94111 Fax (415) 397shy5403wwwishiharacom
page 5
SPE CAD NEWS Fall 2012 page 5 wwwspecadorg
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SPE CAD NEWS Fall 2012 page 6 wwwspecadorg
Color misChief 7Can sTorage of samples or sTandards
be a problem
The answer to the title question is ldquoOh my yes it canrdquo
Many organizations store their standards and samples in more ways thananyone wants to take the time to even think about And Many of them arejust plain wrong
However there is one storage method at the top of the list that defies any reasonable technical justification What is thatawful procedure Storing the standards or samples measurement data in a computer memory Then believe it or notusing that canned data for subsequent virtual judgments for things like quality control of production batches and other vitalissues In all coloring of plastics adventures one must try to reduce or eliminate as many variables as are known Or at leastreduce them to manageable values that can be compensated for Itrsquos the unknown variables that doom projects to failure
Now letrsquos address the chief subject of this article The total objective of standard and sample storage is to protect the piecesfrom any environment that might repeat might alter their visual and or measurement stability There are a number of caseswhere this problem occurs and is totally unknown to the participants These are the killers
Did you know the procedure used to cool a sample from a process such as injection molding as an example can affect itslong term color stability This can occur before andor during long term storage The environmental conditions of the stor-age environment can affect long term color stability
If the surface of the stored sample is not completely protected from scratches smudges and or other defacements the sample is no longer valid for visual andor measurement evaluations
A many laboratories store standards and samples in freezers This is OK so far But many do not temperature stabilize thesample before an evaluation This will bias any subsequent testing This includes removing any surface moisture that maydevelop as a sample warms to room temperature
One of the most insidious problems that many times go un-noticed is the wrapping or protection given samples as they gointo storage One very convenient method used by numerous operations is to put the sample in a manila folder then put thesample containing folder into a file drawer cabinet where the cabinet environment is not considered This may not be agood idea Is the folder used pH neutral The composition of folders andor papers can be highly acidic or alkaline Eithervariety may affect the stability of the standards andor samples stored in these papers The last one for this message is thatmany manila folders contain some form of sulfur in the paper Does any reader remember sulfide staining of polymers andtheir additives Maybe this is affecting your samples
This and many other possibilities may lead to changes in samples during storage The major puzzle for storage is be sureyou know and understand the storage parameters If the parameters are not understood stored samples may not be stableduring the storage cycle
Enough for this mischief for now As usual the guilty shall remain anonymous to protect them Look for the next ColorMischief 8 article soon
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rs
SPE CAD NEWS Fall 2012 page 7 wwwspecadorg
The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry
In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly
The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)
Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years
reTeCreg 2012 Wrap-up
inviTaTion To aTTend our Cad board
meeTings
The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg
The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg
Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesra plastics program is
LC
N
EHHECSRUUROOUYYO
DNND
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EELLEUULDDUEED
y is this internet based three course cerindustr or undererer or undery of the newman
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Section VLDistance Learning Courses Offer
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tificate-educated members of our
s program that can benefite no color education to
y (technicians
or fyy fell as locallclassroom activities This distance learning program has
eningremont
Section VLDistance Learning Courses Offer
aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
aeduxt 2459TERRA e
essoram Profam Professorrram ProfProg ylski
courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
The threeyy The threesegments of the coloring of plastics industrorking in the manone wyor ane fbackground knowledg
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ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
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on their schedule The three courses provide solidywhere
xible
y 14mdashDecember 14)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
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-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14mdashDecember 14)ugust 20mdashDecember 14)
e-stat-state)stiderC3(
y 14ndashMay 9)ugust 20mdashDecember 14)
e-stat-state(3 Credits)
of plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
cellent opporxCourses are an e
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e-stat-state(4 Credits)
tificate can ecompleting this cery behind what they do evthe theor
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xpect benefits includingtificate can e Studentsy dayy day Studentsery behind what they do ev
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Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
DuPonttrade TishyPurereg titanium dioxide
duPont titanium technologies8004419485
wwwtitaniumdupontcom
The DuPont Oval DuPont trade The miracles of sciencereg and TishyPurereg
are trademarks or registered trademarks of EI du Pont de Nemours and Company
PoLYmers Light amp sCieNCe
Polymers Light and the Science of TiO2
Color Concentrates and
single Pigment dispersions
for all Thermoplastic Polymers
A World of Color Perfection since 1964
Corporate Offices
400 old dublin Pike
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(215) 345-6550
Operations amp
Research Center
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hatfield Pa 19440
(215) 997-2221
wwwpenncolorcom
BTitanium dioxide
Brutile amp anatase
Bhigh Performance organic Pigments
B dPP reds hP yellowsB PvC additives
B lubricants amp stabilizers
364 Johnny Mercer blvd b-7 294 - savannah ga 31410
Tel (912)507-8972 - lwaltersagrofertinccom
wwwagrofertinccom
World leader in effect
Pigments
one international Plazasuite 300Philadelphia Pa 19113(888) 367-3275
wwwemdchemicalscom
A Complete Line of DyestuffsInorganic Pigments and
Organic Pigments forPlastics amp Fibers
lanXeSS corporation
111 rIDc Park west Drive 1-800-526-9377
Pittsburgh Pa 15275-1112 wwwlanxesscom
World Leaders in Ultramarine Pigmentswultramarine blue wultramarine violet
wChrome oxide green wlead Chromate
wZinc ferrite wiron oxide
Phone 770-338-4990
6369 Peachtree street fax 770-338-8315
norcross ga 30071 Toll free 886-682-4652wwwnubiolacom
We create chemistry for plastics
effect and functional pigments
eate chemistry for plastics
basfcomplastic-additiveswww
your plastic applicationsovide solutions for all ofand other additives pr
tnadixoitnasrezilibatsthgilVUruOfect and functional pigments efneeds with colorneeds with color ef
nufdnaelytsruoyteemsplehFSAASB
e crWWe cr
eate chemistry for plastics
1 800 431-2360 NJarkFlorham P
100 Campus DrivetionBASF Corpora
ovide solutions for all ofs rotaelcunst
fect and functional pigmentsy tilanoitcn
Color Software Experts
Since 1986
Quality Control Formulation
amp Instrument Profiling
Visit our website and color blog
wwwcyberchromeusacom
CyberChrome Inc
3642 Main Street tStone Ridge NY 12484
PH 845shy687shy26718601 DunwooDy Place Blg 334 atlanta ga uSa 30350
7709935500 wwwcolorchemcom
AMAPLASTreg DYES
IR ABSORBERS
NEOLORTM PIGMENTS
UVAPLASTTM UV ABSORBERS
SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
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Organic Pigments Inorganic Pigments
Pigment Preparations
Heucotech Ltd 99 Newbold Road Fairless Hills PA 19030
wwwheubachcolorcom 215-736-0712
Organic amp InorganicPigments and Preparations
(416) 253-4297 hkennedydominioncolourcomwwwdominioncolourcom
DOM 653 ProgramAd_retec09_v2_ 72209 217 PM Page 1
Quality Formulation oF
Color amp additive ConCentrates
wwwtechmerpmcom
18420 laurel Park road 1 Quality Circle
rancho dominguez Ca 90220 Clinton Tn 37716
(310) 632-9211
(865) 457-6700
ISHIHARA CORPORATION (USA)l TiO2 l Ultra-fine TiO2
l Nickel Titanates l Chrome Titanatesl Conductive Pigments
600 Montgomery Street Tel (415) 421shy8207
San Francisco California 94111 Fax (415) 397shy5403wwwishiharacom
page 5
SPE CAD NEWS Fall 2012 page 5 wwwspecadorg
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SPE CAD NEWS Fall 2012 page 6 wwwspecadorg
Color misChief 7Can sTorage of samples or sTandards
be a problem
The answer to the title question is ldquoOh my yes it canrdquo
Many organizations store their standards and samples in more ways thananyone wants to take the time to even think about And Many of them arejust plain wrong
However there is one storage method at the top of the list that defies any reasonable technical justification What is thatawful procedure Storing the standards or samples measurement data in a computer memory Then believe it or notusing that canned data for subsequent virtual judgments for things like quality control of production batches and other vitalissues In all coloring of plastics adventures one must try to reduce or eliminate as many variables as are known Or at leastreduce them to manageable values that can be compensated for Itrsquos the unknown variables that doom projects to failure
Now letrsquos address the chief subject of this article The total objective of standard and sample storage is to protect the piecesfrom any environment that might repeat might alter their visual and or measurement stability There are a number of caseswhere this problem occurs and is totally unknown to the participants These are the killers
Did you know the procedure used to cool a sample from a process such as injection molding as an example can affect itslong term color stability This can occur before andor during long term storage The environmental conditions of the stor-age environment can affect long term color stability
If the surface of the stored sample is not completely protected from scratches smudges and or other defacements the sample is no longer valid for visual andor measurement evaluations
A many laboratories store standards and samples in freezers This is OK so far But many do not temperature stabilize thesample before an evaluation This will bias any subsequent testing This includes removing any surface moisture that maydevelop as a sample warms to room temperature
One of the most insidious problems that many times go un-noticed is the wrapping or protection given samples as they gointo storage One very convenient method used by numerous operations is to put the sample in a manila folder then put thesample containing folder into a file drawer cabinet where the cabinet environment is not considered This may not be agood idea Is the folder used pH neutral The composition of folders andor papers can be highly acidic or alkaline Eithervariety may affect the stability of the standards andor samples stored in these papers The last one for this message is thatmany manila folders contain some form of sulfur in the paper Does any reader remember sulfide staining of polymers andtheir additives Maybe this is affecting your samples
This and many other possibilities may lead to changes in samples during storage The major puzzle for storage is be sureyou know and understand the storage parameters If the parameters are not understood stored samples may not be stableduring the storage cycle
Enough for this mischief for now As usual the guilty shall remain anonymous to protect them Look for the next ColorMischief 8 article soon
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SPE CAD NEWS Fall 2012 page 7 wwwspecadorg
The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry
In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly
The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)
Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years
reTeCreg 2012 Wrap-up
inviTaTion To aTTend our Cad board
meeTings
The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg
The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg
Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesra plastics program is
LC
N
EHHECSRUUROOUYYO
DNND
AAAN
UOY
EELLEUULDDUEED
y is this internet based three course cerindustr or undererer or undery of the newman
One aspect of Tspeak ofspeak of One aspect of T new hires etc) that havff new hires etc) that havsales staf
e all know people within the industrWWe all know people within the industr
earseral yseved students globallvy sersuccessfull
classroom activities This distance learning program hasOhio campus to parto students who may reside too f
tificatey is this internet based three course cer-educated members of our or under
s program that can benefitrarsquorarsquos program that can benefiter One aspect of T One aspect of Tere no color education to new hires etc) that hav
y (technicianse all know people within the industr
ell as locall as wyy as wed students globallclassroom activities This distance learning program has
eningticipate in full time day or evOhio campus to parremontar from the Fto students who may reside too fto students who may reside too far from the F
Section VLDistance Learning Courses Offer
4195592459at or more infF
tificate-educated members of our
s program that can benefite no color education to
y (technicians
or fyy fell as locallclassroom activities This distance learning program has
eningremont
Section VLDistance Learning Courses Offer
aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
aeduxt 2459TERRA e
essoram Profam Professorrram ProfProg ylski
courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
The threeyy The threesegments of the coloring of plastics industrorking in the manone wyor ane fbackground knowledg
on their schedule The three courses provide solidywhereee can complete anyprogram that the emplo
xibleel fley low cost no travelprogram It is a relativ
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
The threeyorking in the man
on their schedule The three courses provide solidywhere
xible
y 14mdashDecember 14)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14ndashMay 9)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14mdashDecember 14)ugust 20mdashDecember 14)
e-stat-state)stiderC3(
y 14ndashMay 9)ugust 20mdashDecember 14)
e-stat-state(3 Credits)
of plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
cellent opporxCourses are an e
ood fof plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
er coloror newtunity fcellent oppor
ered Spring 2013 (JfOfBooks approees $500 Ohio studentsF
VL Section
or people withtechnicians and others to learn more about the coloringmatchers quality control technicians production
er color
y 14mdashMay 9)anuarered Spring 2013 (Jy $150ximatelBooks appro
-stat$790 out-of$790 out-of-statees $500 Ohio studentsVL
y 14mdashMay 9)
e-stat-state(4 Credits)
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on-the-job This is a gxperience since many eindustr
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xpect benefits includingtificate can e Studentsy dayy day Studentsery behind what they do ev
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Click here
Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
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Since 1986
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7709935500 wwwcolorchemcom
AMAPLASTreg DYES
IR ABSORBERS
NEOLORTM PIGMENTS
UVAPLASTTM UV ABSORBERS
SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
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Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
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infoxxxeshyxyncom
OTHER USEFUL CONTACTS
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SPE CAD NEWS Fall 2012 page 6 wwwspecadorg
Color misChief 7Can sTorage of samples or sTandards
be a problem
The answer to the title question is ldquoOh my yes it canrdquo
Many organizations store their standards and samples in more ways thananyone wants to take the time to even think about And Many of them arejust plain wrong
However there is one storage method at the top of the list that defies any reasonable technical justification What is thatawful procedure Storing the standards or samples measurement data in a computer memory Then believe it or notusing that canned data for subsequent virtual judgments for things like quality control of production batches and other vitalissues In all coloring of plastics adventures one must try to reduce or eliminate as many variables as are known Or at leastreduce them to manageable values that can be compensated for Itrsquos the unknown variables that doom projects to failure
Now letrsquos address the chief subject of this article The total objective of standard and sample storage is to protect the piecesfrom any environment that might repeat might alter their visual and or measurement stability There are a number of caseswhere this problem occurs and is totally unknown to the participants These are the killers
Did you know the procedure used to cool a sample from a process such as injection molding as an example can affect itslong term color stability This can occur before andor during long term storage The environmental conditions of the stor-age environment can affect long term color stability
If the surface of the stored sample is not completely protected from scratches smudges and or other defacements the sample is no longer valid for visual andor measurement evaluations
A many laboratories store standards and samples in freezers This is OK so far But many do not temperature stabilize thesample before an evaluation This will bias any subsequent testing This includes removing any surface moisture that maydevelop as a sample warms to room temperature
One of the most insidious problems that many times go un-noticed is the wrapping or protection given samples as they gointo storage One very convenient method used by numerous operations is to put the sample in a manila folder then put thesample containing folder into a file drawer cabinet where the cabinet environment is not considered This may not be agood idea Is the folder used pH neutral The composition of folders andor papers can be highly acidic or alkaline Eithervariety may affect the stability of the standards andor samples stored in these papers The last one for this message is thatmany manila folders contain some form of sulfur in the paper Does any reader remember sulfide staining of polymers andtheir additives Maybe this is affecting your samples
This and many other possibilities may lead to changes in samples during storage The major puzzle for storage is be sureyou know and understand the storage parameters If the parameters are not understood stored samples may not be stableduring the storage cycle
Enough for this mischief for now As usual the guilty shall remain anonymous to protect them Look for the next ColorMischief 8 article soon
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SPE CAD NEWS Fall 2012 page 7 wwwspecadorg
The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry
In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly
The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)
Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years
reTeCreg 2012 Wrap-up
inviTaTion To aTTend our Cad board
meeTings
The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg
The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg
Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesra plastics program is
LC
N
EHHECSRUUROOUYYO
DNND
AAAN
UOY
EELLEUULDDUEED
y is this internet based three course cerindustr or undererer or undery of the newman
One aspect of Tspeak ofspeak of One aspect of T new hires etc) that havff new hires etc) that havsales staf
e all know people within the industrWWe all know people within the industr
earseral yseved students globallvy sersuccessfull
classroom activities This distance learning program hasOhio campus to parto students who may reside too f
tificatey is this internet based three course cer-educated members of our or under
s program that can benefitrarsquorarsquos program that can benefiter One aspect of T One aspect of Tere no color education to new hires etc) that hav
y (technicianse all know people within the industr
ell as locall as wyy as wed students globallclassroom activities This distance learning program has
eningticipate in full time day or evOhio campus to parremontar from the Fto students who may reside too fto students who may reside too far from the F
Section VLDistance Learning Courses Offer
4195592459at or more infF
tificate-educated members of our
s program that can benefite no color education to
y (technicians
or fyy fell as locallclassroom activities This distance learning program has
eningremont
Section VLDistance Learning Courses Offer
aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
aeduxt 2459TERRA e
essoram Profam Professorrram ProfProg ylski
courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
The threeyy The threesegments of the coloring of plastics industrorking in the manone wyor ane fbackground knowledg
on their schedule The three courses provide solidywhereee can complete anyprogram that the emplo
xibleel fley low cost no travelprogram It is a relativ
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
The threeyorking in the man
on their schedule The three courses provide solidywhere
xible
y 14mdashDecember 14)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14ndashMay 9)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14mdashDecember 14)ugust 20mdashDecember 14)
e-stat-state)stiderC3(
y 14ndashMay 9)ugust 20mdashDecember 14)
e-stat-state(3 Credits)
of plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
cellent opporxCourses are an e
ood fof plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
er coloror newtunity fcellent oppor
ered Spring 2013 (JfOfBooks approees $500 Ohio studentsF
VL Section
or people withtechnicians and others to learn more about the coloringmatchers quality control technicians production
er color
y 14mdashMay 9)anuarered Spring 2013 (Jy $150ximatelBooks appro
-stat$790 out-of$790 out-of-statees $500 Ohio studentsVL
y 14mdashMay 9)
e-stat-state(4 Credits)
tificate can ecompleting this cery behind what they do evthe theor
on-the-job This is a gxperience since many eindustr
of plastics These courses are also g
xpect benefits includingtificate can e Studentsy dayy day Studentsery behind what they do ev
or them to learntunity food opporon-the-job This is a ge learnedy of them havxperience since man
or people withood fof plastics These courses are also g
xpect benefits including Students
or them to learne learned
or people with
y the Office of Print Production of TSCProduced b
aeduterrwwwwwwterrremont OHF
C 030112y the Office of Print Production of TSC
Click here
Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
DuPonttrade TishyPurereg titanium dioxide
duPont titanium technologies8004419485
wwwtitaniumdupontcom
The DuPont Oval DuPont trade The miracles of sciencereg and TishyPurereg
are trademarks or registered trademarks of EI du Pont de Nemours and Company
PoLYmers Light amp sCieNCe
Polymers Light and the Science of TiO2
Color Concentrates and
single Pigment dispersions
for all Thermoplastic Polymers
A World of Color Perfection since 1964
Corporate Offices
400 old dublin Pike
doylestown Pa 18901
(215) 345-6550
Operations amp
Research Center
2755 bergey road
hatfield Pa 19440
(215) 997-2221
wwwpenncolorcom
BTitanium dioxide
Brutile amp anatase
Bhigh Performance organic Pigments
B dPP reds hP yellowsB PvC additives
B lubricants amp stabilizers
364 Johnny Mercer blvd b-7 294 - savannah ga 31410
Tel (912)507-8972 - lwaltersagrofertinccom
wwwagrofertinccom
World leader in effect
Pigments
one international Plazasuite 300Philadelphia Pa 19113(888) 367-3275
wwwemdchemicalscom
A Complete Line of DyestuffsInorganic Pigments and
Organic Pigments forPlastics amp Fibers
lanXeSS corporation
111 rIDc Park west Drive 1-800-526-9377
Pittsburgh Pa 15275-1112 wwwlanxesscom
World Leaders in Ultramarine Pigmentswultramarine blue wultramarine violet
wChrome oxide green wlead Chromate
wZinc ferrite wiron oxide
Phone 770-338-4990
6369 Peachtree street fax 770-338-8315
norcross ga 30071 Toll free 886-682-4652wwwnubiolacom
We create chemistry for plastics
effect and functional pigments
eate chemistry for plastics
basfcomplastic-additiveswww
your plastic applicationsovide solutions for all ofand other additives pr
tnadixoitnasrezilibatsthgilVUruOfect and functional pigments efneeds with colorneeds with color ef
nufdnaelytsruoyteemsplehFSAASB
e crWWe cr
eate chemistry for plastics
1 800 431-2360 NJarkFlorham P
100 Campus DrivetionBASF Corpora
ovide solutions for all ofs rotaelcunst
fect and functional pigmentsy tilanoitcn
Color Software Experts
Since 1986
Quality Control Formulation
amp Instrument Profiling
Visit our website and color blog
wwwcyberchromeusacom
CyberChrome Inc
3642 Main Street tStone Ridge NY 12484
PH 845shy687shy26718601 DunwooDy Place Blg 334 atlanta ga uSa 30350
7709935500 wwwcolorchemcom
AMAPLASTreg DYES
IR ABSORBERS
NEOLORTM PIGMENTS
UVAPLASTTM UV ABSORBERS
SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
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SPE CAD NEWS Fall 2012 page 7 wwwspecadorg
The celebratory SPE CAD RETECreg 2012 was considered a wonderful suc-cess by all reports At the beginning of October 475 plastics coloring indus-try professionals gathered in Louisville KY for an opportunity to learnshare and network This yearrsquos conference was the 50th anniversary of thefirst SPE plastics coloring conference and the importance of this milestonewas celebrated throughout the conference The conference kicked off witha Sunday evening reception at Glassworks an art glass studio and includeda demonstration of the artistry
In addition to the usual technical sessions this year there was an interactivepanel discussion where the audience provided their answers to questionswhich were then addressed by three panelists Dwight Morgan (TechmerPMAccel Color) Craig Sibol (BASF) and Larry Nitardy (ComAssist)While the concept was new to this group the audience responded quickly
The coordination of the conference was team effort lead by Sandra Davis(DuPont Titanium Technologies) with support from Betty Puckerin(Ampacet) Jeff Drusda (Silberline) Johnny Suthers (retired) BruceMulholland (Ticona) Sharyl Reid (A Schulman) Sharon Ehr (UniformColor) Tracy Phillips (Uniform Color) Brian West (Techmer PM)Howard Kennedy (Dominion Colour) and Mark Tyler (Ticona)
Right Bob Charvat receives an honorary plaque for his many contributionsto the Color and Appearance Division over the last 50 years
reTeCreg 2012 Wrap-up
inviTaTion To aTTend our Cad board
meeTings
The Color and Appearance Division regularly holds Board of Director(BOD) meetings at the ANTECreg and the CAD RETECreg In addi-tion a Summer BOD meeting is typically held about 6 weeks prior tothe next CAD RETECreg
The Summer meeting is scheduled in various locations A Winter BOD meeting is held in January The Winter meeting is typically held at a site of a future RETECreg
Any SPE CAD members who wish to attend are welcome at these meetings If interested in attending the next Boardmeeting please contact the Division Chairperson for more information
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
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SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
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7709935500 wwwcolorchemcom
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SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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rs
SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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Sandra Davis 302shy999shy2540
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
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Uniform Color
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Techmer PM LLC
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Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
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203shy775shy0471 phone
customerservicexxx4speorg
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OTHER USEFUL CONTACTS
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SPE CAD NEWS Fall 2012 page 8 wwwspecadorg
soCieTy of plasTiCs engineers
endoWmenT sCholarship program
for The 2013 ndash 2014 sChool year
The Endowment Scholarship Program offered by the Color amp Appearance Division of the Society of Plastics Engineersawards up to five scholarships each year to students who have demonstrated or expressed an interest in the coloring ofplastics industry The students must be majoring in or taking courses that would be beneficial to a career in this indus-try This would include but is not limited to plastics engineering polymer science coloring of plastics chemistryphysics chemical engineering mechanical engineering industrial design and industrial engineering All applicants mustbe in good standing with their colleges Financial need is considered for most scholarships
Undergraduate and graduate scholarships range up to $4000 annually Scholarships are awarded for one year only butapplicants may apply for a re-award for each year they are enrolled in school
scholarship eligibility1 Applicants for these scholarships must be full-time undergraduate students in either a four-year college or a two-yeartechnical program or enrolled in a graduate program2 All applicants must be graduates of public or private high schools
scholarship Criteria1 Applicants must have a demonstrated or expressed interest in the coloring of plastics industry2 Applicants must be majoring in or taking courses that would be beneficial to a career in the coloring of plastics industry3 An applicant must be in good academic standing with his or her school4 Preference is given to student members of SPE and also to students who have a parent(s) as a member of the
Color amp Appearance Division of the SPE5 Financial need of an applicant will be considered for most scholarships
application procedureTo be considered for a scholarship from the Color amp Appearance Division Endowment Scholarship Programapplicants must complete an application available at WWWSPECADorg and return it to the address specified on theapplication by June 15 2013 All applications submitted must include1 A completed application form2 Three recommendation letters two from a teacher or school official and one from an employer or non-relative3 A high school andor college transcript for the last two years4 An essay by the student (500 words or less) telling why the applicant is applying for the scholarship the applicantrsquosqualifications and the applicantrsquos educational and career goals in the coloring of plastics industry
Dear Members
Just a reminder that you can view past and current BOARD MINUTES onthe SPECAD website
We do not typically publish the minutes in the electronic versions of ournewsletter but they are always available for our members to view from ourwebsite The site is is not completely current at this time as we are in theprocess of giving it a makeover and new launch in January
Click here for the link to view httpwwwspecadorgindexphpnavid=28
BOARD MINUTES
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesra plastics program is
LC
N
EHHECSRUUROOUYYO
DNND
AAAN
UOY
EELLEUULDDUEED
y is this internet based three course cerindustr or undererer or undery of the newman
One aspect of Tspeak ofspeak of One aspect of T new hires etc) that havff new hires etc) that havsales staf
e all know people within the industrWWe all know people within the industr
earseral yseved students globallvy sersuccessfull
classroom activities This distance learning program hasOhio campus to parto students who may reside too f
tificatey is this internet based three course cer-educated members of our or under
s program that can benefitrarsquorarsquos program that can benefiter One aspect of T One aspect of Tere no color education to new hires etc) that hav
y (technicianse all know people within the industr
ell as locall as wyy as wed students globallclassroom activities This distance learning program has
eningticipate in full time day or evOhio campus to parremontar from the Fto students who may reside too fto students who may reside too far from the F
Section VLDistance Learning Courses Offer
4195592459at or more infF
tificate-educated members of our
s program that can benefite no color education to
y (technicians
or fyy fell as locallclassroom activities This distance learning program has
eningremont
Section VLDistance Learning Courses Offer
aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
aeduxt 2459TERRA e
essoram Profam Professorrram ProfProg ylski
courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
The threeyy The threesegments of the coloring of plastics industrorking in the manone wyor ane fbackground knowledg
on their schedule The three courses provide solidywhereee can complete anyprogram that the emplo
xibleel fley low cost no travelprogram It is a relativ
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
The threeyorking in the man
on their schedule The three courses provide solidywhere
xible
y 14mdashDecember 14)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14ndashMay 9)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
-stat$600 out-of$600 out-of-statees $400 Ohio studentsSection VL
y 14mdashDecember 14)ugust 20mdashDecember 14)
e-stat-state)stiderC3(
y 14ndashMay 9)ugust 20mdashDecember 14)
e-stat-state(3 Credits)
of plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
cellent opporxCourses are an e
ood fof plastics These courses are also gtechnicians and others to learn more about the coloringmatchers quality control technicians production
er coloror newtunity fcellent oppor
ered Spring 2013 (JfOfBooks approees $500 Ohio studentsF
VL Section
or people withtechnicians and others to learn more about the coloringmatchers quality control technicians production
er color
y 14mdashMay 9)anuarered Spring 2013 (Jy $150ximatelBooks appro
-stat$790 out-of$790 out-of-statees $500 Ohio studentsVL
y 14mdashMay 9)
e-stat-state(4 Credits)
tificate can ecompleting this cery behind what they do evthe theor
on-the-job This is a gxperience since many eindustr
of plastics These courses are also g
xpect benefits includingtificate can e Studentsy dayy day Studentsery behind what they do ev
or them to learntunity food opporon-the-job This is a ge learnedy of them havxperience since man
or people withood fof plastics These courses are also g
xpect benefits including Students
or them to learne learned
or people with
y the Office of Print Production of TSCProduced b
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Click here
Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
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IR ABSORBERS
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SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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Clariant Corporation
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Silberline Manufacturing Co Inc
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
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Steve Esker 614shy679shy4677
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AlanBodixxxPolyonecom
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FrankxxxPigmentscom
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Ferro Corporation
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sharyl_reidxxxusaschulmancom
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A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
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847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
SPE CAD NEWS Fall 2012 page 9 wwwspecadorg
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The beautiful Inner Harbor District is the perfect venue to present your topic to the premiertechnical conference devoted to the color and appearance of plastics
Contacts Paul Bykowski Brenda MullinsGB Consulting Clariant CorporationPortage IN Cumming GA 219-331-6981 678-237-2975paulbykowskihotmailcom brendamullinsclariantcom
Venue Baltimore Marriott WaterfrontBaltimore MD
Call for papers
ConneCt With sPe Cad via soCial media
Join SPECADrsquos Group On Linked In to network with industry peers participate in group discussions of industry and technicaltopics find job opportunities and get the latest division and conference announcements
Group Name SPE Color amp Appearance Division Group ID 152108
wwwlinkedincomgroupsgid=152108
September 22-24 2013 Society of Plastics Engineers
Color andAppearance
Division
Abstract Deadline February 2013 Event September 22-24 2013
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KRRKOWTAATHHA
TTHSSTEESSSESSSAL
YD
NUU
NOOU
RRO
AARKKA
a State Community CollegeerrTTerrat On-Line Plastics and Coloring of Plastics
its ability to provide eature of the Te fy distinctiverA v
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesdistance learningrdquoldquora plastics program isereature of the Teature of the Ter
a State Community CollegeOn-Line Plastics and Coloring of Plastics
(online) coursesra plastics program is
LC
N
EHHECSRUUROOUYYO
DNND
AAAN
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EELLEUULDDUEED
y is this internet based three course cerindustr or undererer or undery of the newman
One aspect of Tspeak ofspeak of One aspect of T new hires etc) that havff new hires etc) that havsales staf
e all know people within the industrWWe all know people within the industr
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tificatey is this internet based three course cer-educated members of our or under
s program that can benefitrarsquorarsquos program that can benefiter One aspect of T One aspect of Tere no color education to new hires etc) that hav
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Section VLDistance Learning Courses Offer
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tificate-educated members of our
s program that can benefite no color education to
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or fyy fell as locallclassroom activities This distance learning program has
eningremont
Section VLDistance Learning Courses Offer
aeduylskiterrjprzybjprzybylskiterror email TERRA eTTTERRA e866A866AT or toll free 4195592459ylskiamie Przybamie PrzybylskiJormation contact or more inf
(3 Credits)edDistance Learning Courses Offer
aeduxt 2459TERRA e
essoram Profam Professorrram ProfProg ylski
courses aresegments of the coloring of plastics industrbackground knowledgon their schedule The three courses provide solidprogram that the emploprogram It is a relativ
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ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
ered Spring 2013 (JfOfall 2012 (Aered FfOf
Books approees $400 Ohio studentsF
Section VL
The threeyorking in the man
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xible
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y 14ndashMay 9)anuarered Spring 2013 (Jugust 20mdashDecember 14)all 2012 (Ay $200ximatelBooks appro
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y 14mdashDecember 14)ugust 20mdashDecember 14)
e-stat-state)stiderC3(
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e-stat-state(3 Credits)
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y 14mdashMay 9)
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tificate can ecompleting this cery behind what they do evthe theor
on-the-job This is a gxperience since many eindustr
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xpect benefits includingtificate can e Studentsy dayy day Studentsery behind what they do ev
or them to learntunity food opporon-the-job This is a ge learnedy of them havxperience since man
or people withood fof plastics These courses are also g
xpect benefits including Students
or them to learne learned
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y the Office of Print Production of TSCProduced b
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Click here
Plastics News Article
highlighting Terra
SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
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(215) 345-6550
Operations amp
Research Center
2755 bergey road
hatfield Pa 19440
(215) 997-2221
wwwpenncolorcom
BTitanium dioxide
Brutile amp anatase
Bhigh Performance organic Pigments
B dPP reds hP yellowsB PvC additives
B lubricants amp stabilizers
364 Johnny Mercer blvd b-7 294 - savannah ga 31410
Tel (912)507-8972 - lwaltersagrofertinccom
wwwagrofertinccom
World leader in effect
Pigments
one international Plazasuite 300Philadelphia Pa 19113(888) 367-3275
wwwemdchemicalscom
A Complete Line of DyestuffsInorganic Pigments and
Organic Pigments forPlastics amp Fibers
lanXeSS corporation
111 rIDc Park west Drive 1-800-526-9377
Pittsburgh Pa 15275-1112 wwwlanxesscom
World Leaders in Ultramarine Pigmentswultramarine blue wultramarine violet
wChrome oxide green wlead Chromate
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Phone 770-338-4990
6369 Peachtree street fax 770-338-8315
norcross ga 30071 Toll free 886-682-4652wwwnubiolacom
We create chemistry for plastics
effect and functional pigments
eate chemistry for plastics
basfcomplastic-additiveswww
your plastic applicationsovide solutions for all ofand other additives pr
tnadixoitnasrezilibatsthgilVUruOfect and functional pigments efneeds with colorneeds with color ef
nufdnaelytsruoyteemsplehFSAASB
e crWWe cr
eate chemistry for plastics
1 800 431-2360 NJarkFlorham P
100 Campus DrivetionBASF Corpora
ovide solutions for all ofs rotaelcunst
fect and functional pigmentsy tilanoitcn
Color Software Experts
Since 1986
Quality Control Formulation
amp Instrument Profiling
Visit our website and color blog
wwwcyberchromeusacom
CyberChrome Inc
3642 Main Street tStone Ridge NY 12484
PH 845shy687shy26718601 DunwooDy Place Blg 334 atlanta ga uSa 30350
7709935500 wwwcolorchemcom
AMAPLASTreg DYES
IR ABSORBERS
NEOLORTM PIGMENTS
UVAPLASTTM UV ABSORBERS
SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
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James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
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Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
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Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
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Steve Esker 614shy679shy4677
Paramount Colors Inc
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Mark Freshwater
Lansco Colors
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Clariant Corp
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ComAssist
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DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
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AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
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Color Science Consultancy
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Ticona
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Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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KRRKOWTAATHHA
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SPE CAD NEWS Fall 2012 page 10 wwwspecadorg
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page 11
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SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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Clariant Corporation
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Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
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Uniform Color
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AlanBodixxxPolyonecom
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Ferro Corporation
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A Schulman Inc
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Clariant Corp
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Uniform Color
tlphillipsxxxuniformcolorcom
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Tronox LLC
thomasrachalxxxtronoxcom
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BASF Corporation
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Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
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608shy246shy2600
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page 11
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BTitanium dioxide
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SPE CAD NEWS Fall 2012 page 11 wwwspecadorg
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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rs
advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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LTL Color CompoundersInc
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Chair-Elect
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Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
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Sun Chemical Corporation
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Councilor
Sandra Davis 302shy999shy2540
DuPont
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Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
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Paramount Colors Inc
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Lansco Colors
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Clariant Corp
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DuPont
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Ticona
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SpectroTechs Color Solutions
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AlanBodixxxPolyonecom
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halbuttonxxxakrochemcom
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Color Science Consultancy
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FrankxxxPigmentscom
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Ferro Corporation
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A Schulman Inc
sharyl_reidxxxusaschulmancom
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A Schulman Inc
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EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
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jchemiexxxaolcom
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Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
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rtodescoxxxinternationalcom
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210 Lancaster Street
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203shy775shy0471 phone
customerservicexxx4speorg
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519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
SPE CAD NEWS Fall 2012 page 12 wwwspecadorg
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The filter pressure Test din en 13900-5 for pigmentmasterbatch dispersions
author roger reinicker basf Corporation newport de 19804
Abstract DIN EN13900-5 is used to measure the degree of dispersion of pigments or other additives contained in a poly-meric matrix If the preparation of the pigment masterbatch is well defined and in addition emphasizes pigment wettingover pigment shear and aggressive pigment development it is also useful for giving neat or powder pigments a passfailon dispersion quality While the DIN or EN standard test has been around for about five years it has not been univer-sally adopted by some segments of industry in the NAFTA region This paper will examine the history and developmentof the test and compare it to more traditional tests used in the US masterbatch industry including some correlation databetween the new test and older methods Suggestions for potential improvements will also be offered
introduction The proper use of pigments in plastics necessitates achieving a qualitydispersion of the particulates thus to achieve a number of goals Reproducible color results Good economics Good physical appearance (lack of specks streaks and other defects) Efficiency in spinning of fine fibers or blowing of films Physical integrity of those plastics which may fail key performance criteria if there are point defects in the matrix
For example some plastic constructions may be pressurized others need to have good impact strength
In order to achieve success for the latter two items those who manufacture and use pigments have instituted various teststo insure that the pigments can be properly dispersed or are indeed properly dispersed in masterbatches and concen-trates Among these tests are the pressure test also know as the screen test or filter value test
pressure Test history and development Prior to the middle of the last decade there was no standard for this test companies developed their own tests based uponinternal criteria or customer demands All pressure tests utilize the basic principle from fluid mechanics of the modifiedBernoulli equation which predicts for incompressible fluids a rise in head loss or pressure drop with decreasing area offlow There has existed an ASTM filter test for plastics but the author is not aware of any specific use by the masterbatchindustry ASTM D3218-07 section 17 describes a test for insuring that polypropylene resins used in monofilament spin-ning are clean enough for efficient use by predicting filter life The main thrust of this test being polypropylene resins andnot particulate dispersions and also the large quantities of material required made this test not really applicable for par-ticle or pigment dispersionsFilter tests that were developed locally in the USA often employed a simple setup of a singlescrew extruder (often 1rdquo diameter) screen pack and breaker plate As in ASTM D3218 use of a melt pump was optional
table 1 Some details of ASTM D3218 section 17 filter test
reason for use screening molten PP resinsextruder 1 inch to 25 inch (25 shy 64 mm)
melt or metering pump optional shy any type
screens composition 304 or 316 stainless steel
screens diameter 2235 inches (567 mm)
screens mesh in order 32550 32550 200X1200 DTW50 32550
breaker plate (screen holder) specified 31 hole 0125 inch diameter in concentric circles
volume of material 025 x ratehr plus 30 pounds
temperature 2 65˚C
throughput not specified
max pressure 5000 psig or 345Mpa
procedure purge 15 minutes then run 30 pounds
measure of rate of filter increase megapascals per kg or psi per pound
SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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LTL Color CompoundersInc
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Chair-Elect
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Clariant Corporation
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Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
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Councilor
Sandra Davis 302shy999shy2540
DuPont
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Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
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Mark Freshwater
Lansco Colors
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Clariant Corp
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ComAssist
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DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
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SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
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AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
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A Schulman Inc
sharyl_reidxxxusaschulmancom
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A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
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jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
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210 Lancaster Street
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203shy775shy0471 phone
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SPE CAD NEWS Fall 2012 page 13 wwwspecadorg
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Screen packs often used a 325 square mesh screen (44 micron) as the critical screen to collect oversize particles but laterthe 165 x 1400 Dutch twill weave became popular Temperatures quantity of material used loading of the pigment spec-ifications etc varied widely Around 2004 the DIN EN13900-51 test became available beginning in Europe but basedon existing tests currently done then in Europe but also in the USA It must be noted from the start that the standardsays absolutely nothing about the creation of the pigment concentrate itself that undergoes test In the examples it refersto 40 loaded dispersions but not how to make them this is beyond the scope of the standard It was written especial-ly for chromatic and achromatic pigments in thermoplastic carriers that have application in extrusion and meltspinningWhat the standard does offer is a method for testing such concentrates that has a reasonable chance of reproducibilityfrom testing lab to testing lab
screen TypesThe standard specifies three different types of screen packs The screen pack is the critical piece of the entire apparatusThe draft standard does not indicate a preference for any of the screen types nor does it suggest a specification on the risein pressure over the course of the test A sealing ring is required for the screen Typically this is an aluminum border thatserves as a sealing surface top and bottom and prevents leakage of polymer around the screen The practice in the indus-try of using loose individual screens without an encompassing border should be discouraged as well as the practice ofusing an automatic screen changer which then implies that the only sealing force is the pressuregenerated during the testScreens in increasing order of fineness
Screen-pack type 1 a two layer screen pack with the key screen being a 615108Screen-pack type 2 a two layer screen pack with the key screen being 615132Screen-pack type 3 a three layer screen pack with the key screen being 1651400
Table 2 shows the screen types and wire diameters Screens must conform to ldquoISO 9044 Industrial woven wire clothndashTechnical requirements and testingrdquo Table 3 gives other important parameters
continued from page 12
1 The standard is available from several sources ANSI httpwebstoreansiorgRecordDetailaspxsku=DIN+EN+13900-53A2005lahblah Or BeuthhttpwwwbeuthdecnJ5BB90E7033486711AE134B5B72EE28684bGV2ZWw9dHBsLUxhbmdhbnplaWdlJnNtb2lkPTc2NzE4MTEzJmxhbmd1YWdlaWQ9ZW4html
TyPE 1 35 ndash 38 25
screen 1 reverse plain Dutch weave 615108 0042 mm 014 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 2 23 ndash 26 20
screen 1 reverse plain Dutch weave 615132 0042 mm 013 mm
screen 2 square mesh plain weave 063 mm 04 mm
TyPE 3 16 ndash 18 10
screen 1 twilled Dutch weave 1651400 0071 mm 0040 mm
screen 2 square mesh plain weave 025 mm 016 mm
screen 3 square mesh plain weave 063 mm 040 mm
estimates
TyPE CONSTRuCTION amp APERTuRE wIdTH wIRE 1 wIRE 2
AbSOLuTE
RETENTION
mICRONS
NOmINAL
RETENTION
mICRONS
TAbLE 2
continued on page 14
SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
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Clariant Corporation
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Silberline Manufacturing Co Inc
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dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
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EMD Chemicals
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Americhem Corporation
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Clariant Corp
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Uniform Color
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Tronox LLC
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BASF Corporation
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Techmer PM LLC
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Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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CDs PerfectBinding
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608shy246shy2600
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SPE CAD NEWS Fall 2012 page 14 wwwspecadorg
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TAbLE 3
continued from page 13
PARAmETER TEST STANdARd ENGLISH uNIT
single screw extruder diameter (D) 19mm to 30 mm 075 inch to 118 inchlength of screw (L) 20LD to 30LD 20LD to 30LDpressure at melt pump 30 to 60 bar 435 to 870 psigpressure maximum achromatic colorants 350 bar 5075 psigpressure maximum chromatic colorants 100 bar 1450 psigoutside filter diameter 338 mm 133 inchexposed filter area 897 cm2 139 in2throughput rate 50 to 60 cm3min 305 to 366 in3minscreen wire diameter 0042 mm 17 milscreen wire diameter 0071 mm 28 milscreen wire diameter 013 mm 51 milscreen wire diameter 014 mm 55 milscreen wire diameter 016 mm 63 milscreen wire diameter 040 mm 157 mil
The throughput rate is probably better understood in the context of the amount of polypropylene in gramsper minute that this volume represents roughly 40 to 55 grams per minute
extrusion apparatus The apparatus for running a filter test is shown in Figure 1 The typical one-inch diameter single screw extruder with a241 or 301 LD is perfectly acceptable for running the test The standard however requires a melt (or gear) pump witha feed back control loop to the extruder drive to maintain a constant pressure of the melt at the gear pump This feedbackloop insures a constant volumetric flow through the pump and through the screen If the melt pump is eliminated fromthe system a uniform volumetric flow rate is unlikely to be maintained during the test since single screw extruders pumpless at constant rpm as pressure at the end of the barrel increases and in addition the mass flow becomes pulsatingSystems with feed back loops to melt pumps are common on laboratory fiber spinning lines and it is likely that such linescould easily be adapted to perform the test with a minimum of cost and re-tooling
breaker plate A specific breaker plate design with nineteen holes is prescribed The breaker plate also has an influence on the degree ofbackpressure in the system which in turn affects the shear given to the pigment under process Hence deviating fromthe exact breaker plate design given in the draft standard is not a good idea just as is deviating from the described screenpacks must be avoided
Test materials DIN EN13900-5 does not dictate the type of polymer to be used in the test either as the ldquobasic test polymerrdquo or as the car-rier for the pigment under test Polypropylene is the most common carrier in our experience and this is the polymer thatwas used for development of the standard In the industry polypropylene is sometimes used as the pigment concentratecarrier for final application in other polymers and in BASFrsquos laboratory nylon concentrates are frequently pressure test-ed in polypropylene Appropriate processing temperatures must be selected in the case of mismatched polymers In our
laboratory 230 0C (4460F) is a convenient processing temperature for polypropylene and 2650C (5090F) for nylon 6 con-centrates It is prudent to specify that the basic test polymer undergo its own filter value test perhaps with the finestscreen available (165 x 1400) and to place a very low specification on the result It is not difficult to find polypropylene thathas a very low filter value For other polymers the development of char must be carefully monitored and appropriate sta-bilization selected to prevent char formation
continued on page 15
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
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ivis
ion
of
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es
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yo
fP
la
sT
iCs
en
gin
ee
rs
CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
SPE CAD NEWS Fall 2012 page 15 wwwspecadorg
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Under the standard the pure pigment content and total throughput weight is set for two different mixtures
Mixture one is set for 25 pure pigment total mixture weight including the basic test polymer is 200 grams andthe recommendation is that this is for color (chromatic) pigments
Mixture two is set at 80 pure pigment total mixture weight including test polymer is 1000 grams and the rec-ommendation is that this is for black and white pigments The larger volume for blacks (assume carbon black) andwhites (assume titanium dioxide) is appropriate for several reasons higher density for the white the need for blacksand whites in some applications to have very long runs (for example in film) and finally the nature of some carbonblacks to suffer from undispersible grit in very low concentrations
The larger volume for blacks (assume carbon black) and whites (assume titanium dioxide) is appropriate for several rea-sons higher density for the white the need for blacks and whites in some applications to have very long runs (for examplein film) and finally the nature of some carbon blacks to suffer from undispersible grit in very low concentrations
Given the volumetric flow rate this implies that mixture one will run only about four minutes through the screen and mix-ture two about twenty minutes This seems adequate for the blacks and whites but somewhat short of the usual process-ing time and amount of pigment processed for organic chromatic pigments in the heretofore-practiced methods in theUnited States Our lab for example has been running about fifty grams of pigment in our version of this test for over twen-ty years Larger mixture amounts are certainly allowed by the standard if agreed upon between interested parties but in nocase should the total pigment processed be less than 50 grams
interpretation of results Running the test involves placing a new screen for each test in the apparatus that has been pre-heated to an appropriatetemperature for the polymer purging with the test polymer adding and processing the test mixture (mixture 1 or mixture 2)until it runs out then purging again with the basic test polymer This will generate a pressure response over time for thepressure transducer marked PT in Figure 2 In the hypothetical chart TS and TP are the points where respectively thetest mixture and the purge mixture are added It is highly desirable that the pressure trace be plotted on a recorder chartor digitally although this is not required by the standard Figure 3 is a photomicrograph of a test screen with captured pig-ment particles
Note that the pressure trace may show a pressure decrease as the basic test polymer is replaced with the test mixture thisresponse is typical for a well dispersed chromatic pigment in an olefin carrier under test in polypropylene since these olefinmasterbatches frequently contain a low melting component such as a wax As the test mixture runs through the screenoversize particles are caught on the screen reducing the available flow area for the polymer Since volume flow rate is keptconstant by the melt pump a pressure rise occurs at PT (again due to the Bernoulli relationship) After the test mixture hasrun out purge material of 100 grams of the basic test polymer is run through the screen after which the test is completeThe pressure response of the purge material is usually a decline as some of the particles caught on the screen become bro-ken down with time and pass through the screen thus slightly increasing the area available for polymer flow
The test result is indicated in the figure as Pmax- Ps Again the standard sets no specification on what constitutes a goodor bad result
Test report The standard requires that the complete test report for a given concentrate contain a reference to DINEN13900-5 detailsabout the basic test polymer the mixture tested type of screen pack used melt temperature and the volume throughputas well as of course the final result (the pressure rise in bar per gram of pigment) and any notes about deviations from thestandard method This completeness cannot be underemphasized given the latitude of polymers mixtures and screentypes allowed by the standard a given test value (for example 5 bargram) is meaningless without proper understandingof the other parameters
continued from page 14
continued on page 16
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
Pu
bl
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ed
by
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eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
SPE CAD NEWS Fall 2012 page 16 wwwspecadorg
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of
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fP
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advantages of the en13900-5 test The new protocol has several good features and some advantages over locally developed tests
The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test is short running only five minutes with color versus many industry tests that run 30 minutes or more The test consumes much smaller amounts of concentrate or pigment allowing better efficiency when dealing
with developmental samples The test employs single screw technology already utilized for this test by much of the industry A melt pump is required to insure constant flow through the screen Tests that utilize single screws without melt
pumps lose flow rate as the pressure rises and also have differential shear throughout the test Critical parameters such as filter screen configuration and breaker plate are defined The screen is bordered and locked into place to insure no bypass of material The test allows for three different screen types and all three are defined
industry response So some seven years after introduction has this standard test been accepted in the US industry and how has it faredagainst existing tests A very unscientific survey conducted by the author found that there has been some adoption of thenew test especially for newly created dispersions and export situations but also a continued use of older tests and somesuspicion that the new test is not satisfactory for some applications
Overall the test seems popular with pigment producers particularly those who produce in Europe but also may produceat locations across the globe This makes good sense in that uniformity of testing within a company allows useful compar-isons of production capability The chief drawback of employing DINEN 13900-5 in this manner is that the test does notspecify how the pigment is to be dispersed prior to the test hence there also needs to be a strong emphasis on uniformityof the primary dispersion step Here is where a comparison of intercompany pigment test results will present a challengesince different companies may claim good pigment dispersion based on a good number from the test without mentioningthe pigment dispersion protocol The subject test is not a test for pigments the test is for a pigment dispersion Let thebuyer beware
For concentrate houses use of the 13900-5 test makes even better sense Let their dispersion process be whatever it is pro-prietary or fully disclosed but a number from the standardized filter value test should allow inter-company comparisonsthat make sense Surprisingly this is where adoption of the test has lagged
US producers continue to rely on a variety of pressure or filter tests Some of this is understandable since specificationsdeveloped between masterbatch supplier and masterbatch user can be long-standing and once implemented and accepteddifficult to displace Also the new test may require capital investment from the one or two machinery vendors that havespecialized in machines matching the requirements of the DINEN test Some masterbatch producers have found it ben-eficial to adopt certain aspects of the test particularly the melt pump at the end of the extruder before the screen pack Thismelt pump isolates pressure build from the extruder and allows the extruder to operate under uniform conditions through-out the test Without this isolation as mentioned shear conditions would vary as the pressure increased
Another reason is mistrust of the new test since for some situations such as organic pigment dispersions it calls for as lit-tle as 5 grams of pigment to pass through the screen Locally developed tests in the US often called for 10 to 20 times asmuch pigment (there are exceptions) Strictly uniform sampling then is a necessity for this test with such a small amount ofsample The DINEN test does allow for larger quantities however and the author feels that a rise in bargram in adefined test is a much better specification than a pressure risein psig that lacks suitable reference and definition
continued from page 15
continued on page 17
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ion
of
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yo
fP
la
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iCs
en
gin
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SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
Pu
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ed
by
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ol
or
an
da
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ea
ra
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ed
ivis
ion
of
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es
oC
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yo
fP
la
sT
iCs
en
gin
ee
rs
SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
SPE CAD NEWS Fall 2012 page 17 wwwspecadorg
Comparison between one local test and din en13900-5 A number of commercial olefin based dispersions were obtained and run in two different filter value tests in the BASF plas-tics laboratory in Newport DE in order to establish a correlation between the older inhouse pressure test and the newDINEN13900-5 filter value test The ldquolocalrdquo in-house test used for more than 20 years employed a single screw extruderand either a 325-mesh screen2 for less critical applications or a 165 x 1400 screen for more critical fiber applications The
test used 1750 grams of nominal 12 MFI polypropylene polymer at 3 pigment loading and ran about 35 minutes at 510FThe same dispersions were then run on a Dr Collin filter value machine dedicated to the DINEN procedures Severalvariations of the DINEN test were run employing three types of screens and also for black and two inorganic pigmentsa higher loading of 80 and a longer run of 1000 grams of material versus 200 grams for the usual test
The sixteen test results are listed in Table 4 three tests were run on the 325 mesh screen and 13 on the finer 165x1400 screen(left side of table) Under the existing in-house test a rise of 800 psig or less over a 35-minute period was acceptable for the165 x 1400 screen (rates a pass if lt267 psigmin) and a rise of 75 psig was acceptable for the 325-mesh screen (rates a pass iflt25 psigmin) Somewhat more than half of these commercial dispersions did not pass this long-established test The cor-relation obtained with the DINEN test (right side of table) primarily the 108 x 615 Type 1 screen (absolute retention 32microns nominal 25 microns) was fair with some notable exceptions It appears that a value of 10 bargram or less on theType 1 screen is adequate comparing against the prior in-house test for the chromatic organic pigments This is in agree-ment with the developers of the DINEN test who suggested that such a value obtained on the Type 1 screen was indica-tive of a dispersion that was satisfactory for most critical applications
Correlation Using 10 barg as the passfail criterion for the new test it is possible to make a test to test comparison Therewere no false negatives comparing the DINEN test to the local test but there were six false positives meaning that thenew test passed six dispersions that would have been rejected by the older local test Does this lend some credence to thosesuspicious of the new test for not employing sufficient pigment passing through the screen
What could be the reasons for the false positives Machine to machine comparisons need to be understood The oldermachine in use for some time had a worn screw and barrel ran at lower viscosity (higher temperature) The newermachine presumably had tighter tolerances ran at higher viscosity (lower temperature) meaning more shear was impartedto the pigment dispersion See Table 4 for some other test comparisons It is expected then that marginal dispersionsmight appear ldquoimprovedrdquo on the DINEN test since the lower temperature higher viscosities and presumably tighter tol-erances would lead to more pigment aggregate breakdown Further the PY34 tests were suspect since polymer degrada-tion was noted during the local test possibly due to inadequate polymer stabilization at the higher temperature
2 Both the 325 mesh and the 165 x 1400 mesh screens contained within a pack of several screens with appropriate coarser backing screens to prevent deformity under high
pressures
Table 4 Correlation between local test and the DINEN test using commercialdispersions
In-house Pressure Rise Test
Pigment inthe conc
PressureRise in
psigTimemin
165X1400psimin
325 meshpsimin
PFStatus
Type 125
Type 180
Type 225
Type 325
corre-lation
Fail ifgt267 Fail if gt25 barg barg barg barg
1 PY93 40 35 1 Pass 045 032 091 OK2 PY95 10 35 0 Pass 032 OK3 PR144 35 35 1 Pass 045 091 082 OK4 PR214 0 35 00 Pass 018 OK5 PR202 840 715 117 Fail 18 17 60 80 OK6 PV19 830 3 277 Fail 30 OK7 PV19 120 15 80 Fail 15 OK8 PV23 120 35 3 Pass 045 OK9 PB151 150 25 60 Fail 086 NG
10 PB151 830 16 52 Fail 07 NG11 PB153 gt800 6 133 Fail 20 OK12 PG7 830 2325 36 Fail 145 332 345 OK13 PBl7 860 252 34 Fail 045 050 10 NG14 PW6 840 303 28 Fail 009 018 05 05 NG15 PY34 800 11 73 Fail 027 036 NG16 PY34 800 6 133 Fail 036 NG
ISODIN EN13900-5
some decomposition noted during local test
Table 4Local test and the DINEN test as locally adapted
local test EN13900-5screw diameter
screw rpmscrew LD
screw amp barrel wearfeed rate
developed pressure variable bar
polymer
12 MFI PP
(unstabilized)40MFI PP pellettemperature
Given this experience it seems that all the factors that influence dispersion come into playwhen comparing tests done on two different testing devices To say that one test does notcorrelate with another without first understanding the details of both tests is to avoid the duediligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers by reporting uniformlyFPV results in bar per gram of pigment on standardized equipment
Table 4 Correlation between local test and the DINEN test using commercial dispersions
continued from page 15
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
Pu
bl
ish
ed
by
Th
eC
ol
or
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da
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ion
of
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SPE CAD NEWS Fall 2012 page 18 wwwspecadorg
Given this experience it seems that all the factors that influence dispersion come into play when comparing tests done ontwo different testing devices To say that one test does not correlate with another without first understanding the detailsof both tests is to avoid the due diligence required to establish a correlation Therefore in principle it should be possible tocorrelate older tests to newer ones and provide benefit to customers byreporting uniformly FPV results in bar per gramof pigment on standardized equipment
Still there are areas where the DINEN13900-5 test would have to be severely modified to be useful Some of these situa-tions approach the conditions of the ASTM test mentioned at the beginning of this paper For situations of creating effi-ciency in very long runs (eg one or two weeks of continuous production) on fiber or film lines it really is necessary to runquite large quantities of polymer through the machine to look at very dilute concentrations of additives or particulates orpolymers that may produce gels The latitude to do so however is available within the test standard
ConclusionsThe following quote is taken from a European publication soon after the test was established3 the authors were fromBASF AG Ciba Specialty Chemicals and Dr Collin GmbH
ldquoThe new standard allows a global harmonization of filter test methods and creates a common denominator forpartners in business transactions Used as part of quality control of colorants and concentrates suppliers of well-dispersed concentrates can now use this method to establish a leading edge over competitors
The general availability of a normative standard will significantly affect the manufacture of testing equipment andincrease the existing pressure on the dispersion quality of colorants and concentrates
Moreover The EN13800-5 provides an ideal foundation for establishing filter tests forother applications such as tests for additives fillers and polymer materialsrdquo
The mechanics of the DINEN test are robust It is the authorrsquos opinion that older pressure tests can be adopted to usethe newer equipment with a melt pump for probable advantages in reproducibility and certainly to aid in uniform com-munication and understanding within the industry In the data gathered for this paper a filter pressure value of 10bargram correlated roughly with a long-established passfail in a local dispersion test
TAbLE 4 Local test and the DINEN test as locally adapted
LOCAL TEST EN13900-5
screw diameter 1 (254mm) 20 mm
screw rpm 75 102shy105
screw LD 25 25
screw amp barrel wear unknown (old) new condition
feed rate 44gmin (varies) 40 gmin
developed pressure variable constant at 435 bar
polymer 12 MFI PP homopolymer flake 40MFI PP pellet
(unstabilized)
temperature 5100F (2650C) 4460F (2300C)
3Dr Volker Koumlnigstein Hans-Peter Meyer and Dr-Ing Gunter Mullerferli Kunstoffe plast Europe 102004
continued from page 17
continued on page 19
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SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
SPE CAD NEWS Fall 2012 page 19 wwwspecadorg
FIGuRE 1 Filter Value Apparatus
FIGuRE 2 Fiber Value Pressure Trace
FIGuRE 3
Test screen with
pigment particles
PigmentConcentrate
BreakerPlate
meltPump
screen Pack
Feedback Loopto extruder
Drive
extruder
to
recorder
Pre
ssu
re
bar
Time
Pmax
Pmax - P
Ps
Ts Tp
PT
PE
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS
Color amp appearanCe division board of direCTors
OFFICERSChairman
James Figaniak 215shy736shy1126
LTL Color CompoundersInc
jimfiganiakxxxltlcolorcom
Chair-Elect
Ann Smeltzer 412shy298shy4373
Clariant Corporation
annsmeltzerxxxclariantcom
Finance Chair
Betty Puckerin 812shy466shy9828
Ampacet Corporation
Bettypuckerinxxxampacetcom
Immediate Past Chairman
Scott Heitzman 513shy681shy5950
Sun Chemical Corporation
scottheitzmanxxxsunchemicalcom
Councilor
Sandra Davis 302shy999shy2540
DuPont
sandrapdavisxxxusadupontcom
Treasurer
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
Secretary
Jeff Drusda 570shy668shy8321
Silberline Manufacturing Co Inc
drusdajxxxsilberlinecom
dIRECTORS until 2014Sharon Ehr 616shy494shy7577
Uniform Color
sehrxxxuniformcolorcom
Steve Esker 614shy679shy4677
Paramount Colors Inc
steveeskerxxxhotmailcom
Mark Freshwater
Lansco Colors
markxxxpigmentscom
Steve Goldstein 508shy829shy6321
Clariant Corp
stevengoldsteinxxxclariantcom
Larry Nitardy 423shy312shy3439
ComAssist
lnitardyxxxaolcom
Jamie Przybylski 419shy559shy2459
Terra Community College
jprzybylskixxxterraedu
Austin Reid 228shy255shy2362
DuPont
Austinhreidshyjrxxxusadupontcom
Mark Tyler 859shy372shy3221
Ticona
marktylerxxxticonacom
dIRECTORS until 2015Earl Balthazar 817shy719shy0224
SpectroTechs Color Solutions
ebalthazarxxxtxrrcom
Alan Bodi 419shy356shy7308
PolyOne
AlanBodixxxPolyonecom
Hal Button 330shy535shy2100
Akrochem
halbuttonxxxakrochemcom
Jack Ladson 215shy369shy5005
Color Science Consultancy
jackladsonxxxverizonnet
Frank Lavieri 401shy461shy4100
Lansco Colors
FrankxxxPigmentscom
Bruce Mulholland 859shy525shy4756
Ticona
brucemulhollandxxxticonacom
George Rangos 724shy229shy5371
Ferro Corporation
rangosgxxxferrocom
Sharyl Reid 864shy968shy2426
A Schulman Inc
sharyl_reidxxxusaschulmancom
Cheryl Treat 419shy483shy1063
A Schulman Inc
Cheryl_treatxxxusaschulmancom
dIRECTORS until 2013Scott Aumann 912shy210shy0175
EMD Chemicals
scottaumannxxxmerckgroupcom
Doreen Becker 914shy772shy5580
Americhem Corporation
dbeckerxxxAmerichemcom
Paul Bykowski 219shy331shy6981
Finos LLC
pbykowskixxxfrontiernet
Brenda Mullins 678shy237shy2975
Clariant Corp
Brendamullinsxxxclariantcom
Tracy Phillips 770shy995shy0887
Uniform Color
tlphillipsxxxuniformcolorcom
Tom Rachal 405shy775shy5014
Tronox LLC
thomasrachalxxxtronoxcom
Roger Reinicker 302shy992shy1252
BASF Corporation
rogerreinickerxxxbasfcom
Johnny Suthers 423shy229shy4258
jchemiexxxaolcom
Brian West 865shy457shy6700
Techmer PM LLC
bwestxxxtechmerpmcom
Please note The email addresses above contain xxx which should be ignored when actually emailing
The purpose of the triple ldquoxrdquo is to render the automated spam grabbers useless
Pu
bl
ish
ed
by
Th
eC
ol
or
an
da
PP
ea
ra
nC
ed
ivis
ion
of
Th
es
oC
ieT
yo
fP
la
sT
iCs
en
gin
ee
rs
CDs PerfectBinding
OmniPress
608shy246shy2600
twagnerxxxomnipresscom
ACE Chair Roberto Todesco
rtodescoxxxinternationalcom
National Plastics Center
Museum amp Collections Director
Marianne Chalifoux
210 Lancaster Street
Leominster MA 01453
SPE Headquarters
203shy775shy0471 phone
customerservicexxx4speorg
CAD Newsletter Publication
Peacock Graphics Inc
847shy341shy4066
peacockgfxaolcom
WebSite HostDesigner
Becky and Jeremy Hodge
519shy824shy3434
infoxxxeshyxyncom
OTHER USEFUL CONTACTS