07/19/95 09:50 DOCU11ENTENGINEERIN!3C.O.. INC. .; 5~5 892 1159 NW,ll:l!:l 1"1.::1"'~{!dl,

! :

41I~ D"lgnltlon: 8 458 .. 94 ,

Cl,""~... I -

J .. :.AMlIllIc:AHIClClITV1'01' 'l'!lnt.O AI«) MA~AI.I : '

111. fIIaee Sl f'1I18d81pIllt,I"AI.,C13"'U,11II8' 110111IPII AM..., IIooh' AtN IIta,..j.",., °"';'18111 AI N ".

It 1lll11io.1ItIillIh. 'IIIf.1I .""'II\IcIIIIft.. 111"""'11111"" ...", 10...:. ,c.;~.Jr' (

St.ndard Specification 'orElectrodeposlted Coatings of Copper Plus NickelPlusChromiumand NIckelPlusChromium1

Tb.. 8Iund.rd Is iuucd ul'd~r Ihi flud GealinallOIl a ~S61,hi number1"""01118\.1)'Ibllillllln, Ibt CltII",allOlllnClhlllCSth' ~r Drorll'n.' Idoplioll or. in ,tit ca. or "..Ision. Ih. yeit 6( lu, revllinn.It. IIU",.' IIIpaNn'blllft MIl III' ,lIr arloft nlppro".,I, It.II/PO"""P' ...il.n hI '"dlcl4,. III ,di'8ri.1 thllna. Ii,," ,he Iii' ""lllon or tCI,ptO,/II., '

J. Scope" J This specincatlon covers reQuircmenu(ar Slveral

typesand arudes of eJl!ctrodepo~itedcopper plus nickel plus~hromium or nickel plus chromium coatin&t$on'teel,nickelph~5chromium coatin.- on copper and copper aUo)l',andC'opperP'UI nickel plus f:hrontillm eoatinp onzinc8J10)'1torapplicationl whereboth appearanceand. protecllan of thebasil me&lllllinst carro.ion are imponant. Five artdes ofcoltin,s .ra pravldedto correspondwith the set'Yicecondi-tlonl underwhichneh is eJtpccted to provide sad.factoryperformance:'namely. extended "cry severe,very severe,Ryer,.modetate, ,nd mild. Dennidon~ and typical eumplesof ,hlle leJ'\lict conditions are pro\'ldltd in Appendi~XI.

1.2 The rullowift&huards Clveatpenain. only tDthe teatmothods'ponions. Append;"..Xl, X3. and X4. or thisspecification: This s'QltdtJ,d dots """purpOrt to addre:u d'i (Jjitl,/iIJI CQn(~rnl. if alf)'. tl$S(Jcf4ted with iu wcf. II is thertJpOltilbi/ilJ' (Jf the JlICf ()f this IltJ.nda,d 10 ellfJblish fJppro-prill" stlltt.\' I2nd hefl/th prattle,.s tJnd de"",,;n, the applica.bility 0/ r~t~l/tllO"J'limiUll;()n.sprlfJr tQ uSt.

Non I-The tSO stand_rd&1436&ftd 145' are no! requir.tI\cntlbutun b; rcf8l',nctd,rot additionallnrormatiOIl.

2. Refcrtnc:o(1Document~

2.1 ASTM Stflndllras;8 11,. rCSt Method ror Sal,t Spray (Faa) TOitina2B 183Praeticcror P,reparationbf Low-CarbonSteelrar

ElecuL~Ialina' .B 242 P"'t;tice for PrepatutitJn of Hip-Carbon $\011ror

ElectrapJatina'B 252 Practiceror '~eparalion of Zinc:AllOYDie CUtin..

for EleetropJatina and Conver'ion Coatinp', 8 281 Prac1,jcefal' Preparauon of Copper and Copper base

Alla~'1for EJec:uoplatlnaand Conversion Coatings'B 287 Method of Acetic:Aeid.Sal\ Spra)'.(Foa) Tesung. '.B 320 Prattice, fbr Jlrepl\ration ot Iron CUtin.. ror

EleetroplBtinA'3B 368 Method for Copper-Acceterated Acetic!Acid-Salt

Spray(Fal) TcsUna',S 380Methodof Corro.lon Tc.th\1of DecorativeEleetro.

pla\edeoltinas by tht: Cl)I'1'QdkoteProcedur.'

I Thil Iptclfia.lioll il unlltr lilt Jvri84/CIID"of ASTMComlllineeB.8 onMtullic ""tllnOlplllc CO&tin81Ind f8 1111"j,., IIIIOnll"lIIl~ or Ivbeoml'll'""IOLO) 011DteortllYt COIIIIII',Nlcklf. OI'Ol'llilllll, I"d Nitk,loChromlloll'll COI'.11\81.

tV""'1 Idilioll .~,tO..c.cI Ma,cll I.. 1994. Publlslled Mo, 1994. Oniinill~Plllali"',I1... .Sf. U. w, "'twiO",' ~4i,io" 1\45. - 9311.

. "'It'/ifli .,101; qf .tSrM S'lfnda,tI,.. YOI03.0~.

. '''''It/al S...& rl( .1.'1'101 .~la"Jfltfl.r. Vol 02.0~." Dlaro/niny.,I-Sa 11/116AItIl'HlIIJI)(JJ;,1 A5"1'M$I...IIII.,dy.VOl0).02.

p'd

B487 T.11MethodI'or M.alufement of Metal and OltideCoatlnsThlekn*C8 by MicroscopIcsl£uminatlon oraCrollSoction' .

8 499 Teat Method (or Me.uremtat of Coadn. Thi,k.. nO&8by theMaane\icMethod:NOftllllllftoticCo.t.iltll

on Ma.netic Jnstt; M,tallI'a 504Test Method fbr Mcu~rnmlSln uf Thickn/:ss of

Metallic Coat'n.. by the CoulomlJlric:Method'8 530 T.lt Me\hod for Mouurtmont of Coatins Tbi~lc.

neuee by &heMapede Memed: I!lecirodeposi~ NIckelCoatln.. Oft Mnlnetlc aDd Nonml8netic SubsltttesJ

B 537Pra!rticcfor Ratin, of Elt.ctroplatedPanels Sub-jectedto AtmollphericExposurel '

14554Guidefor M~urcJ!tent of 1'h.lclcneuof MeWllcCOltln.. on Nonn1CtaJllcSubstrate,' ,

B 568 Tut Method ror Mellurement of Coa\ina Thick-nell by X-Ray Spcunrometry3 .

B 571 Tesl Methacil for AdhtlioJl ot MehllJi~Coati"..'e 602TeAtMethodfot AttributeSlamplinlJaf Metallic:and

Jnorpnic Coati11&1:1'IS659 Ouldo ror MeBSurin~Thickneas of Metallic and

loarpnlc CoatinpJ ,

B 691Quid! (orSelectionor SampllnaPIanofor h,.pee:.110n of £I,elrodeposited Metallic: aDd InorpnleCoatinga) ,

a 762 Mtthod 01'VariablesSampLinlof M.ta11i~andlnol'pnlc COAdlllpJ

a 764 Method tor SimultaneousThicknessand Electro-chemicalPotenualDetermination!)rhldividuallayers'n Multilay.r NicklslD.po.h (STEP Te:ln)3 j " ',~

D 1193 Speclncationtor a.a,.nt Wa1er' .D39S' PractJ=(or C.ommerctaJPj&cka&!ul\'1:50 Pra~llcesfor Apparatus, R~lelllll, and Safety'Pre-

cautionstor Chemica! Analyaiaelt Meulls'2.2 ISO StaMQ,ds:JSO1456M.callic cOtunas-ElIIIC1rod,potijtedcoadnpof

nickel plus chromhlM and ot copper 1)lusnickel pluschromium'

ISO I." Metallic lcoatinss-Electroplatedcoati"r ofcopperplus nickel jpJuachromium 'iirtln or,lteel

~C '

3. T.rmlnOI~IJ. Che ~ /3.1 Dt/iIflIiD".. I17fTes V~ D

" J(jll eqrch. ""'ltIlIl Sault 01ASTM ,f//lllfit/fl/"Vol 11.01, lYe. 9 19.ra'/:'. """lUll&4OIt0/A$TH.'ftlltlj.,I,.Volls,ot. LI vle~ oJ,A"nUM8DO~ ~ tt&T",,Tttmft,4"VOl0).05. "I/p ed /:) ,

. ,4".illl_l,1i,I'IIIn"",aU8Mlllllldafd.Cttillllllhti'/i{ll~ drfjttll1l11.(lelltVII20, Swl\q,IIIId. ,""fJFch.

.."

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6S11-268S0S N3A31S 'l'~21:21 S6. 61 lnr--- --- -~-------

217/19/95 09:51 DOC\J1'1EtiTENGINEERIN~ CO. I INC. ~ 505 892 1159 ~J.1S6 pa~3/012

SUMMa" of tile Aequlram."la lor Double- ",II T"pl.-La~~ HI.lctl C~.tII\O'fIIlllIII811 AtltiiYiiOTOj;NICI(1t Tr\;;;'".... _.~Doubl&-l.AJ8IP- ftlplioL&ytt

0l1l8I'" 81l1litnlf01",,11-;~eo. -'5o4Di

Jli101-=:lDI1II0te40

411}t 8 456

TAIL! 1

I.'~" Trill 01 NIC'l8I I_'ie 1I0IIgI,lon .111111' Coftt8ll'

...-

cUo.""..">0." 11'1""~O,O.."'In'NOI.I'

BoIIOlllMICSGllilllllihaalJllU')

TOil"'1T~ M.~ .. a.. ~~ XI

ACopperWIdline:,lAMlr."1 .". tfttIt a_I.. 'or NOI'I ., aM .. .. Seotlon e.

3.1.1 J/",I/II:,.1I'$uqalu thollsurflcunormallyvisible(direc\Jyor byrcnecdon)thatareessentialto theappearanceor .ervfceabllltyof the anicle when 811CmbledIn normalposition:or that can belthe sourceor c:orrosionproductslhatdefice visible sul'f8CC$ou the assembledarticle. Whennec:elllry,the II.nlOcantsurracesshall be speeinedby thepurchuer and shall beIndicatedon the drawinp of the parts.or by the pravilioft of lultabl)l markedsample..

4. ct..,U1car1oft

4.1 FIvearaclol orcoatinas desiaoatod by service condition, ftumben and ..v.tI! types of coetin..dcO~edbyclasslfica.tion numberaatecovuedby thi. speeincation.

4.2 Smlt, COlldillDnNumb":4.2.1 The 8trvlce condition numb.rindicatel the ..verity

of ejtpo$ure ror which the gradeor cOltlnaII Intended: ,

SC j extended .eycr~ $CJ'\tiecsC 4 very.,vert Hrvicc,'SC J "VIr. .'rYiCt,SC 2 modentf. Ilf\llce.andSC 1 mild service.4.2.2 Typical serviClcondition. for which the varioul

servicecondition number! Ife appropriate are Jiven inAppendix X I.

4.3 Comi", Claslijlc:atiQfINumb,r- The coAtil\8clwin.cationnumbereomprtses:

4.3.1 The cliemlcal symbolrorthebui. meJaI(orfortheprincipIImew It.n aUoy)~nowedby . .Iashmark.

".3.2 The chemlcals)'mbolror copper(Cu)(If capporIsU&~d). ' ,

4.1.1 A num~r indicatln.theminhDumthiclenessof thecoppercoalinain micrometret(U'copper il used),

4.3.4 A lower-cue letter designatlns tho t)'J)Cor co~perdeposit(ir Gopperil used) (se. 4." and 6.2.3),

4,3.5 The chernlcaJ uymbol ror nickel (Ni).4,3.6 A number indic:atlnathe I'I\h'limumthickneaaorIhe

nickel coalin" in mic:rurnetre.,4.1.7 A. lower~cuelete.rdelianatln.thotypt of nickel

dCPQlit(see 4.4 find 6.2.4),4.3.8 The cl\cmlcilsymbol rarchromium(Cr), and4.3.9 A lotter(or leuors)deaianatin.thetypoofchromham

, deposit and it. minimumthlckn... in micrometrCl(He 4.4and 6.~.5).

,~.4 $)Jmbo/Jji),E.qJtlls/nt CltUl(j1tmIDfI-Th.faUowln,.lowor-tase letten shall be used in c:OItln8c:laullic8tion

~ numbersto describetho ty. ot coatinil:. -duc:tlle tc)~I~t,dej:lOSltedr,orn.cid.t1fP8 bathsb -sinllt-1aye1 I\lOkcldeposited in the fbllY.brialucondition,. -dull or ltift\:-h"'ah. n~"cl rCQllirini pal:lhi... '0' &I-. tlil/

brisJuneu "

..

S'd

Steel-_71S

1D':'28" '0 0I,

d -doubt.. ortripl..I.~.rfliek~1~oalin&Sr -",1I11t (thilla, CCnYflllllollal)ehtomilolmme -mictOCllcltld chromhlmmJl-mlotQporo". chrornlum

4.5Exampl,qf'CDmpl",ClatlijlCtltiO"NumbtrJ-A coat.in. on Iteelcomprilin. I' j.Lmminimum(ductileacid)c:apperplus2' 11mminimum (duplex)nickelplul0.25~mminimum (mlc~racked) chromiumhu the (:Iaulftcatlonnumber: Fe/tu15a NI2Sd Cr mc (- 4.3 and 6.1 for.~pl.n.tion or Iymboll),

S. OrderinllnfoflDadolS,S.I When ordenq uUcl.. to b. electroplated in conform-

aneewith this standard, the puroha.ser shall IIlIItethe rol..lowing:

'.1.1 The!ASTM de$iSnAtionnumber of thl~ Stt\ndatd.,. '.2 EithertheclUllOcaUonn&&mberor &fteIpcctnccoat-

In, required (see4.3) D' the lubltrlle maceri.a1and thelOrvlt:e:conditio" "\lmbet denotiq the Beyerityof the conditionsitis required to wlthltlnd (lee 4.2). If ttte !IOl'Vlce~oncUtioftnumber is quoted alld not Ihe ellllint:ation nunlbet, themanufacturer '5 free to supply Iny or the tYp6!1of cO8llnasd..lan.ted by thl claasificationnloJmbel'llc:ot1'l!spcndin.to

TABL.!I NI.tl "lullCllremlumCoolIl\g' elt lta,lND'. 1-Au\IIt, 01. "" 1II'IIf1/ll1rlGlla1'Ultr't 18II)1\IImil'" wMUWIlI8

bII,IliII!a "y.'I""S dfllItIIlI6d by IJ'II c~..slftca'iatl nllmlj.,.. II'\w~~II'D 'UClutll cIwomillm .,. uli'factorY for SC 4 IIId ~C 3.

Non 2-Whtn pennllttCI till Ih. II\IfCNIIf, cop!* mill)' ~ Illed .. 811undercoal/Of ttk:ktl bII' It noC!tuGtlih..1aDIefar ."y wt 01 "'" IIlcMj Iftj,knest,pecllIed. If \l1li ~ 01 /!Oppel t. pCImIilttd, T.bIIt 3 till, 118ullOO10 oIal8in tho.am. ro.~1IOn..

Clt..IIIcI'1On NO." -- NIck81 1'1I1CICnIII.-1'111

'o/Nidd Crma ,;Fu/NI3$cfCt m~ 35F"/N~011Of r .0Fol"ll30c1Ct me 120PII/NI~OCIer mp 3DFClINI~OtCf, 30Ffl/NIIIOCrIl1O' 21"'/Nlllei Cr"'~ IIF./NMCJCt, 40II"NI~O.C,mo :10'II/NI:.OpCt~ 30'e/NI20110, r :tof:'JNII'~Cr1M l'Fefl'4l's.Cr 1'111 1.

Ie ,. Ft/NIIOI0/, 10- ~" WIIaIIa &dItit ..d" """" IIIr"'. """"'. Dnldtl/ IIU, D8IIID8ulllt8lf

lOt a b ftlckll or lor IN IriOn' lI,er 01 d 1IIokII.

.. p 014 lI!ellal m.y De lutI"IMICII« , /\ICk. In SInice CeIIcdllonHOt. I andI, ~ m: ormpClVotnIwl'ln'I8)'., lloIIIIcll\II8Grill, CftlanlumIn~ ~tJOftNO,I.

IIrvIot CIfIGIIiM No.

8CI

so'.

sea

8ca.

2

6S11-268 S0S N3A31S 'l'~ E1:21 S6. 61 lnr

~ ~------------

07/19/95 09:51 D~I8NT ENGINEERINGco., INC. ~ 505 892 11~~ NU.ll:Jb 1"'Id\O4/\Ql":

TABLE3 Copper Plul Nick., Plul Ch,omillmCoaUngl an Bt..,

StrvIceCondltiC1ll ClassIllCatlOnNo.. NIcktI'nIicknn.,~ . pmSO 1\ "1/Cu'S.N"t3Od Cr"'° 30

Fe/Cu'S. NI3OdCr mp 301ft/CutS.Ni25d Ct II'rC 25Fe/OU'S, Ni25dcr "'P 25FI/Cu,2a NJ2OdCf me 20F8lCu12aNi:lOOOr mil 20

.. WhIrl a d...11or lIalin 'InlShls required. ""buffed II nickel may be IUI'ISliluled

lor lhe bf"IGI'lIIIy8'( 01 IS nlck.l.

sc.

SC3

TABLE 4 CO"," PlUINick,1P/ul ChromiumtOltinlll' onZInc. . Alloy

NOTi-Result$01. tosl program iMitate Ihal8 ill lome dOl/i'll wl'lttl'l.t lhe

coating systems de.etj~CI 1'1,th8 dll8lificedon IIlImllerS itIVOlvingrogutar C/Uoomum 8f1Ut!SIICtC/YlorSC. InllSC3. .

ServfoeConCli.tOIiNo, Clessl'lcatiOn No.~~-SC S ZnlCuSNi35dCt I'IC

2n/CIIS N'135d Ci' nip

Nk1kel ThIcIInns. JIM.

3535

set

SC3

SC2'

so ,. %/l/Cu&Ni'DbCr, '0

" When . Gull Of sat!r'i FinIsh IS roqu.rOd. uJ\lIIIn~ p'niekelllllY 1:18lubSlit1.lttdfor b nICkel or for the brigMt llyer 01 d nlc:kel. .

. p or ISnlck.1 t"tI., be IWbslitutlCl'OI b nldwlln Service ConditlOtt NOs. 2 and1. and I'N:or mp dlromlun\ mly be substituted 'Of r tIIromlum In ServIcI Cl:lndluonNo.t.

the specified service conditionnumber,as JiveDin Tables2.,.3, 4, or ::i. On request, the manufacturer shaJJ infonn thepurch8JC!:ofthe classification number of the coating applied.

5.1.3 The appearance required, roOrexample,bright,dull,ot $Btin.Ahemalively, samples showina the required finishor RInge of fini$h shaJl be supplied or approved by thepurchaser.

S.I.4 The IIlanHicantsurfaces, to be indicated on drawingsof the parts. or by !.heprovision or suitably marked speci-

mens (see 3.1).S.1.S The poshions on significantsurfaces for rack or

contact marks, where such marks Ire unavoidable (see6.1.1).5.1.6 The f:ktent to which defects shall be tolerated on

nonsignificant surfaces.5.1.7 The ductility Ir other than the standard value (see

6.4).5.1.8 The utent of tolerable surface deterioration after

corrosion testlna (sct!6.6.3).5.1.9 SampUnamethods and acceptanc:eIcvels(see Sec.

\ion 7).

5.1.10 The minimum values orth~ electrochemical poten.tial differences between individual nickellayeJ5 as measured

9'd

-~-- -- ~

4t B 456

TABLE 5 NiCk.' Pltll t:hromlumCoaUng'"on r.ap~..' or COlllpt,Alloy, .

N~TI!-AItIICIu;h h dUliftcltlan ~ are lIuarnctcry for UCft cf iI8InCIiCIttel aervIcecandltICIn n\IIIW.. """'"' UIinQ n'iCJctRI=nI/n~. ~Iumare ;1I,.,.an~ IUperIor in ocrroCIIan ralltani:8 to 11'1010ua1118Ng!Aat ctIraINum.

SMvieeCct1dItlcnNo. Cl8WllcltIOnNo,A N1dc.,~nolll..

SC4 CU/N13OdOr, :SOC\I{NI25dCrme as .

CU/Nl2Sd Cr 1111) 25 .1SC3

SC;!O

SOl' Cu/Nl5bCr, 5--~~~ Whena dvllor otin tllllllllt ,_8d, Ullbutlacsp nlC*f' may beIUrJ8UIllt~

t« tI niCkel or for tI1t Clrlfht 11)'" 01 d n1cIcll.I Pcr G nIt:okeimay be subllIMeCI fer b nlckll h SIW\riCI8CcnditIan NoI. 2 and

1 ~ me 01'mp cI1rcml\llllMat t)fraubstllUI8d fDr t ct\romILnTI InService~IOIINo.t.

in accordance with Method B 764 within the limits Bivenin6.7. .

5.1.1J Adhesion Test-The adhe$lon test to be used (see6.3)..

6. Product Requirements6.1 VisualDdtcu:6.1.J The sisnific.antsurfacesof the electroplated article

shaJJbe freeof cleatl)'visibleplatinsdefects,suchas blisten,pits, rouihncsS. tracl($. aDduncoatedlUgs and shalldot besWncd or diSCDlored.On articles where a visible conlictmark's unavoidable, its posi\ion shall be specHied by thepurchaser. The electroplated article shall be clean andfreeofdamale,

6.1.2 Defects in the surface of thc basis metal, such asscratches, porosity, no~conductin8 Inclusion~, roll and diemarks, cold shuts, and cracks, ltIay advu~l)' affect theappearance and the perfonnance Df coatings applied theretodespite the observanc!: of the best electroplating practices.AccordinsJy, the plater's responsibility for defects in tbecoatins resultins frorn suchconditions shall1:e walv~d.

. Nora 2-To minlmi2e,problemsor mis f~, the specificationscoven". the basismaterilJ0" the item to beelectroplatedshouldconl.ainappropriato Iimit8tJoas OD'\lcb basIJ mcral CX)oditioos.

6.2Processand CC)AlingRequirernentt:6.2.1 Proper prepantory prOC:edures and thorough

cieaniul of the basis metal surface are ~ssentia\ for satisfac-tory adhesioD and cOrTInlonperformanco of the coatins.Accordingly, the applimtble praCticcsfor the preparatiDn ofvarious basis meWs for electroplatingshall be followed.Various ASTM practiCC$ tor the preJlaracion of basis me",\are available. See Section 2.

3

6£tt-268 £0£ NGA31S 'l'~ vt:2t £6. 6t lnr------------

INCuS Ni351SCr r 35Zn/Cu5 NI3OdCr mc 30Zft/CIIS NI3011 Ct mp 30

%n/CII5 1I/'25C1 CI' r 25Zn/Cu5 Ni2DuCr meZn/Cu5 NI2OdCr mp 20

nlCl/$ Ni3SP Cr r 35tn/CuS Ni2SpC'.mc 2SZnJCu5 N125pCr I'll) 25

tn/Cull NI2QbCr r 20Zn/C5 Nasl'I Ct me . '52n/Cu5 Ni1Sb Cr "'II 15

Cu/Nl25dCr, 25 .Cu/N12Od C, me: 20Cv{NI2Od Cr nip 20

OulNi25p Cr r 28

Cu/N12OpCr me 20CII/NI20p Cr Inp 20

CwJNi30bCr r 30CuJNt2lib(irme 25CujNl25b Cr mp 25

CIIJNI15DC, , 1SCuJNi10DCr me 10 :

CU/NI10bOrmp. 10

"'. ( I' J.='1'='=> Ia::' ; =>~ 1)UI..UI'It:.I't' t:.1't\:lJ r~t:.t:.r::I 1"11.;:1'_U., J ""-. .." ..JI:J..J l:I:;Jc; 1.1 J::1 "fW. J.'.'U I ~" ,

41ftt B 4$8

6.2.2 FOllowing the preparatory operations. the parts(articles) to be electroplated arc introduced in s~ch platingbaths as required to producethe typesof depositSdescribedby the spec:if1ccoating c:fassiftC:lItiannumbers or one of thecoatins classification numbers listed in Tables 2, 3, 4, or 5appropriate.for the specified set'lice condition number.

6.2.3 Type of Copperand Deposil Thlckness.-6.2.3.1 Type o/Copper-The type ofeoppet is designated

by the ronowingsymbolsthat are placedafter the thicknessvalue:

a for ductile copperdeposited from acid-type baths' con-tainins additives that promote leveling by the copper deposit'and that havean elonption not lessthan8 %.

No symbol is placedafterthe thicknessvalueif a min-Imum elansatlon Is not requiredor if a depositfrom anon-levelingbath ispermiued. .

6.2.3.2 Thicknejj 01 Copper Deporits- The number fol-lowina the c:helJ~ical symbol for copper (Cu) indicates inmicro metres the minimum thickness of the c:opper deposit at

. pointson significantsurfaces(see3.1).6.2.4 Type of Nickel and Deposit Thickness.. .

6.2.4.1 Type of Nickel-The type of nickel is designatedby.tho fOliowinBsymbols,whi,b are placedafterthe thick-ness value(Note5):b for nickel deposited in the fully bright condition.p ror dull or st~mi-bri&htnickel requiring polishlna to eave

full brightness. This niclccl shancontain less than 0.005mass% sulfut (Notes3 and 4). and have an elongation ofnot. less than 8 ~.

d for a double-layer or triple-layar nickel cOllins. Thebottom layer of this coating system shall a)ntain les.sthanO.ooSmass% sulfur(Note4),andshanhavean elongationof not less than 8 %. The top layer of this system shallcontain more than 0.04 mass% sulfur (Notcs 3 And 4),and its thicknessshaUbe not IC$$than 10% of the totalnickel thlckMSS: the thickness of the bottom layer indouble-layer cQatinss shall not be [ess than 60 % of thetotal nickel thickness, except (Otsteel. where it shall be atleas17$ %. In triple-layer coatings. the bottom layer shallbe not less than SO% nor man: than 70 %. It there arethree layers, the intermediate layer shall contain not lessthan 0.15 mass% sulfurand shallnot exceed 10%of tbetOtaJ nickel thickness. These' requirements for multilayernickelcoatin...o;aresummaritedin TableI. . .

NOTE3- rhe sullUrconteIllSan specifiedin ordor ~oindicatewhichtypeor nickllelmvoplatins sol"uon must ha used. AlthouSh at pracnt.no simple method Is available for decenninlna ttle sulfur COntent or anickel depQsit on a coated article. chl:mlc:a1determinations are possibllusina speciaJly pnpared test specimens (HI! Appendix X3).

NOtE 4-t~ will usually be IIOssible10 idl!lItify the t)/lle of nickel bymicroscopical CJlarnlnation or lhe polished and Itched section or anIlrticle i>replred In ILCcOrdalletwith Test Memed8481. The thickneu orthe individual nickel la~el$ in double-layer. and tIi!)lc.la)'Clrcoatinl\.!. aswell II Ihe ele~uoehemlcaJ relaliol\$hips between thl! Individu" laycr.!.eliI'!al$o be mell$lIred by Ihe STEP test.' in accordance wilh Method8764. . ..

6.2.4.2 Thick111U Df Nickel Otpotil- The number rol-- lowing the chemical symbol Ni indicates. in micrometn:s,

'HmuIDk. E. P.. "Simulttnecl'" T1titkncsa and EleCltOI:l\emicDIPOlenli:llOclcnnlnallon of Il\di..idu:lll.Q~etl in Mullil:aver N'relt.1 ~pOsils,' PltJI'"R QlldS"r/IIC/! I'1nl.r/,;",. Vol 67. No. 49. February 1980.

..

L'd

the minimum thldcne$sof the nickelclecuodeposit at polnuon the significant surface (see 3.1).

6.2.5 Type 0/ ChromiumandDepositThickl'less:6.2.5.1 Type 01 Chromium-The Iype or chromium de.

posit is designated by the fOllowina symbols phlcedaftet thechemicalsymb.olCr: .

r for "regular" (that is, conventionaJ) chromium.

me for microcracked chromium, having More than 30cracks/mm in any direction over the whoLe of the silnifi.cant surface. The cracksshall be invisibleto the unaidedeye (see 6.9).

mp for microporou$chromium containinga minimum of.10000 pores/lO mm b1'10mm square (LO000 em1). Thepores shall ~ Invisible to the unaided eye (lite 6.9).

6.2.5.2 Thicknell of Chrom{umDepos/r- Theminimumthicknessof the chrami\lm deposit shall be 0,25 11monsi&nificantsurfaces (see 3.1),exceptthat for serviceconditionSC I (see4.2.1) the minimum thicknessmay be reducedtoO. f 3 ~un. The thickness of chromiunt is designated by thesame symbol as the type,irlstead of by numerals as in the caseof copper and nickel.

6.3 Adhl$(on- The coatins shall be 5ufficltmtlyadherentto the basis metal, and the separate layers of multilayercoatingssbanbesufficiently. adherentto each otber.to passthe appropriatetC!$t$detajledin Test Method$B571. Theparticular test or tests to be used shall be spc~cif1edby thepurchaser.

6.4 DUClililjl- The ductility shalt be such that theelonga-tion will not be less than stated in 6.2.3.1ror copper and6.2.4.1for nickel when tested by the method gjven InAppendix.X2. Greaterelongationmaybe requestedbut shallbe subject to asrcement between the purchaserand themanufacturer. .

6.S Coaling Thlckne.rs: .6.S.1 The minimum coltin, thickne$SshaJJbe IS desig-

nated by the coatitll elassUicahon number.6.5.2 It is rea)gnlzcd cbat requirements 018)' exist (or

thicker coatings than are c.overedby this slJeCiflcalion.6.S.3 The thicknessor a coating and iu various layers

shall be measured at paints on the slgnifi4::antsurfaces (Sel:3.1 and Note S). .

NOT!! 5-When slanificantsurfacesare 1Jwolvtdon which (hespcciOcdthickness ot deposit cannot readilYbe controlled.such asUlreads,koles. deep teCCSSCt,bws or an&les.!I\!Idsimilar ara&, 1I1epurchaseundthe manufactutlt shouldr8C0anluU,cnc<.~!SSityrorlitherthicker dcposll$011thc more ac:c:essIbles\tr(accs Of for spcciaJ r:ilckin8.Specialricks mlY Involvc~hcU5Cor conrolTltlng.aUliiliary.or bipolareleeU'Odesor ft<lDl:ollduct!nlst\ie1d8. .

6.S.3.1 The coulometricmethoddesclibedin Methoc:tB 504 may be used to lt1e.uurethicknessof the chromium.the total thickness or the nickel, and the thkkness of thecopper. The STEP test. Method B 7641 whicl\ is similar tothe coulometric: method, may be used 10 c:losely estimate thethicknesses of Indillidual layers of nickel in Ii multilayerc:olning.

6.5.3.2Thc micro$CopiaJ method describc:d in TestMe&hodB 487 may be used to measurethethictmessof eachnfckellayerandof thecopper layer.

6.S.3.3 The X-ray method described in Test MethodB 568 may be usedwhenthe total thickness -clfa coppetl

46S11-268 S0S N3A31S 'l'~ 91:21 S6, 61 lnr

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£17/19/95 1i1=':~,j UUCUM~NI ~NblN~~~lNb LU.. IN~. ~ ~~~ ~~~ !!~~ I'!U. J.OQ r\:J"-'Qr \:JJ."-

,iii B4SS

nickel/chromiumcomposite coating is to be measured,withoUI an)' indication of tbe thickness of each individuallayer; "

6.5.3.4 Other methods may be used if it can be demon.stratcd that tt\e uncC:J1.aintyof the measurement is less than10%, or lessthan that of any applicablemethod mentionedin 6.S.3.0Iher methodsarc outJint:din Guide B659. .

6.6 Corrosion TeSt;ng:6.6.1 Coaled arlides shall be subjected to the COlTosion

. teSIfor a period Dftime that is appropriate for the panicularservice condition n.:amber (or for the service conditionnumber corrcsponding to a specified class.ification number)as shown in Table 6. The test is ()esc:ribed in detail in thereferenctd ASTM desianation.

NOTE 6- There is nc direct relationbetweenthe reslIlu or an.ct~lerated «:ol'1oslonleSI "nd the rlSiSl3ncr to toITosion in other mcdia.be~allse seve:ral f.clorl. sueh as the fonnadon of protecUvI films.'nnllenc:t Iht pro&fCSSof cOITOiionand vary areatl)' with the eonditionsenrounlel'td. The resuh5 obtained in the: tlsl should. thererore. nol berc:,:ndC!das a direel (luidll to Ihe c:onosion rtsisl:t.n~ of Ihe: ICSledmalenals In all envitOnmenlSwherethese m~nerialsmay be used. AI50.perfotmance: or ditTerenl malerial, in thl tesl cannOI always be taken asa dire"l &uide10the relative tesislanceof Ihesemalen;lIsin service.

6.6.2 After the anide has been subjected 10 the treatmentdescribed in \he relevant corrosion test method. it' shall beexamined (or corrosion of the basis metal or blistering of thecoatin&. Any basis metal eorrosion or blistering of thecoatins shall be cause for rejection. It is to be understood thatoccasional widely scattered, small corrosion defects may beobserved after the teatina period. In general, "acceptableres.istance" Jhall mean that such defects are not, when viewedcritically,slenificantiydefaclna or otherwise deJeterious tothe function of the electroplatedpart. A method of ratinacortosion is ,.iven in Pmctice a537.

6.6.3 Surfacedeteriorationof thecoatini itselfisexpectedto occur during the testins of some types of coatinls. Theutent to which such surface deterioration will be toJeratedshallbe speclnedby the purchaser.

6.7 ST,~P j~$r Requirements:6.1.1 The electrochemical potential differences between

individual nickel layers shall be measured for muJtilayercoalings c:ormpond1ha to SC5. SC4, and SC3 in accordancewith Method B i64 (STEP Tesl).

NOT£ 7-Un;vtr$aUy accepltd STEP values havt 1101beln eslab-liihtd but someagteement in Ihe valueof ranaeshas been obLained. TheSTEP 'Valuts del,end upon which two nickell.ycn are bein. measured.

Thc STEP pountial differencebclwec;n the: seml-briE'.ht nieltellll)"!rand Ihe bri8ht nickel la)'Cr lias 8 ftlnlt 1)( 100 to 200 mY. For allcombinations or nlekellaym. mo scml-brisJtl nicklilayer Is mOR noble(C8thodic) than the briaht nlcket layer.

The StEP pOtential difference between the hIJh-a.cti\'ity ui«:kellayerand the briJht nickeillyer In Uiplc-Iayer cn.lJnas 111,\a potentlAl.1Ingeor I S to " mY. The hiah-ac:tMt)' nickel 11)'lIrIs nlora active (anodic)than the bliSht nickell.)'If.

The STEP potlntial differeDu bllween the brisht Dickell.)'Ir and ..nickeillyer belwccn me bright nickcll.ytr and the cbromlum layer has. polen1ialranae oro to 30 mY. The bri8ht nleblla)'er Is morc ao1ivc(anodic) than th~ mckel laYITprior to ebromium.

6.8Sul/urCo",ent:6.8.1 The sulfur content of the nickl:I dc~po$itshaltmeet

the maximum' or minimum vaJues as JUttedin 6,2.4.1 IndTable I.

6.8.2 Methods for sulfur dctemlinatlons are given inAppendix X3.

6.9 Dens;tyand Measurementof tile Di.5continu;liesinChromium:

6.9.1 'The density or cracks Dr pore$ in microcracked ormicroporous chronlium deposits slutll meet minimumvaJues. Microcracked chromium shall have more than 30cracks/mm(300crac~ks/cm)in Anydirection over ,he wholeof the significant surface. Mi~rOPi3rouschromium shallcontain a minimum or JO000 pores/IOb:l 10 mm square

. (to 000 pores/em;') in any direction over me whole of thesignificant surface, The cracks and pores shitlllx: invisible tD

the unaided eye. ,

6.9.2 Methods for measurin8 the di~Ohtil1uit.iesIIrcth,cnin Appendix X4. See X4.4 in Appendix. X4 for a meansofdetenniningQct;vecorrosion sites by COITOsiol'lt!lstins.

"1.Samplina Requirementsi.1 The samp1ini ptan used for lhe .Inspectionof a

quantity of coated articles Shan be as agreed upon by thepurchaser and supplier.

NOT'; 8-Usually, who" a eollll::uon or CO'atedanlcl", Iho inspectionlot (8.2). is eltlmlnedforcompliance with the l'8Qul~menlS,laerG onthe cDatina. a relativelyamaJlDumber of 'he .mcles. the sample!.isscI~tcd II random and is hl3pected. The inspection 101as \hen classinedIS complying or not comptyiaa with dill requirem.nts baaed on theresultsof ~heinspection af 11\,ample. The sl~eor ~hlfiIiIImpJe andIhe,criteriaorcompliance .8111determined by the appllc:allon of stalistics.TIle procaduR! is knownas amplin. Inspecr.ion.Thnte standards. YeslMethodB602,Guide8691. Incl MethodB '/62 <:011141"somplinaplansthat are desi8ned for the IIRlplins Inspecti(1I) of coatinf,$.

Tat Melhod B602contains(our umplinl plans, three for IIU wbh

TABLE & Corro.lon T..,. Appropri.tetorEachStryl~. COndition NUMbtrNOT£ 1-The I~ed '"",1"" ISllspray IC'SI,TISI Melhod8117 "*' bIIenQlntlf'8I1yClIlCired1tlCllISan 1CCIII..111Id CORVSIon1151lor cJeconItlve "1cklf.d\romlURI

COllings IArge~ t1eC"4I1S.01 t.Ck 01"plodIICibifily 01 ,esulIS,"lIla r8cQgn1zed. ftOwlver. Ihllilhe tl"" tllU UHISIn 8OR'IIMglftllllt. 01Il1o l!Ic1rcpl8brlQ ,""u,.ry 10 CIIedc

11\. tju.fity 01 COII/J\gs 1t\lelldeG '011118 wn"" rellllvely II\ItI $Inrlct COIICIition1.~ly.111a SUOIIlltId ~I any u.. of IlIIt ttltllMlllf18 r8Q\riItmtmlS tu balMl De theeuajeel 1)1'egrll8lllQl\1 bet"'Mn 1118PJICh"" 1Mb manullClwrtr and. furthIII'. thai il8 we be canfinecl to the CDI'lrlQt IndIcaIld .. tppI~111' to' Serlica CQndIIIIII'IINos.2aI1d1. '

Non 2-Tne 'AC81ic;'s8lt Melhod 8287 has been 1IIscon1inl/ld.

8asIsMtI.I. 6eMco OnllianNO. ' Acetl(:ollllt MllhOd B 287

CASt MIIhOdISH

SC5 44SC 4 ft TWII18-1tCytIe& '144~3 d ~ Hsca ... 1!4SC1 8

,. MlndiUI. A...Slal'ldardSill.Spray Te'I-ls It. ValidAc:oeptance fe',? PropertJ... T'81111114PerfORnlrlC801 E~odeposl'lId M18lldUcCoatlnUI. ASTMSTP liT.ASTM t8~G. p. 107.

S

SlteII, me. ,/loy.Cr copper .rId

, g)Dpet IUoy

8'd

Caro8Ion-;:;11nd IJutaIlorl h

CIc:mIc1kOII Me\hocl B 380---,

6S11-268 S0S N3A31S .l'~ 81:21 S6. 61 lnr

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0'7/19/95 09:54 DOCUMENTENGINEERING CO., INL;. ~ ::'\:j:::! C!:!;:: 11:::!~ I'~IJ. It:Jb t"""'" (" "'J.":

4. B 456

le5\s thaI An: n6n~e$tNttivt and one when thc)' II~ dcstNctivc. Thebuyer and seller may asree on the plan Ot plans to b.! used. Ir they donoi. Test Method.8 602 Identities the plan to used.

Guide B691 provides I carp number of plans and also a!ves ,uidaneeon the sell:l:lion of ~plan. When Ouidc 8 697 is sptl;incd. the b\lycr IIndteller need to a&reoon the "llIn 10 be used.

Method B 762 ell" be used only for coatltlC requirements Ihat ha1lCanlimeriC41 IImi" such U C:OItinll thicknas. The lest must yield 11n\lmericaJ value nnd "ruin slatisticaJ req\liremencs must be met.Method B 762 contains Sl:vctal plans and also &ivC$instl'UctioRS forealeulatin. plan. to meet soeeiQJ needs. Tile buyer Illd UIosellet mayIlJtee on the pilln or plans to be USId.If lhay do not. 8 76.1 Identities Iheplan to be used.

NOTE 9-Whcn both destructivaand .nondatructivi testa exist rorthe mc~uremClnt of. c:haraCkris\ic. the purchaser needl to state whichis to be used SOIhe proper samplinl plan i5 scllcled. A test may. de"roythe coatill8 but in a nonc:ritica1arca; Ot, althou8h it may desiroy thecoatlnL a lested part may be reclaiMed by sttippins and rec:oalJn.. Thepurcllnscr needs to state whether the IC$tis to be considered destNctivcor nondestftlctlve.

7.2 An insPectionlot shall be defined as Ii collection ofcoatedarticlesthat are ot the same kind, that have beCDproducedto the same specifications,that havebeencoatedby It sin&.lesupplier at one time or approximately the same

time under essentially Identical conditions, ~nd that afftsubmittedfor acceptanceor rejectionas a group.

7.3 If separatetestspecimensarc used 10 r.cpresent thecoated anlcles in a test. tbl~specimens shall be of the nature,!!I~e,and number and be prcx:essedas tecluiredilt Appen-dixesX2, X3, and X4. Unlessa needcanbedemonstrated.separately prepared specimens shall not be used In place ofproduction items for nondestructive tests and visuIl1exami.nation. for destructivetestS includins determination of ad.hesion, ductility, sulfur contents. the number of discontlnu\.ties, andcorrosiontestinl. separatelypn,pan:d specimensmaybeused.

I. Packagina8.1 Pans plated for the:U.S. Oovemmentand military.

inc:ludinssubcontracts, shall bepackagedinaccordancewithPractice D 39S 1.

9. K.)'Words

9.t corrosion:decorative;eiettrodeposited c:hromiumielec:uodeposited copper, electrode posited niCkel

APPENDIXES

(NonmandBtory InformatloQ)

XI, DEFINITIONS AND EXAMPLES OF SERVICE CONDITIONS FOR WHICH THE VAR10US SERVICECONDITION NUMBERS ARE APPROPRIATE

. XI.I Service Condition No. SC j (Extended VII')' St-vere)-Service conditions that include likely damaacfromdentin.. scratchJnl, and abrasive wear in addition to expo.-sure to corrosive environments where long-time protection ofthe substrate is required; for example, conditions encoun.teredby Some"tenor componentsof automobiles. .

XI.2 COlldlttonNo. SC 4 (Very Severe)-Servlce condi.tions that Il\clude1ikelydamagefrolll dentin.. scratchina,and abrasivtIwc:prin addition to exposure10 corrosiveenvironmentSi for example, conditions encountered by ute.

. riorcomponentsQfautomobilesandbyboatnningsin saltwater service.

XI.) Se~/ct Condition No. SC j (Severe)-Exposurethat is likely to include oc:c:<a.sionai Ot tre~uel'lt w~tting by rainor dew or possibly strona cleaners and saline 5Olutlons~forexampic, conditionsencounteredby porch and lawn furni-ture: bicycle and perambulator pan$i hClspitalfurniture andfixtures. .

X 1.4ServiceConditic)1INo.SC2 (Modertlle)-ExpoSUrCIindoorsin placeswherecondensationof nmisturemayoccur;forexampte,in kitchensandbathroom~.

X 1.5ServiceConditionNt).SC I (Mild)-Ey,posure in-doorsin nannall)'warm,dry atmospheresv.-ithcoatingsubjectto minimumwearor abrasion.

Xl- DUcrlLlTY TEST

NOT!!XZ.I- Th.ls lest is used 10 ensul'O cQmplianec or the typil ortopper and nickel d.er>ositwitb !hI appropriale dlfinilian &i\'Cftin 6.4.

X2.' PreparationofTen Piece:X2.i.l Prcpar~an electroplatedtest strip, ISOmm (onl.

10rnm wide,and 1 rom thick by the followingmethod:X2. 1.1.l Polish a sheet or the appropriate basis metal,

similar to that of the a!ticles bein, electroplated, eJtcept thatIf the basismota!is zincalloy.thesheetmay be:of softb~,(Use a sheet sufficlentl)fIBraeto aJlow the test strip to be cut

~ from itScent$rafter trimmingofTa border25 mm wideallaround.r Electroplate the polished cide of the sheet withcopper or nickel to a thickness or 25 ~m under the same con.ditions andin thesamebath 81the corresponding articles.

X2.J.J.2 Cut the te3t.$trip from the: cl~c:troplatcdshect

6'd~- --

with a nat shear. Round or chamfer the longer edgtS of thestrip, at least on the electroplated side, by C41'I~fuIfiling 01'Jrindlns.

X2.2 Procedure-Bend the test strip whh the electro-plated side In tenGloG(C1I1the outside), by steadilyapplyinspressure, through l80. over a mandrel of I LS mm diameteruntil the Cwoends or the test strip are pa(;~lIel.Ensure thatcontact between the test scripand the n,andrel illm~~ntaineddurina bending.

X2.3 As.sessmenl-The electroplatlns is deemed 10cOlUplywith the minimum requirement of an elongation of8 % if after~"tina ther~are no cracksP8.&Sinacompletelyacross the con\"exsurface. SmaJlcracksat theedgesdo notslanity failllA:.

66S~~-268S0S N3A315 'l'~02:2~ S6. 6~ lnr

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. B458

X3. DETERMJNA TlON OF SULFUR IN ELECfRODEPOSITED NICKEL (NO1"EX3.I)

The roUowir'l&twomethodsforthe determinationof sulfurin electroplated nickel arc given as guidelines for use to testcompliance of the type of nickel deposit with the appropriatedclinltioneJvenIn 6.3.:2,They representmethodsthat havebeen used with success commercially; they 8rc not ASTMstandards, nor is It the intent in publishing these methods topreclude the use of other methods or variotions in theseMethods, ..

X3.1 TOlal Sulfur in Electroplated Nickel by CombusUon-. IodateTilr.1io"

X3.1.1 Stope-This methodcoversthe detennlnationofsulfur in concentrations from 0.005 to O.S mass %.

X3.1.2Swmmary of Melhod-A major pan or the sulfurin the sanlple is converted to sulfur dioxide (SO2) bycombustion in a slrtam or oxygen using an inductionfutnlce. During the combustion, ,be SO1 is absorbed in anacidified 5Utrcb-jodidesolution and titrated with potassiumiodate Solulion, The latt~r is standardized against stcels ofknown sulfur con~ent to compensatefor characteristi~of aBivenapparatusand for day.,;to-day\'ariationin the per.

. centaaeof sulfur recoycred as 802, Compcnsadon is made. (ot the blank because of accelerators and crucibles.

Non X3.1-lnstrumentsorea\'ailablefor .tneasurin&the sull'urdlo~idefrom combustionby Inrrareddeteetiot\methodsand uun.built.incomputen to Intesraleand displaythe.lull'urcantontas apen:entage.

X3.1.3 lnrerfereficcs- The elturlen\Sordinarily present inelectroplated nickel do not interfere.

X3.I,.4Apparatus-Induction heatina apparatus for de.termination of sulfur by directcombustionas describedin

. Practices E 50 (Apparatus No. 13).X3.I.S Reagenl$: . .X3.I.S.1 Purity of Rtagenu-Reagent grade chemicals

sha1l be'i.lsed in all tests. Unle$Sotherwise indicated, it isintended that all magcnts shalt contonn to the Specifications

.of the Comlniuee on AnaJytical Rea,ents of the AmericanChemical Society. where such Specifications areavailable.1oOther grades may be used.provided it is first determined thatthe reagent is of sufficiently hiah purity to pennit its use

. without lesseningthe accuracyof the determination.X3.) .S.2 Purit)' of Water-Unless otherwise indicated,

reference to water shaUbe understood to mean reagentwater. conforming to Specification D 1193.

X3.I.S.3 Hydrochloric Acid (J""97)-Mi'l 3 volumes ofconcentrated hydrochloric acid (HC!) (sp 8t J.l9) with 97volumes of water.

X3.I.S.4 Iron (LOw-Sf.if"r) .Accel~'QlOr-Chips;X3.U.S Iron (Low-Sulfur) Accelerator-Powder.X3.I.S.6 Potassium loda(e. Standard Solulion A ( J mt-

O.t mBS)-Dis50lve 0.22.25&or pl)tWium iodate(KJo.,) In

10-Reoaenl Chemlells, AmC':rltln ClleMteal Sociel)' Spctll1callOlls," AM.Chemical Soc:.. Weshil\&ton. DC. For '1IlIlISlions an the Irtlina or tOIsenl. nOtlisted by Ih, "Mericln f.bemlcal Socld)'. see -Rea",nl Clltmical. and Slandards,.~ Joseph AOlin. O. Villi Nostrlllld.Co.. Ine.. Naw Vorlc. NY. Rnd the .UnlledStalA PII\lr"'.co~ia. - .

0J'd

900 mL Dfwater and dilute to t t.X3.I.S.1 Polauium Iodate,StandardSolution B (1 mL-

0.02 mil S)- Tnansfer 200 ntL of potassium iodatlt SolutionA (I mL lilt 0.1 ms S) tg a 1.L volumetricflask,dilute tovolume. and mix.

NOTEXJ.2- Tht sulfurequivalentIabll3el:lon .he completec:cmvcr-sion of sulfur to sullUr dio~dde. The I'ecOY'I'yof uul(ur as the dioxidemay be lessthan 100$, ')\.Itit II consistent1~hcn the \emperlt\lre andthe rateof OA)1en now Ire malnwneCI eonslant, An ompiricalfaeaormustbe deltnnlnerJ by ah analysisor 8 standard $ample. .

X3.1.S.8 Sla'ch-/odideSolUIIDn-1'ransfer t 8 of solubleor arrowroot starch to a small beaker.add 2 mL of water,and stir until a smQothpaste is obtained.Pour the mixtureinfO SO mL of baiting water.Cool, add l.!i I of po~siumiodide (KJ)\ stir until dJssol\'ed, and dilute to 100 mL.

X3.t.S.9 Tin (lowaugur)AcceJel'lItor,sranular.X3.1.6Slalfdards-5tandards fol'cal.ibrationare National

Institute of Standardsaod Technology$\"1$of the propersulfurcontent.

X3.1.7 SamplePrepa'ation:X3.1.7.1 Pn:paR!"test panelor cold-rolledsteel ISOmm

Ions by 100 mm wide by t mm thick or any otherconvenient site. C1e;t.n.IIQid dip, and ,~lec1.roplatewithapproxlmatClly7.S ~m of an adherent nickel deposit andthoroushlYrinse. ButTednickel or buffed ttainless steel mayalsobe used asa1tel118ttvesto steelelectroplatedwithnickel.

X3.1.7.2 Passi'iate the test panel unCldicaJlyat 3 V for 5 to10 s in a hot alkaline cleaner (~perature 70 to 80.C)containing30slL ofaodJumhydroxide(NaOH) and 30 &lLof trisodiumphosphate (Na3PO.,or 60 8IL or aD)'o&hcrsuitable anodicaUcWinecleucr.

X3.1.1.3CoattbepassivatedIe$!panel '\lith 25 to 37J1mor nickel deposited from the same soluda" usingtbe sameparameters as for the coated artitlCtIrepresentedby tht testspecimen.

X3.1.7.4 Remove the edges of the et~troplated panelwith a hand or power shear or any othl."famycnicnt methodthat permits readyseparationof the tes' fail

x3.\.7.S Separationfrom the palDel, wn1htbe rilckel foilelectroplatewithwaterto removesaltsBndbiOidry. Cut intopieces 2 to 3 mm J'tr side with a sdssol'lc.Transfer to aIOO.mL beaker, cover with water, and heat 'o boiling.Pouroff tbe water and wash with methanol. Air dry the nlclc(!1onfilter paper. .

X3.J.8 Weight /0" Standards and $amJ'ies,-Select aDdwelsh to the nearest0, I mg an amonn, of !Mlmpleas follows:

EXI*1H SulfurConlcn"MUS~ WCi~1ofSanlplt..

0.005to 0.10 I,CI:I:0,020.10100.$0 0,:1!t.O.C:U

X3.1.9CdlibratiOfl-Sclcct a minimum (If two standardswith sulfur contents ntar the high,.and low-limitsof theranse tor a given sample weiJht and also onc: near the mean,The meanstandard may be simulated, if necessary,by takingonc-half the sample wci&ht of each or the other two. Followthestepsofthepr~ure.

"3.1.10I'r(Jcedure:

7

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/" -lilt B 456

X3.I.IO.1 To the crucible add I g of iron chips, 0.8 g ofIron powder, and 0.9 8 of tin. Transfet' the proper weight ofsampleand covt:r. .

X3.1.10.2 Turn on the power of the induction furnaceand anow the unit to heat to' operating temperature. Withoxnen flowln, through the absorption vessc:l, fill it to apredetermined point with HCl (3+91) (X3.1.$.3) (NoteX3.3). Add 2 mL or starch solution to the vessel. With theoxysen flow adjusted to 1.0 to 1.5 Llrnin (Note X3.4). addKIO) solution specIfieduntil the intensity of the blue color isthat which is consideredas the end point. Refillthe buret.

NOTt X3.3-AlwIYs 811the titration ve&:l to the samepOint.Non. )(3.4- Tbe OX1B~nRow nil may be adjusted10 meet the

requitcmel'llSof individutl openllors or equipment: however. tho nowra&lmuSibe the SaMefor me test samplesand ,hi s1andard$l\mples.

X3. I, 10.3 After the unit hu been at opcratins tempera~ture for at least 4' s. place the covered crucible containingthe sample and acceleraton on the pcdeml. Witb the o)t)'scnnowadjusted,raisetho crucible. close the f'urnaco,ttnd tumon the power. Bum the sample fot 8 to 10 min. Titratecontinuousty with the KIO) solution at such a nne as tomaintain 85 nearly as pO5.siblethe oriainallntenslty of theblue color. The end point is reachedwhen the ori&lnalbluecolor is stable for I min. Recordthe final bun:t readinsand

. drain the titratIoD vessel throu&h the exhaust stopcock.X3.I.IO.4 Blank-Detennine the blank by placing the

same amount of accelerator.; used In the test sample in II- preignited crucible. Covet and proceed as in X3.1.10.3.

X3.l.11 Calculation-Calculate the sulfur faCtot of the. . potaSSiumiodate asfollows:

Sul(ur (actor. aluni' ...alume- (C _AD~: 100where:If' . grams of Standard sample used.B - percent$uIrurinthestandardsample .

C - mtUilitres of KIO)solutionrequiredfortitrationof thestandaflt sample {Note X3.S), and

D - miJIIlitresofKIO, solution required for titration oftheblank (Notl X3.S).

NOTE XU-Or a"parel11 percentaseor sulfur (Ot -direct-readina-burets. .

X3.1.11.1 CaI<:ulate the percentage of sulfur in the testMmple as follows:

(E -D)FSulfUr.mass" . G x 100

where: .

E .. KlO) solulionrequiredfor titration of the test sample(NoteX3.S),mL, .

D "" KIO, solution requiredfor titration of the blank. mL,F II: averaae sulfur factor of the KIO, for the standards

used (see X3.J.lI), gfunit volume. andG - sample used, 8.

--- X3.Z DetermlnatioQof Sulfur in Electroplated NIckel by theEvolution Mechocl

X3.2.1SttJpt- This methodcoversthedeterminationofsulfide sulfur in electroplated nickel in the range from 0.005

. to 0.2 mass CRt.

n'd-- - - - -

R€C!lvIIoiGFLASI(

0FIG.X3.1 App.r.",. ror Ihe DeterminllUonQf$\llf," InEI.~pl.tld Nick"Foilb~thl EVDluUonM,UlocI .X3.2

X3.2.2 Summaryof MethodII-Sulfide sulfur is evolvedas hydrasen sulfide (H25) on dissolvina. the sample ofhydrochloric acid' (HCt) containini a smaU amount of .

platinum as an accelerator for dissofution.The sulfur isprecipitatedas un!: sulfide(ZnS) in the receiving vc~s.selandthen titrated with standard powslum iodate solution. Valuesarc based on potassium iodate (KJOJ) as the primarystandard.

X3.2.3Apparatus:X3.2.3.1Theapparatus is shownin Fig. X3. J. 11may be

assembledusinsa SO-mLErlcnmeyet f1a:skwith a No. 19/38outer joint. A washbottle fitting with a No. t9/38 inner joint~Q be :cut to fit the SO-1uLnask. The exit tubctcanbebentand c:onn~tcd to the 6.mnl aas tube with tubing.

XJ.1.3.2 A nitrogen cylinder with valyes and prcS$ureregulator. .

X3.2.3.3 Buret,:to-mL.X3.2.4 Reagtltts:X3.2.4.1 PurilY of Reagents-Reagent aradt. chemicals

shaDbe usediD au testS.Unless Qtherwisuindicated, il isintendedthat aUreagentsshaDconformto the specificationsof the Committee on Analytical Reagents of tbe AmericanChemical Society, wheresuch $pecHicationsare available.1Otber &tadesmay be used, J~rovided It 1$first ascertained Ihatthe reagentis of sufficientlyhi8h purity to permit its usewithout lessenlna the accuracy of the detennina.tiQh.

X3.2.4.2Purity of Wate,-Unless othCl'WiR.indicated.referencetowatershallbeunderstoodto meanreagentwaterconformina to Specification D 1193.

X3.2.4,3 AmmoniacalZinc Sulfate $orllfio1l-.DiS:lolveSOg ohine sulfate (ZnSO... 7H:sO) In 2S0 mL orwator. tdd 2'0mL ofammo&\ium hydroxide (NH"OH, sp it 0.90) and mix.

"Lllk.,C.I... A"alYlletlIChtrniJIIJ'. VoIZ9. 19'1.11. ';!27.

86£11-268 £0£ N3A31S 'l'~ £2:21 £6. 61 lnr

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4t B451~

Transfer10a Rask and anow to stand about 24 h and filterinlo a polyethylene bottle.

Xl2.4.4 Hexachlotoplatint'cAcid SolutiO1l(JO g/L)-Dissotvc 0.5 8 of hclt&chloroplatlnicacid (H2P1C16.6H2O) inabout 40 mL of water. add S mL of hydrochloric:acid (HCISp gr 1.19). ftnd dilute to 50 mL.

X3.2.4.' Hydrochloric Atid.PltJlillum Chloride Solu.. lion-Prepare SOOmL of diluted hydrochloric acid(HCIsp

Sf 1.19 I pan acid in I pan water). Add 2.5 mL of thehe"achloroplatinic acid solution and milt.

X3.2.4.6 PotQSsillm}odatt. Siandard Solwion (0.1 N)-DJ}'the crystals of potassium iodate (KlO,) at 180lC fOf I h.Dissolve 3.510 B or the KJOJ in about 200 mL of water.transferto a I-Lvolumetricf1ask,dilute to volume, and mix.

X3.2.4.1POllUS;U", Iodate. Standard Solution (0.00$. N)- Transfer2SmL of the0.) N KlO) solutiDntoa SOO-mL

volumetric flaskwith a pipet,dilute to volume,and mix.X3.2.4.8Starch Solution (10 gIL)-Potassium Iodide (50

tlL) Solution-Add about 5 mL or water to I S of solublestarchwith Stirrinsuntil a paste is (ormedand add to 100mL Qfboilinawater.Cool. add 5 I Ofpo1asi1iumiodide (.KJ),And slir unttl the KI is dissolved.

. X3.2.S Sample PrepQralioh-Prepare sample as outlined. in X3.1.7.

X3.2.6 Weight .0/ Sample-Select and weith to thenearest 0.1 m& an a.mount ofsarnple as follows:

Weiahl or SIImpir.I :t 0.02

1.00..

E.~r.cd SlIlr"'t Co-nltnl. maas .I).OOSto 0.07o.OS 102

X3.2.7 Procedure.-X3.2.7.1 Weigh the specified amountof sample to the

nearest 0.1 DIgand transfer to the SO-mLevolution flask.X3.2.7.2 Add 20 mL of water and 3 mL of ammoniacal

1Ine sulfate solution to the receivina nask .

X3.2.7.3 Adjust the hot plate to maintain the temperatureof 2S mL of waterin I SO-mLErlenmeyerRISkat 80.C.

X3.2.7.4Add IS mL of the hydrochloric acid.~:

hexachloroplatinlc acid solution to the sample. Assemble theapparatus as shown in Fla. X3.1 aud 8tm 1\ very aendestream or nitrogenthrouah the sys\em.

NOTEXU-A now of about 30 c:m'/min is aatisl'Ktory.Ir IheIImpl!:dissolvosrapidly, Ihe now IbO\lldbe dtcrCNiIdduri8l1the timehydroaea is freelylibe..ted.

X3.3.7.S Coatinue tho hcatiD8 alld flow"fnitrogen untilthe sample is completmy dissolved. then continue for 5 min(Note X3.6).Separatethe sas deliverytubes(rom the evolu-tion head and remDve the m:civin8 Oaskwith the deliverytube.

NOT! X3.1-Tb,sol"licJn In die reeeiYin. Oask\~ n:mal" alkalir.etbJousho\tt the dissolution period if the hot ~llatt Wll'lplraM'e and tbenitroaen now are proporly IdJlIstcd. Additional 8mMClnillcalzillc IlIlf.tesolution may beaddld, if 1Iec:essary.but tile IImplf: lihould be c1iIeardeciIf the rcceivlnl solll\loo btcoma acidic: (leA thJn pH '7 by \1St paper).

X3.2.7.6 Add I mI. of the starch-Iodide solution and 5mL of diluted HCI (11'I) and mix. Titr-ateImmediately withStandard potassium iodate trom a tO-mL burtt to the firstblue color. Draw some of the soluticln into the delivery tubewi\h a Nbber bulb and ~lease along the Deckof the na$ktowash down any adherins zinc sulfide. Swirl tM solution towash the O\ltside of the tube. Continue the titration to apermanent blue color.

X3.2.1.7 Run a blank titration to the samt $tarch.iodinecoloron a mixtureor 20 mL ot water,3 mI..of ammoniacalzinCsulfate,I mt of starch-iodatesolutionand 5 mt ofdiluted h)'drOQhloricacid (1 part UC:Isp sr t.' 9 and 1 p~11water) in a So..mLli.rlenrn,)'or nask.

X3.2.8Caiculation.s-CaJoulatethemasspercentof sul-fide sulfuf as foUo\Vs:

S llid I" t!l (.4 - B )( 0.005~ 0.016) X 100. U I ~su,ur, mauJV. Wwhere:A. = 0.005 N KIO) solution used for the sample titration,

mL,B - 0.005N KJO,solutionusedin theblank,mL,andW - sample used, I.

x.. DETERMINING TH;E NUMBER OF DJSCON11NUmES IN CHROMIUM ELECT.ROPf..ATING. (DUBPERNELL TEST)

,--

X4.1 Pri","iplea/the Me/hadl-Copper will be depositedon nick.elexpDsedthrouGh discontinuities in chromium but

. not on the chromium,providedthat potentialis properly.controlled (kepi Jowenoush to avoid activation of passivechromium).

X4.2 Prepo.rllliol'lolitsl Pitel:X4.2.1Ma$k all edaes not co\lered by the chromium with

a nonconduclive paint or preS$uresensitive tape, includinsthe wire used to make contact to the calhode bar. Aftermasking, clean the speciqlen by sOlkins in a hot alkalinecleaner until the surface Is free or water breaks. A mildsCNbbin, with I 50n brush is helpful. Follow the c:1caninabya thorou&hrinse in cold deionized wIter, then a dip in a 5 "by ma$Ssolutionof H2SO". .

X4.2.2 Make freshly cl~.I\C<isample anodic at 0.8V for 30s in the copper plating ba\h, then switch to cathodic (see Fia.X4.1) 8t appr~ximately 0.2 to O.4V. for 2 min (see NotesX4.J and X4.2.);'CCautJon-Do nOI&0beyond the specified

2J'd

anodic votta,e or tilne becausenickc:1will slowly di&solveorbecome passivated.)

Bath formulatioD-(Don.mdca1)CuSO,.5H2O i UI (250&,L)H2SO, (Spa 1.95) 0.5 m (20-2S.C)Temperature(rO(lm)Anode (copper)Uveentry .

X4.2.3 Following copper electroplating, carel"uJJyremo\'ethe specimen, rinse in cold then hot deionizl:d wa~er.and airdry. The specimen should nOI be wiped where pores orcracks aM to bt counted, nor should the part be force airdried. Drying can be AI:celeratedby ro1lowinSthe last waterrinse by a rinse with aJcohol (ethanol) or other vDlatilewatermiscib)e solvent.

X4.2.4 Tbt copper deposits only on the ullderlyinsnickelthat is exposed through discontinuities (pgR'.Jiand cracks) inthe chromium.

9

6S11-268 S0S N3A31S 'l'~ S2:21 S6. 6J lnr

- -- - - - - - ~-- - -

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41Dt B 45&

X4.3 Asse.ssmenl:X4.3.1 The numberor discontinuitiesin tho chromium

can be estimatedby countingthe:coppcrnodulesdepositedwithin a known area of the specimen or the number of crackaIn a known leftlth. These determinations are facilitated witha sncta11\lllicalmicroscopefittedwith a calibrated",ticle inthe eyepiece,Ot from pbotomicrosraphstakenof a ",presen-tative field of the specimen. (See X4.4 for a pide to the.detennination ot active: cOn'Osionsites in the chromiumlayer.) .

X4.3.2 Currentmeasuredor recorded durina the cathodiccycle,or both.servesas a reliableindi~tor of porosity,[(current remains low «I mA/cm2) durina the cathodic cycle,porosilY is low. Rapidly risins cumnt (6//41 = I to 2mA/mln) and hip (2 to 4 mA/cm2) final current isiddicati\'cof high porosity. Use of a strip chan recorderprovides a pennanent record of the test current. Withexperience, direct counts of nodules of Cu deposited can bereduced to periodic verifications as the f.r silDature. Aqualitative visual check (microscopically) will then sufficeforre,loIlarroutine use.

Nora X4.t-b8le1 potentia).usedI, dependallton ancde~thcdespacing.At IIdiS\anc:eof 8 1010em. 0.2 V usuallyproducestho desiRddeposit.As ,pacinI incroaK'S.th. poI.ntlal can be Incl'O8$Od100.4 V.

NOT!!X4.2-Aner cleani"s. anodle rreatmellt to tepat.sivatt:chro-miumIs essential.Platinatlm. cainbe varied(rom' to S min.Twomin1lteshASbeen found to he near optilnum.With hisht)' porous.chromiuM. lonser times illeur risk Qr merlina the deposit nodules,&ivln.rift to ambiluitin in cauntllli pores(nodules).

X4.3.3PrecQul/(ms-Do not exceed 0.6 V cathodic. Highcathodic potentials CAnactivat~ chromium loaIUy,8ivins riscto spuriouslyhis.hnodulecounu. If this condition is sus-pected, it can be tested by gently wiping the copper ofl'wlth a

..tissue. If copper adbe:m to specimen; it is probable thecathodic potential was too hlah. tbus depositina copper onthe chromium instead or just i.- tho pores.

~

~R, 1

e~.A

V-SOURCE R.:

E~c

A3

eEA- 2-1 + As

A,.R, ...R3

X4.4 Dwl.rmlnGlion of Acllve COIrQJionSit's By Corro-sionTesling: .

X4.4.1 Before\estin& the part shoulci bq,cleanedtoeliminate wacer breaks. Mqneslum oxide. warm water andsoap, or solvents, or 8 combinat.ion therel)l~ tJ\iSht benecessaryfor thorau&h cleaniu8.

X4.4.2To developthe ac;tive corrosion sitcm~subject thepart to the number of houn of CASS exposure corre--spondln8 to the corrosion spedfication for tho requiredservice condition And thickness specification. After CASSlestin,.ril15ethe part in warm waterto removeIhesaltlayer.If the part contains corrosive product scaininn,it can bewashed with a very mild sponge in warm waterbut the paRshould not be. subjected 10 an)' abrasivecleaning. Afterdryint either by hot air or solvent suchas n~ethanol.the panshould be examined at a masnificAtion between100 and2001.and the active pan: size Dnd densitydetermined.Theconadin, pore sites are typically distinctly latger than theunconodcd sites Ind havea darker and roushertexture. Bymeans of photosraphsat I 'known magnification,the activepore site$ can be counted and the "cUVt $it-CI.per Ireacalculated. Different photographs should be taken at thesame magnificationat all significantsurfacesand cunentdensities to recordthe ditrerencesin pore densityand sizeafter corrosion. As a auide, the: averaac dJanleter orthe activesites should not exceed0,032 mm (0.00125 in.) and thelargest individual site should not exc«d 0.063Smm (0.0025in.).Comparisonswith krJownpore densitychans can be '

usedfor determinationorthesiteSpersquarecenthnetre.X4.4.3 Even thouah the nec:essary work has not been

conductedto estabUshacorrelationbetweenactivecorrosionsitesand stanina aiteles measuredby DubpemeU. it appeanthat for a givencurrentdensityand depositsystemthereis acomlation between the number of poresbefor~corrosionandthenumberoractive corrosion sites anerCASStestina.Once this corrtlation he been establishedat a giveninstal.lation, a simple 100 to 200 X viewina or a pan misht

s . 1.DPDr switCI'lposilion 1 . cathodicpasltlan 2 . anodic

Ec. Rs. R + R + R NOT!: Ammeterand voltmcuercan. . ~ tie replacedbya 2 .ChannelSlr1p

chart recorder.

Schamlltle DI o. . 8"10111"8App.,.tua t6 ConvenlenllyCe/ltl'OIPOltlrltr81111Volta;. DUrI,,-Para.l" T.8t1nllVIIeo,pttO,poIlUOft

Fla. X4.1

Et'd

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. 1456~

nond~tructiveJy indicate the service perfonnance of the panafter carTasian. The desired number of active corrosion siteshas not been definitely established. This number dependssomewhaton the sizeof the poresbeforeandaftercorrosion.

the thicknessand potentialsor the d~J)ositIystem.and thedesired trade-off betwetenbasis metal corrosion and stainin,in CASSo

TII' AmI,IeMl Sac/lly lor TNtlng and MII"I./s ,.k.. 110poJiI/oII fM/»Cllfl8111eIlllitJUy0I8IIJ' .,"" 11"", ual1tld In lItJII/ICll:I/ott...IIh fII'/ /t,m /llt1l1/0llH in llIi. .,.~tI'tI. U8Ir. of tit" "IfIdllfl 81. .1IptNI/r IlMnd th.8r tI.,1tfffIInfI1OII fII .fIt rJ11(11tycf Illy .IICII",lflll IIIfI'" IIJd flit litlt 01 W,/rIgamInI of '1Ia" tlQhll, '" 'III/IIIY .hllf own ftIPOIIIClIII//J.

1ft;' "lIItJIrd 1&allbj8cl to ,,1I1J/oItII 811;litnt by tfle ftIIptJI!.lb1. teeMl. "",,","It end mUll III mlMNd ftWty 1M y"" ",dIfnotrlftlled. ,II/Iff 'NPP'OtlttJor...ltM",*n. YIIIIICommtll/. 11. 1ft'll/lidIIrhtf tOl ffWI.1Ot'I01m/ft,tw"" orIll'fdtll/II)I'II/lllI1dt/(f,an~ ,"ovItI btI .tl6na8tJ 10 ASTM I/NdqLlllf".. VO/,/,oOlMltIll,winftCl/'tt Utetut OCIIIlldtratfon., . r/Ifellnt oJ"'" nllWit/biotllOllnlc81 QQmmtnH. wlrlcll JfOIIm.yan'lId. II ycu 1881Ih" ruur ~r. haV8 tIOIllCllvIft . "" NfI/lIQrw ,fIouIdfNkI '/OfIIII",",,! It"",,, 10 111.AIm Corrtmilr- 0/1Sll/Irll1d., fff8 AIel St.. PtlJlJtllIpIIl.. PA flt03.

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(;qIYI':f.ht f,mericanSocie~yfor Testing:md Matori<ltE(ASTM).1916 RaCI!Streel,~hiladclphia.PA 19103. UnitedStatesoff\meflc:tThiscopyhasbeenmadehyDocumentEnp,ineeringCo.,Inc. underlicansetrnrnA~~n.1.

II

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