application pack for the ecolabelofficial use only - application number ..... / ..... / ........

OFFICIAL USE ONLY - APPLICATION NUMBER ........ / ......... / .........

APPLICATION PACK FOR

THE ECOLABEL

PART 2:Application form for detergents for dishwashers

[Insert date of issue]

[Insert name of Competent Body and contact details, including address, telephone and faxnumbers, e-mail address]


Introduction

1. This part contains an application form for applicants for the Ecolabel for detergents fordishwashers, with annexes containing the full technical criteria for detergents fordishwashers (in Annex 1), the description of the two approved performance testmethods (in Annex 2), the Detergent Ingredients Database (in Annex 3), theenvironmental matrix calculation programme (in Annex 4), and a list of approved testcentres (in Annex 5);

Product group definition and criteria2. The product group definition for detergents for dishwashers is set out in the box below.

The product group detergents for dishwashers comprises all detergents intended foruse exclusively in automatic domestic dishwashers and all detergents intended for usein automatic dishwashers operated by professional users but similar to automaticdomestic dishwashers in terms of machine size and usage

3. Criteria for the Ecolabel for detergents for dishwashers have been agreed by takinginto account various impacts at each step of the products life, such as water pollution.They are listed in the formal Commission Decision of 29 November 2002 (see Annex1).

4. The criteria aim in particular at promoting:

reduction of water pollution both by reducing the quantity of detergent used andby limiting the quantity of harmful ingredients.

reduction of energy use by promoting low temperature detergents.

the minimisation of waste by reducing the amount of primary packaging.as well as setting an appropriate standard for the fitness for use of the final product.Appropriate tests also ensure that the different type of products conform to certainquality standards.

5. Additionally, the criteria enhance the consumers environmental awareness. Thecriteria are set at levels that promote the labelling of detergents for dishwashers thathave a low environmental impact.


6. The criteria will be valid for five years (from 1 January 2003 until 31 December 2007),when they will be revised. During the period leading up to the revision, due attentionwill be given to the following issues:

• Fragrances, including their possible health effects• Matrix versus pass/fail criteria• Total chemicals• The impact on energy use• Safety issues, such as risks for children or contact with eyes• Reusable and recyclable packaging• Dosage with respect to machine size• Widening the product group to include more products for industrial or institutional

use


Health, safety and other environmental requirements

7. Products awarded Ecolabels must also comply with the general provisions of theRegulation. Article 2 of the Regulation states that the label may not be awarded tosubstances or preparations classified as very toxic, toxic, dangerous to theenvironment, carcinogenic, toxic for reproduction, or mutagenic in accordance withCouncil Directive 67/548/EEC or Directive 1999/45/EC, or to goods manufactured byprocesses which are likely to significantly harm man and / or the environment, orwhich in their normal application could be harmful to the consumer.


Application for the EU Ecolabel for detergents fordishwashersSection 1 of this pack describes how the Ecolabel application should be assembled, and theprocess of assessment to ensure that the product complies with the criteria. Compliance isshown by a mixture of tests and applicants declarations, as indicated in Section 2 of the form.

Applicants should complete Sections 1 and 2 of this form (in black, either typescript ormanuscript) and submit in duplicate - as a paper copy, not by e-mail - to the Competent Body.

Applicants should also provide a technical dossier of laboratory test reports, and sendthis in duplicate to the Competent Body, and keep an up-to-date file on their premises to showcontinuing compliance with the criteria. The dossier should include an illustration of howapplicants intend to use the Ecolabel on the product and packaging, so that the CompetentBody can satisfy itself that the label will be properly used.

Section 1 – models of letter and documents to fill byapplicant

Please complete or type in black,and submit in duplicate(as a paper copy, not by e-mail) to the Competent Body

For official use

A. The applicant

Full name of applicant company:


Address:

Contact name, and function:

Tel no, and fax no:

E-mail:

Website:

In what capacity are you applying for the Ecolabel? (manufacturer, importer,service provider, trader or retailer)


B. The product

Registered trade name(s) of product or product range:

Model names (or internal reference numbers) for products to be covered bythe label within the product range above:

Please describe the type of product:

Category: [include this question only if relevant to the product group]

Range: [include this question only if relevant to the product group]

Characteristics: [include this question only if relevant to the product group]

Main composition:

Name and address of manufacturing site (if different from above):


Where the product is made outside the EU, please confirm that it has been orwill be placed on the market in the [insert name of Competent Body’s country](see paragraph 6 of Part I of this pack):

Other EU countries in which this product is manufactured in the same form(please give addresses of manufacturing sites):

Other EU countries in which this product is sold (if sold under differentnames, please give names):

Rough estimate of annual number of articles produced:NB: this means items as sold on store shelves so if goods normally sell indouble packs, the double pack is one item or unit

Rough estimated value of annual sales, excluding VAT, in the EuropeanEconomic Area (ie the European Community plus Norway, Iceland andLiechtenstein) of the product at ex-factory prices (in £ sterling/ in € etc.,please specify currency): ie before transport to the purchasers premises orthere is a wholesalers or retailers profit so excluding the cost of carriage,carriage insurance, and settlement discounts, but including any bulk discount(which is where the customer is offered a percentage reduction in the total pricewhen ordering large quantities of goods).


C. This application

Is this the first application for the EU Ecolabel for this product? (if not, whenand where was the first application made, and with what outcome?)

Is this an application to add a new product (that is, with a technical formulationnot covered by an existing Ecolabel that you hold) to a licence for a productrange already covered by an Ecolabel? (if so, please give details of the existingEcolabel)

Please name any other environmental labelling schemes under which theproduct has already been registered, such as the Nordic Swan:

The assessment and certification method I have used is:certified self-assessment / independent third party assessment: (please saywhich)

The approved test centre is: (see Annex 2 or individual application packs for alist)

The Competent Body will invoice applicants for a non-returnable application feeon receipt of the application. If the application is successful, the Competent Bodywill invoice the licensee for an annual fee, as explained in Part 1 of this pack. Itwill apply all relevant reductions.

1. Do you wish to claim a fee reduction as an SME? If so, please provide proofof status.


2. Do you wish to claim a fee reduction for EMAS registration or ISO 14001certification? If so, please provide proof of status.

3. Where the product uses components for which an Ecolabel fee has already beenpaid, the annual fee will be based on the annual sales of the products afterdeduction of the cost value of the components. Do you wish to claim a reductionon these grounds? Please provide details if relevant.


D. Applicant’s undertaking (all applicants must sign and date this undertaking)

As the applicant for an EU Eco-label, I hereby declare that:

I understand and accept the provisions of Regulation EC No 1980 / 2000 on the EUEcolabel scheme, and in particular Article 2, which states that the Ecolabel may notbe awarded to goods manufactured by processes which are likely to significantlyharm man and / or the environment, or which in their normal application could beharmful to the consumer;

I understand and accept the standard assessment and contract procedures proposedby the Competent Body, and accept its terms during the duration of the contract;

I undertake to ensure that the product compiles with the Ecolabel criteria at all timesand to notify the Competent Body immediately of any significant modification to itor to the production processes;

I take responsibility for the correct and proper use of the EU Ecolabel.

Signed:

Name in capitals:

Position in company:

Date:


Section 2 – Compliance undertakings : Summary of testsand results

Where no specific requirements about the test method are stated, the Competent Body simplyexpects applicants to make what they regard as reasonable tests, and to keep the reports on thesetests ready in case they are required. However, applicants are advised to check with their chosenapproved assessor that the assessor would be content with the testing method used.

[insert details of the criteria requirements that the applicant must meet, as far as possible byasking the applicant to tick boxes to declare compliance, and to sign the completed form]

Signed:

Name in capitals:

Position in company:

Date:


Annex 1

Technical criteria for detergents for dishwashers


ECOLABEL ASSESSMENT REPORT AND CERTIFICATION OF COMPLIANCE

PLEASE READ THE FOLLOWING CAREFULLY

This part of the application form is a record of the assessment of the product against the criteria forecolabelling as laid out in EC Commission Decision

Commission Decision 2003/31/EC

A breakdown of the actual data is not required. The applicant is advised to compile a dossier of dataused to demonstrate compliance with each criterion and after application retain it for use in the eventof a challenge to the decision on the award of an Ecolabel.

The Guidance Document for the Application for an Eco-Label for Dishwashing detergents has beenprepared to assist with an application. The applicant is advised to read it thoroughly along with thesupplementary notes for guidance which attached to this Application Form. In particular theapplicants attention is drawn to notes 4.1 - 4.3.


2/2

PRODUCT DESCRIPTION

Name of Product

Category of Product (domesticand/or professional)

Trade Name/Code

Manufactured at

Countries in which Marketed

Tonnage of product onMarket (reporting on March 1strelated to previous year)

SUBSTANCES OR PREPARATIONS CLASSIFIED AS DANGEROUS

Under Article 4(2) of the Regulation, the ecolabel may only be awarded to products containing asubstance or preparation classified as dangerous in so far as the product meets the objectives set outin Article 1. If the product contains a dangerous substance or preparation, and you consider thatnevertheless the product should be awarded an ecolabel, please indicate why you consider that theproduct meets the objectives in Article 1. Please continue on a separate sheet if necessary.

Substance/Preparation Classification Reasons for inclusion in Product


2/3

1. GENERAL

1.1 General Requirements (see Note 4.1)

In order to demonstrate compliance with the Ecolabel criteria, a manufacturer may assemble adossier on the candidate product.

This declaration must be completed by the person responsible for assessing the compliance of thecandidate product with the criteria for Ecolabeling.

ASSESSOR´S DECLARATION

As responsible for assessing the candidate product, I declare that the information provided in theproduct dossier meets the general requirements set out in Commission Decision .. /.../EECEstablishing the ecological criteria for the award of the Community eco-label to detergents fordishwashers

Signed .................................................

Name ................................................... (Block Capitals)

Date .....................................................

Position ................................................

Company Stamp or Seal


2/4

1.2 Product Formulation (see Note 4.2 - 4.3)

The ingredients of the candidate product must be listed below. If an ingredient (except perfume)consists of more than one chemical compound all individual compound must be listed and thecontent specified (in % of the product).

Ingredient CAS.no. (or CI no orother precisedescripition)

DID Number(if applicable)

Content (wt %)


2/5

1.3 Modification of the Product (see Note 4.4 - 4.6)

Once the candidate product has been awarded an Ecolabel, the manufacturer is free to modify theproduct formulation or packaging so long as compliance with the criteria is maintained.

To cover its contingency, the following declaration must be completed by the manufacturer.

MANUFACTURER`S DECLARATION

I/We as person(s) responsible for manufacturing the candidate product agree to inform the CBs ofany changes made to the product, during the entire period of the license, before the changed productis marketed, declaring whether or not the changes to formulation necessitate a new washperformance test.

I/We understand that if changes to the product formulation or packaging result in a break ofcompliance with the Ecolabel criteria, then the changed product will no longer be licensed to carryan Ecolabel.

Name...............................................(Block Capitals)

Signed..............................................

Position.............................................

Date:



2/6

2. FIELD OF APPLICATION (see Note 4.7 - 4.9)

The Ecolabel can be awarded to Dishwashing detergents in powder, liquid, tablet or any other formfor being used in automated dishwashing machines. The Functional Unit for the candidate producthas to be based on the quantity of product required to wash 12 place settings with a standard soil.

The candidate product is a:

Consumer product

I`n`I product. Please specify: ___________________________________

The candidate product form is *:

Powder

Liquid

Tablets

The functional unit for the candidate product is:

................. g/wash

The reference dosage - which is also indicated on the product - is:

................. g/wash for normal soiled dishes

................. g/wash for heavily soiled dishes

................. g/wash for water hardness class 1(**) defined as ..



* delete as appropriate** most dishwashers have water softening devices equipped. Hence the dosage will be the same forall water hardnesses because Calcium and Magnesium ions are removed by the softening device. Themanufacturer must indicate what dosage the consumers that use dishwashers without softeningdevices should use.


2/7

3. CRITERIA

1 Environmental scoring matrix (see Note 4-10 and calculation programme)

CriterionDosage (g)per wash

Excl.Hurdle

Score WeightingFactor

Sum

Total chemicals 22.5 3

Critical Dilution Volume, tox 200 8

Phosphates (as STPP) 10 2,5

Non-biodegradable organic(aerobic)

1 1

Non-biodegradable organic(anaerobic)

0.2 1.5

TOTAL ( > 30 )


2/8

3.3 New Chemicals/Additional Ingredients (see Note 4.12)

In the case of new chemicals or additional ingredients not listed in the Detergent Ingredients Database,the assessor must complete the following declaration and enter the summary data in the table inapplication form 2/9.


As responsible for assessing chemicals used that are not listed on the DID, I declare that theexperimental data for the candidate product provided by the manufacturer support the values forToxicity, Loading Factor, Anaerobic Non-biodegradability, Aerobic Non-biodegradability aresummarised on page 2/9 of this Application Form.

Signed ............................

Name .............................. (Block Capitals)

Date ................................

Position .................................



2/9

New Chemicals/Additional Ingredients (see Note 4.12)

Toxicity * CF = Correction Factor (see Annex III, part 2)

Ingredients

NOEC

Measured

LTE LoadingFactor

Anaerobic

Non Biodegradable

Aerobic Non Biodegradable

CF *

OFFICIAL USE ONLY APPLICATION NUMBER ...............

2/10

2. Biodegradability of surfactants

a) All surfactants used in the product must be easily biodegradable, both under aerobic andanaerobic conditions.

This declaration must be completed by the manufacturer.

DECLARATION FROM THE SURFACTANT MANUFACTURER

I/We as Person(s) responsible for manufacture of the surfactant, declare that the surfactant meets thefollowing criteria:

a) The surfactant is readily biodegradable.

Compliance can be demonstrated by referring to the relevant DID-list number. If the compound is not onthe list or it is not indicated as readily biodegradable, biodegradation tests must be performed.Documentation can be test report or copy of published data.

b) The surfactant is anaerobically biodegradable.

Compliance can be demonstrated by referring to the relevant DID-list number. If the compound is not onthe list or it is not indicated as anaerobically biodegradable, biodegradation tests must be performed.Documentation can be test report or copy of published data.

Name................................................... (Block Capitals)

Signed......................................

Position....................................

Date:



3. Dangerous, hazardous or toxic substances or preparations

Certain specific ingredients shall not exceed a maximum content in the detergent formulation or areexcluded. This declaration must be completed by the manufacturer.

MANUFACTURER´S DECLARATION

I/We as Person(s) responsible for manufacture, declare that the candidate product meets the followingcriteria:

a) The candidate product does not contain ingredients which are classified as having one of the following riskphrases as defined in directive 67/548/EEC and 88/379/EEC:

R40 (limited evidence of a carcinogenic effect)R45 (may cause cancer)R46 (may cause heritable genetic damage)R49 (may cause cancer by inhalation)R60 (may impair fertility)R61 (may cause harm to the unborn child)R62 (possible risk of impaired fertility)R63 (possible risk of harm to the unborn child)R64 (may cause harm to breastfed babies)R68 (possible risks of irreversible effects)

Each ingredient of any preparation used in the formulation that exceeds 0.01% by weight of the finalproduct shall also meet this requirement.


Signed......................................

Position....................................

Date:





DECLARATION FROM MANUFACTURER OF THE INGREDIENT

I/We as Person(s) responsible for manufacture of the ingredient ., declare that the ingredientmeets the following criteria:

a) The ingredient should be evaluated according to the classification limits for the risk phrasesR50/53 and R51/53 as defined in directive 67/548/EEC and 88/379/EEC. Any ingredient thathas not been evaluated will be regarded as having the risk phrase R50/53. Each ingredient ofany preparation used in the formulation that exceeds 0.01% by weight of the final product shallalso meet this requirement.

The ingredient:Fulfils the limits for classification as R50/53 Fulfils the limits for classification as R51/53 Does not Fulfils the limits for classification as R50/53 or R51/53 Has not been evaluated

There are not enough test results to evaluate the ingredient regarding these risk phrases but thefollowing scientific data and reasoning strongly indicates that the ingredient should not beclassified as harmful to environment with one of the mentioned risk phrases. Please give adetailed account in an enclosure.


Signed......................................

Position....................................

Date:



2/11





b) No preservatives shall be used that are or may be classified as R50-53, as laid down in Council Directive67/548/EEC and its subsequent amendments or Directive 1999/45/EC and its subsequent amendments,whatever their amount.

c) The following ingredients shall not be included in the product, either as part of the formulation or as part ofany preparation included in the formulation:

• alkylphenolethoxylates (APEOs) or other alkyl phenol derivatives (APDs).

• EDTA (ethylene-diamine-tetra-acetate)

• NTA (nitrilotriacetate) d) The quantity of phosphonates that are not readily biodegradable (aerobically) does not exceed 0.2 g/wash.


Signed......................................

Position....................................

Date:



2/10

4. Fragrances

Certain specific ingredients shall not exceed a maximum content in the perfume formulation or areexcluded. This declaration must be completed by the manufacturer of the perfume.

DECLARATION FROM PERFUME MANUFACTURER

I/We as Person(s) responsible for perfume manufacture, declare that the perfume meets the followingcriteria:

(a) Nitromusks and polycyclic musks.Nitromusks and polycyclic musks shall not be included in the product, either as part of the formulationor as part of any preparation included in the formulation. This concerns, amongst others, the following:

musk xylene:5-tert-butyl-2,4,6-trinitro-m-xylenemusk ambrette:4-tert-butyl-3-methoxy-2,6-dinitrotoluenemoskene:1,1,3,3,5-pentamethyl-4,6-dinitroindanmusk tibetine:1-tert-butyl-3,4,5-trimethyl-2,6-dinitrobenzenemusk ketone:4'-tert-butyl-2',6'-dimethyl-3',5'-dinitroacetaphenoneHHCB:1,3,4,6,7,8-Hexahydro-4,6,6,7,8,8-hexamethylcyclopenta(g)-2-benzopyranAHTN:6-Acetyl-1,1,2,4,4,7-hexamethyltetralin

Each ingredient of any preparation used in the formulation that exceeds 0.01% by weight of thefinal product shall also meet this requirement.

(b) Code of practiceAny ingredients added to the product as a fragrance shall have been manufactured and/or handledfollowing the code of practice of the International Fragrance Association.


Signed......................................

Position....................................

Date:



5 Ecological Criteria on Product Packaging (see Note 4.11)

Packaging MaterialA sample of the primary packaging must be submitted to the Competent Body assessing the application.

The packaging is: Plastic / Metal / Cardboard *

* delete as appropriate

a) Primary Packaging Weight

The calculation of the weight of primary packaging must be given in detail. The weight of primarypackaging is

........................ grams per wash

b) Percentage of recycled material of cardboard



Cardboard primary packaging shall consist of ≥ 80 % recycled material.


Signed......................................

Position....................................

Date:



5. CONSUMER INFORMATION

5.1 Information on the packaging (see Note 4.14)

The following information shall appear on the product in such a way as to be clearly visible forconsumers. This declaration must be completed by the manufacturer.

MANUFACTURERSS DECLARATION

I/We as persons(s) responsible for manufacture, declare that - as a general rule - the followingstatements appear on the packaging of the candidate product:

This eco-labelled detergent works well at low temperatures (***). Select lowtemperature washing cycles on the dishwasher, wash full loads and do not exceed therecommended dosage. This will minimise both energy and water consumption and reducewater pollution.

For more information about the Flower: http://europa.eu.int/ecolabel.

*** The applicant shall insert here the recommended temperature or range oftemperatures that shall not exceed 55°C.

Name..................................................(Block Capitals)

Signed......................................

Position....................................

Date:



2/12

5.2 Dosage Instructions (see Note 4.15)

Dosage instructions shall appear on the product packages. The recommended dosages shall bespecified for normally and heavily soiled dishes, and for the ranges of water hardness appropriateto where the product is marketed. The instructions shall specify how to make best use of the productaccording to the soil. The instructions should specify that if a softening device is used the dosageshould be the same no matter what the water hardness is. If the dishwasher does not have a softeningdevice, the dosage must be varied according to the water hardness. Accordingly the dosage fordifferent water hardnesses must be given, together with a notice that this only concerns machineswithout a softening device.

The applicant shall take suitable steps to help the consumer respect the recommended dosage, forexample by making available a dosage device (for powdered or liquid products), and/or by indicatingthe recommended dosage at least in ml (for powdered or liquid products). A recommendation shallappear on the packaging for the consumers to contact their water supplier or local authority in order tofind out the degree of hardness of their tap water.

5.3 Information and labelling on Ingredients (see Note 4.15)



(c) Information and labelling of ingredientsI/We as person(s) responsible for manufacture of the candidate product, declare that the CommissionRecommendation 89/542/EEC on the Labelling of Detergents and Cleaning Agents will to beapplied to the product.

In particularly the following groups of ingredients will be labelled independently from their masscontent:

• Enzymes: indication of the type of enzymes • Preservation agents: characterisation and labelling according to IUPAC (International Union of Pure

and Applied Chemistry) nomenclature • If the product contains perfume, it is indicated on the packaging.

The exact wording is indicated in the product dossier.

Name......................................................(Block Capitals)

Signed..........................................

Position........................................

Date:


2/13

6. EXCLUSION OF INAPPROPRIATE INFORMATION (see Note 4.16)OR ADVERTISING CLAIMS



I/We as person(s) responsible for manufacture of the candidate product, declare that product andadvertising claims are in conformity with Directive 84/450/EEC concerning misleading advertising.

Neither we nor our agents shall use any form of advertising or product claim whichwould mislead a potential buyer of the product.

Documents justifying the validity and accuracy of any claims made in advertisements relating to theproduct or on the product packaging about environmental aspects of the candidate product are includedin the documentation submitted to demonstrate compliance with the ecolabelling criteria.

Name.......................................................(Block Capitals)

Signed.........................................

Position.......................................

Date:



2/14

7. TEST ON PURITY OF ENZYMES (see Note 4.17)

A test of the purity of enzymes has to be performed on enzymes which are produced by bio-techno-logical processes and are used in dishwashing detergents applying for an Ecolabel. It is the aim of thistest to ensure that production organisms are not contained in the final enzyme preparation.


As responsible for assessing the candidate product, I declare that the experimental data provided forthe candidate product provided by the manufacturer, demonstrate that no production organisms weredetected in a test sample of the final enzyme product.

Signed.................................

Name................................................(Block Capitals)

Date.....................................

Position................................



2/15

8. PERFORMANCE CRITERIA (see Note 4.18 - 4.20)

The candidate product must be compared in its washing performance with a reference detergent byusing the one of the Test methods described in Annex IV of this Guidance Document.

This declaration must be completed by the person responsible for supervising the performance test.

Name of testing laboratory

Address of testing laboratory

Accreditation standard of testlaboratory

A copy of the test report is attached Yes/No

TESTING DECLARATION

I/we as responsible for performing the performance test for dishwashing detergents declare that thecandidate product was tested as required by one of the test methods described in Annex IV of thisdocument. I/We as persons(s) responsible for assessing the performance test declare that thecandidate product full-fills the minimum requirements for the test which are also defined in AnnexIV.

Test method:Product assessed by: (Block capitals)Signed: Date:

Report checked by: (Block capitals)Signed: Date:



2/16

9. CERTIFICATION OF COMPLIANCE WITH ECOLABEL CRITERIA (see Note D.21)

For all applicants this declaration should be completed by the person responsible for assessing that thecandidate product complies with the criteria.

I/We as responsible for carrying out the assessment required for this application for the Ecolabel fordishwashing detergents, declare that the data and calculation of ingredient and packaging criteria are atrue record of the results and that the product

.............................................................(Name of Product/Type)

meets the criteria laid down in the Commission Decision 2002 / yyy /EC establishing the ecologicalcriteria for the award of the Community eco-label to detergents for dishwashers.

Product Assessed by.......................................(Block Capitals)

Signed...................................

Position..................................

Date.......................................

Report Checked by.........................................(Block Capitals)

Signed....................................

Position...................................

Date........................................


42

Annex 2

Technical criteria for detergents for dishwashers

Performance tests

1. Method 1 (IKW-test) for ascertaining the cleaning performance ofdishwasher detergents (PC-version only)

2. Photo Catalogue for the Evaluation of the IKW test CleaningPerformance (PC-version only)

3. Reference Detergent and Pass/Fail-level (IKW test)

4. Method 2 (Modified EN 502 42) for ascertaining the cleaningperformance of dishwasher detergents (The actual test protocol must beacquired from the National Standards Organisation).

5. Modification of EN 502 42.

43

1. Method for ascertaining the cleaning performance ofdishwasher detergents (IKW-test)

Introduction

In 1995, under the auspices of the German Industrial Association of the Manufacturers ofToiletries and Detergents (IKW), a work group of mechanical dishwashing experts was set up,which was joined by representatives of leading European test institutes and dishwashermanufacturers. The goal of this working group was, to choose appropriate soiling methods fromcurrent practice in order to determine the cleaning performance profile of automatic dishwashingdetergents. The methodology and experiences of the working group including the methodsdeveloped were presented in part A of the publication (SÖFW-Journal 124, 11/98, 702 pp., inGerman). Part B (SÖFW-Journal 124, 14/98, 1022 pp., in German) describes in detail theprocedures to test the performance of an automatic dishwashing detergent.

44

Instructions for preparation/ Test soils/ Test procedures

Contents Page

1. Preface 16-------------------------------------------------------------------------------------------------------------------

Bleachable stains

2. Tea 18-------------------------------------------------------------------------------------------------------------------

Persistent, burnt soil

3. Minced meat on glass dishes 19

4. Milk in the microwave 20-------------------------------------------------------------------------------------------------------------------

Amylase-specific soil

5. Starch mix (by analogy with IEC SC 59A / WG II) 21

6. Porridge (in accordance with EN 50242) 24-------------------------------------------------------------------------------------------------------------------

Protease-specific soil

7. Egg yolk 25

8. Minced meat on porcelain plates(by analogy with EN 50242) 27

9. Egg/milk 28--------------------------------------------------------------------------------------------------------------------Appendix 1 Loading plan taking the example of the Miele reference dishwasher--------------------------------------------------------------------------------------------------------------------Appendix 2 Apparatus and raw materials--------------------------------------------------------------------------------------------------------------------Appendix 3 Production instructions for ballast soil--------------------------------------------------------------------------------------------------------------------Appendix 4 Production instructions for hard water--------------------------------------------------------------------------------------------------------------------Appendix 5 Calibration instructions for the microwave oven--------------------------------------------------------------------------------------------------------------------Appendix 6 Photo catalogue--------------------------------------------------------------------------------------------------------------------

45

1. Preface

1.1 Selection of soil typesFor the test, at least one of each of the 4 soil types (bleachable, persistent/burnt, amylase-specificand protease-specific) is to be used. As the minced meat soil on porcelain plates and porridgesoils, due to the influence of the alkalinity of dishwashing detergents do not constitute purelyenzyme-specific soil types, but can also be included to some extent in the "persistent/burnt"category, at least one other enzyme-specific soil type should be included in the selection of thesesoil types.

To produce the individual soil types, synthetic water rather than tap water should be used, with thehardness raised to 3.00 mmol (Ca+Mg) = 16.8 °d in accordance with the draft IEC 734, 2ndedition, method B - salt mixing technique (see Appendix 4).

1.2 Thorough washing of the crockery/utensilsBefore the individual soil types can be applied, the various dishes must be thoroughly washed.This is particularly necessary as residues of certain persistent stains may still be present on thedishes from previous tests. New dishes should also be subjected to three thorough washes beforebeing used for the first time in a test. The initial washing is carried out in a laboratory dishwasherat 95°C with a special, commercial dishwashing detergent of high alkalinity and containing activechlorine (e.g. Perclin Supra, Henkel Ecolab).

1.3 StorageThe soil should be stored in controlled conditions of 20°C/40 - 60% relative humidity as weighingerrors may occur particularly with gravimetric soil types due to varying levels of water content onthe surface of the crockery.

The storage life under the above conditions is at least 14 days.

1.4 Preparation of the detergent samplesThe samples to be tested should be as representative as possible of the detergent formulation underexamination. It is therefore necessary to pass the contents of a test package of the detergent inquestion through a sample divider before taking samples for the detergent tests.

1.5 Procedure / Test conditionsThe detergents are tested following the criteria used by the German Stiftung Warentest and thefollowing parameters were chosen:

Program : Universal 55 °C with prewash

No. of test runs : At least 3 tests are to be carried out.

Water hardness : 8 - 10°d (1.4 - 1.8 mmol Ca+Mg) in the main wash.

Detergent dosage : The detergent is dosed in accordance with the manufacturer'sinstructions. In the case of no dosage instructions being available, thefollowing dosages are recommended :

Classical detergents IEC type A 30 g

46

Compact detergents IEC type B/C 20 g

No. of soiled items : 6 of each kind

Additional ballast soil : 100 g of ballast soil in the form a frozen lump in the main washcycle.The frozen soil consists of food ingredients (Appendix 3), includingstarch, protein and fat containing components. Additionally,ingredients that impart color, e.g. ketchup and mustard, are alsoincluded. This additional soil is to simulate the presence of easilyreleased food residues and thus additionally burden the cleaningsolution.

Use of rinse aid : It is left to the test laboratories' discretion whether to use a rinse aid.

Machine load : For the dish loading plan, see Appendix 1 which uses the example ofthe Miele G 590 reference machine conforming to EN 50242. Ifanother test machine is used, the loading should comply with theplan as closely as possible

47

2. Tea

2.1 Apparatus• Tea cups: The cups should have a wall thickness of 6-8 mm (e.g. Bauscher, Art. No.

6215/18)• Pipettes 100 ml, 20 ml or automatic metering pump• Strainer, mesh width 0.5 mm• Container for boiling and pouring out the tea• Eppendorff pipette (0.1 ml)

2.2 Raw materials

• Tea (Assam, e.g. Lipton)• Synthetic water, (hardness raised to 3.00 mmol (Ca + Mg) = 16.8 °d, conforming to

draft IEC 734, 2nd edition, method B - "salt mixing technique", cf. Appendix 4)• Stock solution of ferric sulfate

2.3 Pretreatment of the cups See preface (thorough washing). 2.4 Preparation (for approx. 20 cups) Mix 2 liters of hardness-enhanced water with 0.1 ml of ferric sulfate solution and bring it to theboil. Pour boiling water onto 30 g of tea in an open container and leave to draw for 5 min. Thenpour the tea through a strainer into another temperature-controlled vessel. 2.5 Test The clean cups are filled with 100 ml tea such that the temperature of the tea in the cups is 85°C.The initial temperature of the poured tea is about 93°C. Remove 20 ml every 5 minutes with apipette until all the cups are empty (5 times). Thereafter, this process is repeated once more withfreshly brewed tea. 2.6 Evaluation Visual with reference to the photographic catalogue (Appendix 6) 2.7 Important remarks

- Initial temperature in the cup 85 °C (Temp. of the tea during fill about 93 °C). - Wall thicknesses of the tea cups determine the tea cooling rate - Assam tea is particularly difficult to remove - Thorough washing of tea cups:

Household dishwasher/65°C/detergent IEC A or laboratorydishwasher/95°C/commercial detergent

- When drawing off the tea, make sure that the tip of the suction device penetrates theskin of the tea before starting to draw off the tea.

- Before washing, the soiled cups are stored for at least 3 days in a room with constantconditions (20°C, 60 % relative humidity). It has been shown that when synthetic water is used whose hardness has beensupplemented solely with Ca and Mg ions, the tea cups were not stained darkly enough.For this reason it was decided to add ferric ions to the synthetic water to produce adarker tea stain.Production of the ferric sulfate stock solution:In a 1 litre beaker dissolve 5 g Fe2(SO4)3 (see chemical list) + 1 ml HCl (37 %) in

48

demineralized water and fill to 1 litre. Using an Eppendorf pipette add 0.1ml of thestock to 2 litres of tea.

3. Minced meat on glass dishes 3.1 Apparatus

• Drying oven (recirculating air) up to 300°C (e.g. Heraeus UT 6120, 104 liter volume)• Crystallizing dishes (e.g. Duran/Schott, dia. 115 mm, height 65 mm, Order No.

213114908)• Mincer (hole diameter 3 mm)• Rubber wiper• Freezer cabinet• Kitchen hand blender

3.2 Raw materials• A total of 225 g lean pork and beef (half and half)• 75 g egg (white and yolk)• 80 ml synthetic water conforming to IEC 734 - draft (Appendix 4)

3.3 Preparation Put the finely chopped and cooled meat (after removing visible fat) consisting of equal quantitiesof beef and pork through the mincer twice. Avoid temperatures in excess of 35°C. Mix 225 gminced meat with 75 g egg (white and yolk) with a fork and freeze (can be stored for 3 months at-18°C). To soil the dishes, bring the mince-egg mixture (300 g) up to room temperature, mix it with 80 mlsynthetic water and subsequently homogenize it with a kitchen hand blender for 2 min. Weigh 3 g± 0.1 g of this mixture and place in each glass dish. Uniformly distribute the mince on the basewith a spatula-shaped rubber wiper. The weighed minced meat should not be allowed to stand formore than 30 minutes before processing it further. 3.4 Baking conditions Preheat the drying oven to a value which yields 200°C after inserting the glass dishes (determinebeforehand experimentally). After loading, reset the temperature controller to 200°C. Bake for 10min at 200°C. After removal of the crystallizing dishes, only fill when the initial temperature has been reached. 3.5 Evaluation Visual, with reference to the photographic catalogue (Appendix 6). 3.6 Important remarks

− If no pork is available, beef alone can be used.− Make sure that the temperature after inserting the glass dishes in the drying oven does

not drop below 200°C.

49

4. Milk in the microwave 4.1 Apparatus

• Microwave oven with a glass rotating plate, at least 750 W output (e.g. Bosch HMT752), without an overload cutout, calibrated

• Glass beakers, 150 ml, short form (dia. 60 mm, height 80 mm)(Caution, pictures in photographic catalogue 250 ml/tall form)

• Serial dispenser (e.g. Fortuna Optifix Basic 10 ml, Graf, Wertheim)• Thermal cabinet (recirculating air)

4.2 Raw materials• Semi-skimmed UHT milk (1.5% fat, ultra-high temperature, homogenized)

4.3 Preparation Set the microwave to an output of 450 W (see calibration instructions in Appendix 5). To preheatthe microwave, arrange 6 glass beakers containing 50 ml water symmetrically around the edge ofthe rotating plate and heat them for 10 min. Then pour 10 ml milk at room temperature into eachof the 6 glass beakers and arrange them in the same pattern as the beakers of water on the rotatingplate and heat them in the manner described below. Make sure that the baking time is preciselyobserved in order to ensure that the results are reproducible. After baking, the milk soil is post-treated for 2 hours at 80°C in the thermal cabinet. 4.4 Baking times The baking time is 10 min at 450 W. As the actual output of microwave ovens may deviate fromthe setting, it should be checked every three months, in accordance with the relevant instructions(conforming to EN 60705, see Appendix 5). Depending on the degree of deviation, the bakingtime should be adapted either with an independent time switch or, in the case of microwave ovenswhich can be set to the nearest second in the 10 minute range, by varying the oven's own timesetting. The exact baking time (in seconds) should be marked on the microwave together with its period ofvalidity. 4.5 Evaluation Visual in accordance with photographic catalogue (Appendix 6). 4.6 Important remarks

− Microwave without a safety cutout− Keep to the specific heating time with accuracy to the nearest second− Regular calibration of the microwave

50

5. Starch mix 5.1 Apparatus

• Water bath (e.g. IKA TS 2)• Glass beaker (depending on the quantity of the mixed starch)• Glass beaker for weighing the starch• Electric laboratory stirrer + blade-type agitators• Serial dispenser (e.g. Fortuna Optifix, Graf, Wertheim)• Glass plate, arcoroc®, "Octime" series, Cristallerie d'Arques, black, octagonal, dia. 25

cm (from edge to edge), inner surface area 270 cm2, individually numbered• Rack for storing and predrying the soiled plates horizontally• Thermal cabinet (recirculating air), e.g. Memmert• Balance, e.g. Sartorius LC 1201 S (weighing range up to 1200 g, weighing accuracy 1

mg) 5.2 Raw materials The following types of starch from Merck are required:

• Potato starch: No. 1259• Maize starch: No. 11686• Rice starch: No. 11684• Wheat starch: No. 11685 • Synthetic water as defined in Appendix 4

5.3 Preparation Make a quantity of 0.65% starch suspension appropriate to the number of plates to be soiled. Example for a 1000 g batch Weigh 993.5 g cold synthetic water as described in Appendix 4 in a 2 liter glass beaker. Place theglass beaker in the water bath before it is switched on and position the stirrer as close as possibleto the base. Weigh 1.625 g of each of the four starch types (total weight 6.5 g) and pour into thesecond glass beaker. Stirring continuously, transfer the starch mixture into the beaker of cold water. Cover the glass beaker containing the starch mixture (e.g. with aluminum foil) and place in asimmering water bath, stirring continuously, until a temperature of 95°C is reached. Continuestirring at this temperature for a further 10 min. Then remove the glass beaker from the water bathand, stirring continuously, allow it to cool to room temperature. Add an appropriate quantity ofwater to compensate for any water evaporation loss (reweigh to check). The starch should be stirred continuously but slowly, so that no sediment can form. It should notbe stirred too vigorously, so that the suspension remains free of bubbles and the dispenser does notintake any air.

51

5.4 Starch application/weighing After thorough washing, leave the plates to stand for at least 24 hours. Weigh the plates accuratelyto the nearest mg. The scale should be placed in a cabinet with a door to protect it from airmovements. Now set the dispenser so that about

29.5 ± 0.1 g of the suspension is metered (this is a guide value; the exact setting must be determinedexperimentally beforehand). Using the dispenser, now meter the exact quantity of suspension onto the plates and distribute ituniformly by swilling it over the inner surface. Now place the plates with the starch solutionhorizontally on shelves and leave them there until they are visually dry (overnight). Then stack the plates in plate racks and continue drying for 4 hours at 80°C in the thermalcabinet. After drying, leave the plates to cool for at least 1 hour. Then weigh them. The layer of starch onthe plates should weigh between

0.189 and 0.216 g (0.75 ± 0.05 mg/cm2). Plates deviating from this range cannot be used. If the plates are outside the approved range, thequantity of starch applied can be adapted by varying the quantity dispensed (in this case 29.5 ml). After the wash test, place the plates in the thermal cabinet to dry at 80°C for at least 1 h. After cooling, weigh immediately or within 30 minutes at the latest. 5.5 Evaluation

mg starch released x 100 % cleaning performance = -------------------------------- mg starch applied (dry)

5.6 Important remarks− The quantity dispensed must always be checked before the soiling process. The above

mentioned balance should be used to check the quantity dispensed. Make sure thatthe balance is always horizontal to prevent weighing errors.

− It is advisable to calibrate the balance once a day with a suitable calibrating weight(obtained from the balance manufacturer), particularly if weighing is carried out ondifferent days.

− Protect the balance from drafts by enclosing it.− Store the soiled plates at 20°C/40-60% relative humidity.− If for space considerations the plates are stacked on top of each other, a clean paper towel

should be laid between the plates.

52

− Before applying the starch solution, the plates must be free of surface-active soil asotherwise the plate surface will not be wetted.

− If no laboratory dishwasher is available for thorough washing, it is possible to use theheavy-duty cycle in a household dishwasher with a classical high-alkalinity detergent orthe IEC reference detergent type A.

− To prevent evaporation losses, particularly during the boiling process, aluminum foilcan be used.

− Do not use plates with irregular bases.− Particularly in conditions of low humidity, glass plates can attract a static charge that

can lead to weighing errors. This can be prevented by placing the glass dishes on ananti-static surface prior to weighing.

53

6. Porridge (conforming to EN 50242) 6.1 Apparatus

• Soup plates, diameter 23 cm, white, glazed porcelain (e.g. those corresponding to ENstandard, tableware from Arzberg or similar)

• Magnetic stirrer with hotplate and magnetic stirring table• Stainless steel saucepan• Time switch• Temperature sensor• Thermal cabinet (recirculating air)• Brush for application

6.2 Raw materials

• 50 g porridge oats (e.g. Peter Kölln, tender Kölln flakes)• 250 ml milk, pasteurized (fat content: 1.5%)• 750 ml cold water, synthetic as defined in Appendix 4

6.3 Preparation Stir the porridge oats into the water and milk, heat uniformly and boil for 10 min, stirringcontinuously. Using a brush, evenly spread 3 g of hot porridge on the inner plate surface. Keep the rim of the platefree. Quantity applied/area: 10.6 ±±±± 0.5 mg/cm² Dry the soiled plates for 2 h at 80°C in the thermal cabinet. When they have cooled to roomtemperature, the plates can be washed. 6.4 Evaluation After washing, the remains of the porridge are evaluated by visual inspection with reference to thephotographic catalogue (Appendix 6). To facilitate easier identification of the residual porridge soil, the plates are immersed in an iodinesolution. Prepare the iodine solution in accordance with DIN 44990.

54

7. Egg yolk 7.1 Apparatus

• • Stainless steel sheets (brushed on one side), 10 x 15 cm• Flat brush (pure Chinese hog bristles), 2 1/2"• Glass beaker• If necessary, auxiliary device for manually separating egg yolk from egg white• Fork• Kitchen strainer (approx. 0.5 mm mesh)• If necessary, holding device for immersing and drying (purpose-built)• If necessary, frame for holding device (purpose-built)• Saucepan (round)• Thermal cabinet (recirculating air)

7.2 Raw materials

• 200 g egg yolk (approx. 10 - 11 eggs) 7.3 Preparation The stainless steel sheets to be soiled must be clean and grease-free. To this end, thoroughly wash thenumbered sheets at 95°C in a laboratory dishwasher with a high-alkalinity commercial detergent(1.2). Dry the sheets before soiling (30 min/80°C/thermal cabinet). The brushed surface of thecleaned sheets should not be touched. Weigh the cooled sheets before soiling. Separate the yolks of the raw eggs (if necessary using a special device), stir with a fork in a glassbeaker to homogenize them and pass them through a strainer to remove the coarser particles andfragments of eggshell. Using a brush, apply 1.0 ±±±± 0.1 g egg as uniformly as possible over an area of 140 cm² on the brushedsides of each of the stainless steel sheets, leaving an approx. 1 cm wide unsoiled rim (use adhesivetape if necessary). Dry the soiled sheets horizontally at room temperature. for 4 hours (max. 24 h). For denaturation, immerse the sheets for 30 seconds in boiling, demineralized water (using a holdingdevice if necessary). Then dry again for 30 min at 80°C. After this, weigh the cooled egg-coatedsheets. After weighing, leave the sheets for at least 24 hours at room temperature before submittingthem to the wash test.

Approval requirement: 500 ± 100 mg/140 cm² (egg yolk after denaturation) After the wash test, dry again for 30 min at 80°C in the thermal cabinet and weigh again aftercooling.

55

7.4 Evaluation mg egg yolk released x 100 % cleaning performance = ------------------------------------------------ mg egg yolk applied (after denaturation)

7.5 Important remarks

− To prevent injury, deburr the steel sheets before they are used for the first time.− No water stains or fluff on the surface (visual inspection/repolish if necessary)− Leave the freshly coated sheets horizontal to prevent the formation of droplets on the

edges.− The egg yolk sheets can be stored at 20°C/40-60% relative humidity.

56

8. Minced meat on porcelain plates

8.1 Apparatus• Tea plates (Arzberg, white, glazed porcelain) conforming to EN 50242, form 1495, No.

0219, diameter 19 cm• Fork• Thermal cabinet (recirculating air)• Freezer cabinet• Mincer• Kitchen hand blender

8.2 Raw materials

• A total of 225 g lean pork and beef (half and half)• 75 g egg (white and yolk)• 80 ml synthetic water as defined in Appendix 4• Ninhydrin solution, 1% in ethanol

8.3 Preparation (Preparation as for minced meat in glass dishes as defined in section 3). Put the finely chopped and cooled meat (after removing visible fat) consisting of equal quantitiesof beef and pork through the mincer twice. Avoid temperatures in excess of 35°C. Mix 225 gminced meat with 75 g egg (white and yolk) with a fork and freeze (can be stored for 3 months at-18°C). To soil the plates, bring the mince-egg mixture (300 g) up to room temperature and mix with 80ml synthetic water. Then homogenize it with a kitchen hand blender for 2 min. Using a fork,spread 3 g of the minced meat/egg/water mixture on each white porcelain plate, leaving an approx.2 cm wide unsoiled margin around the rim. Quantity applied/area: 11.8 ±±±± 0.5 mg/cm² Place the plates in the preheated thermal cabinet. Dry for 2 hours at 120°C. The soiled plates can be used as soon as they have cooled. Stack the plates with paper towelsbetween them. 8.4 Evaluation After washing, spray the plates with ninhydrin solution (1% ethanol) for better identification of theminced meat residues. To promote the color reaction, heat the plates for 10 min at 80°C in thethermal cabinet. After washing, the evaluation is carried out by visual inspection of the color reactions of the mincedmeat residues with reference to the photographic catalogue (Appendix 6). 8.5 Important remarks If no pork is available, beef alone can be used.

57

9. Egg/milk 9.1 Apparatus

• Bowl• 50 ml measuring cylinder• Egg whisk• Flat brush• Saucepan (height at least 17.5 cm)• Hotplate• If necessary a holding device for drying and immersing (purpose-built)• WMF stainless steel sheets (brushed on one side), 10 x 15 cm• Laboratory balance (accuracy 1 mg)• Thermal cabinet (recirculating air)

9.2 Raw materials

• 160 g egg (egg yolk and egg white, approx. 3 - 4 eggs)• 50 ml semi-skimmed UHT milk (1.5% fat, ultra-high temperature, homogenized)

9.3 Preparation The stainless steel sheets for soiling must be clean and grease-free. To this end, thoroughly washthe numbered sheets in a laboratory dishwasher with a highly alkaline commercial dishwashingdetergent (1.2) and polish dry with a cellulose cloth. Thereafter, the soiling surface of the cleanedsheets should not be touched. There should be no water stains or fluff on the surface. Beat the raw egg (egg yolk and egg white, 160 g) in a bowl with the egg whisk. Stir 50 ml milk and160 g egg together without generating froth. Before soiling, treat the sheets in the thermal cabinet (30min/80°C), allow to cool, and weigh. Using the brush, uniformly distribute 1.0 ± 0.1 g egg/milkmixture on the brushed side of the stainless steel sheets (use the balance to check), leaving an approx.1.0 cm wide unsoiled margin along the short sides. Dry the sheets horizontally (for at least 4 h and max. 24 h at room temperature). Then immerse thesheets in boiling demineralized water for 30 seconds. Dry the sheets in the thermal cabinet for 30min at 80°C. After cooling, weigh the egg/milk sheets. Leave the soiled sheets for at least 24 hoursprior to washing. The quantity applied/sheet after denaturation is:

190 ± 10 mg Sheets deviating from the specifications must not be used.

58

9.4 Evaluation After washing, dry the sheets again for 30 min at 80°C, allow to cool, and weigh. mg egg/milk released x 100 % cleaning performance = ------------------------------------------------- mg egg/milk applied (after denaturation) 9.5 Important remarks

− No water stains or fluff on the surface (visual inspection/repolish if necessary)− Keep the freshly coated sheets horizontal to prevent the formation of droplets on the edges.− The egg/milk sheets can be stored at 20°C/40-60% relative humidity.

59

Appendix 1 Loading plan taking the example of the Miele reference dishwasher

upper basket

lower basketporridge

porridge

porridge

porridge

porridge

porridge

starch-mix

starch-mix

starch-mix

starch-mix

starch-mix

starch-mix

egg yolk

egg yolk

egg yolk

egg yolk

egg yolk

egg yolk

egg/milk

egg/milk

egg/milk

meat on porcelain

meat on porcelain

meat on porcelain

egg/

milk

egg/

milk

dess

ert p

late

mea

t / p

orce

lain

mea

t / p

orce

lain

mea

t / p

orce

lain

egg/

milk

dess

ert p

late

dess

ert p

late

dess

ert p

late

dess

ert p

late

minced meat

milk

tea

minced meat

minced meat

minced meat

minced meat

minced meat

tea

tea

tea

tea

tea

milk

milkmilk

milk

milk

60

Appendix 2a Raw materials

Ballast soil : see Appendix. 3

Eggs : use good quality eggskeep in the refrigerator until ready to use

Ethanol : Ethanol 96 Vol.- % p.a., (for export)Order.-No. 24106Riedel-de Haën

Mincemeat : Minced pork - free from fat and sinewMinced beef - free from fat and sinew

Porridge oats : tender Kölln flakesFull grain oat flakesPeter Kölln; D-25333 Elmshorn

Iodine : 0,05 mol I2 volumetric solutionOrder.-No. 35090Riedel-de Haën

Milk : U.H.T. milk1,5 % fatIt should have a validity of at least 45 days

Ninhydrin : Ninhydrin p.a.Order.-No. 33437Riedel-de Haën

Starch mix : Wheat starch for biochemical purposesE. Merck/Darmstadt; Order.-No. 11685.1000 E

Maize starch for biochemical purposesE. Merck/Darmstadt; Order.-No. 11686.1000 E

Rice starch for biochemical purposesE. Merck/Darmstadt; Order.-No. 11684.1000 E

Potato starch for biochemical purposesE. Merck/Darmstadt; Order.-No. 1259.1000 E

61

Tea : black teaAssam, voll & kräftigLipton GmbH, P.O. box 305588, D-20317 Hamburg

synthetic water (see below)

Ferric Sulfate, dehydrated, pure (x H2O)Riedel de Haën, Order No. 12357

Water : Synthetic water(3,00 mmol Ca+Mg as described in Appendix 4)

Calcium Chloride Dihydrate for analysisE. Merck/Darmstadt; Order.-No.2382.1000

Magnesium Sulfate Heptahydrate for analysisE. Merck/Darmstadt; Order.-No. 5886.1000

Sodium Hydrogencarbonate for analysisE. Merck/Darmstadt; Order.-No. 6329.1000

62

Appendix 2b : Apparatus

Device Example Adress Application forDrying oven (up to 300 °C) Heraeus UT 6120, Volume 104 l Heraeus

W.C. Heraeus GmbHProduktbereich ElektrowärmeP.O. box 1553D-63450 Hanau

Minced meat in glass vessels

Electric mincer Perforated disk No 8/3,3 mm diameter holes

Electric appliances stores Minced meat in glass vesselsMinced meat on porcelain plates

Freezer cabinet Electric appliances stores Minced meat in glass vesselsMinced meat on porcelain platesBallast soil

Kitchen hand blender Braun Electric appliances stores Minced meat in glass vesselsMinced meat on porcelain plates

Microwave oven with glass turntable Bosch HMT 752 Electric appliances stores Milk in the microwave ovenSerial dispenser Fortuna Optifix Basic, 1.0 ml Graf/Fortuna

Am Bildacker 3-7D-97877 Wertheim

Milk in the microwave oven,Starch mix

Water bath IKA TemperaturheizbadH34 basic

Janke & Kunkel GmbH & CO.KGIKA LabortechnikP.O. box 1263D-79217 Staufen

Starch mix

Electric laboratory stirrer + blade typeagitators

IKA Eurostar Janke & Kunkel GmbH & CO.KGIKA LabortechnikP.O. box 1263D-79217 Staufen

Starch mix, Porridge

Through circulation thermal cabinet Memmert ULE 800 Memmert GmbH & Co. KGP.O. box 1520D-91126 Schwabach

Starch mix, porridge,Minced meat on porcelain plates,Milk in the microwave oven

Balance Sartorius LC 1201 S Sartorius AGWeender Landstr. 94-108D-37070 Göttingen

Starch mix,Egg/milk,Egg yolk

Magnetic stirrer with hotplate IKA RET basic Janke & Kunkel GmbH & CO.KGIKA LabortechnikPostfach 1263 D-79217 Staufen

Porridge,Egg/milk

63

Appendix 2c : List of necessary items to be soiled

Soil amount Item Description/sourceTea 6 Tea cups e.g. Bauscher; Order. No.: 6215/18

orSchönwald; Dekor:weiß; Form: 98L/ 0,19Schönwald / Rehauerstr. 44-54 / D-95173 Schönwald

Minced meat, encrusted 6 Crystallization dishes e.g. Duran/Schott;Ø 115 mm; h 65 mmOrder No. 213114908 ;Schott Glaswerke / Hattenbergstr. 10 / D-55014 Mainz

Milk in the microwave 6 Glass beakers Laboratory supply150 ml, short formØ 55 mm, h 80 mm

Starch mix 6 Glass plate arcoroc ®, Octime-series, black, octagonal, Ø 25 cm (from edge to edge) inner surfacearea 270 cm2 ;Verrerie Cristallerie d Arques / Avenue du General de Gaulle / F-62510 Arques

Porridge 6 Soup plates Ø 23 cm; e.g. Arzbergwhite glazed porcelain or the dishes conforming to the EN 50242 standardArzberg / Ludwigsmühle / D-95000 Selb

Egg yolk 6 Stainless steel sheets 10 x 15 cm, brushed on one sideWMF AG / Dr. Fehse / D-73309 Geislingen/ Steige

Minced meat on porcelain plates 6 Dessert plates Arzberg (see porridge)white glazed porcelain or the dishes conforming to the EN 50242 standard,Form 1495, Order No. 0219; Ø 19 cm

Egg/milk 6 Stainless steel sheets See egg yolk

64

Appendix 3 : Production instructions for ballast soil

StepNo.

Raw material %content

g for a setup of 5 kg

a) Starch containig ingredients1 Potato starch 5,43 2721 Gravy (powdered/instant) 2,19 1104 Wheat flour 4,38 219

b) Fat containig ingredients5 Vegetable oil 4,32 2163 Margarine 4,32 2163 Lard 4,32 2166 Cream (32 % fat) 8,76 4383 Deep frying fat, semi-liquid 4,32 216

c) Protein containig ingredients5 Full egg (liquid) 8,76 4386 Fresh milk (3,5 % fat, pasteurized) 8,76 438

d) Miscellaneous ingredients2 Tomato ketchup 3,00 1502 Mustard 4,00 2004 Benzic acid (Riedel de Haën, Order-No.: 18102) 0,73 371 Synthetic Water, 3.00 mmol Ca+Mg according to Appendix 4 36,71 1836

Total amount 100,00 5,00 kg

1. Pour the water into the vessel and add the potato starch together with the gravy powder while stirring. Heat themixture until it is obviously swollen (ca. 64 °C). Allow to cool to ambient temperature.

2. Add ketchup and mustard while stirring vigorously.

3. Melt the solid fats in a separate vessel and allow to cool to ambient temperature. Add the fatty ingredients whilestirring vigorously.

4. Weigh the wheat flour and the Benzoic acid together and stir in. 5. Weigh the liquid egg together with the vegetable oil and homogenize with the kitchen blender. Add

subsequently while stirring. 6. Stir in cream and milk. 7. When all the ingredients have been added, stir the soil mixture for a further 30 minutes. 8. Finally weigh 100 g of the liquid soil into plastic beakers (e.g. polypropylene beakers, 250 ml volume, ø 65

mm, height 80 mm). Deep freeze them and keep them in the freezer until required.

65

Appendix 4 : Instructions for the production of synthetic water

a) Hardening the water

1) Preparation of the stock solutions

• solution 1: 800 mmol/l NaHCO3 (67,2 g/l)• solution 2: 154,2 mmol /l MgSO4 * 7 H2O (38,0 g/l)• solution 3: 446,1 mmol /l CaCl2 * 2 H2O (65,6 g(l)

2) Preparation of synthetic water with 3.00 mmol Ca+Mg (16,8 °d)

Put 50 ml each of the stock solutions 1, 2 and 3 in a vessel with 7 l demineralized water and fillwith additional demineralized water up to 10 l. Before use the pH value of the synthetic watershould be adjusted to 7.5 with HCl or NaOH.

b) Ferric sulfate stock solution (only for tea)

In a 1 litre graduated measuring flask, dissolve 5 g Fe2(SO4)3 + 1 ml HCl (37 %) in demineralizedwater and fill with demineralized water up to 1 l.

66

Appendix 5 : Calibration instruction for the microwave oven

Instructions to check the actual microwave output

The microwave output is calculated in accordance with EN 60705.

Fill a cylindrical vessel made of borosilicate (glass beaker, external diameter 100 mm, max. glassthickness 3 mm) with 1000 g ±±±± 5 g drinking water.The water's initial temperature is 10°C ±±±± 0.1°C. Measure it immediately before placing it in themicrowave (using a calibrated thermometer).Place the glass beaker in the center of the rotating plate and set the microwave to maximum output.

In several tests now determine the time (using a calibrated stop watch) in which the water at atemperature of 10°C ± 0.1°C is heated by 10°C ± 0.1°C. After each test, the microwave should beallowed to cool for at least half an hour. The test is to be repeated at least once.Measure the water's final temperature after mixing it thoroughly.

The microwave's effective output is calculated with the following equations:

4187 * (T2 - T1)Peff = ------------------------ (t - 1.6 s)

Peff = Microwave's effective output in WT 2 = Final temperature in °CT 1 = Initial temperature (10°C)

t = Time switched on in seconds

4187 = Water's specific heat capacity in J kg-1 K-1

1.6 seconds should be deducted from the time switched on as the magnetron in the microwave takesthis time to preheat.

The correction factor is calculated from the ratio

Nominal output / Calculated effective output (Pset/Peff).

Extend or shorten the baking times by this factor. A time switch is recommended for this.

Appendix 6 : Photo catalogue for IKW-test

Due to the high data storage requirement of the photo catalogue, the complete collection ofpictures is only available on the CD-ROM.

3. Reference Detergent and Pass/Fail-level (IKW-test)

1. Reference Detergent

The IEC Reference Detergents Type B is the reference detergent for the IKW Performance test. Thecomposition of the reference detergent is described below.

Table: Composition of IEC 436 Reference Detergents Type B

INGREDIENTS (IEC 436, Type B) (wt. %)

Sodium-tripolyphosphate (STPP) 0Tri-sodium-citrate-dihydrate 30.0Sodium-carbonate 29.0sodium perborate monohydrate 5.0Tetraacetylethylendiamine 2.0Sodium-disilicate 25.0Nonionic surfactant (low foaming) 2.0Maleic acid/acrylic acid copolymer Na-salt 6.0Protease 0.5Amylase 0.5Sodium-dichloroisocyanurate 0Sodium-metasilicate 0Sodium-metasilicate-pentahydrate 0

TOTAL WEIGHT 100

The Reference detergent may be obtained from:

wfk Testgewebec/o Mr Dr. ScherbaumChristfeld 10D-41379 BrüggenTel: +49-2157 72 41fax: +49-215790657

2. Pass/Fail-level

The detergent under test should comply with the following requirements:For each of the four soil classes of the IKW Test Method (bleachable, persistent/burnt, dried/starchcontaining, dried/protein containing), the performance of the tested detergent has at least to be asgood as the reference detergent.

☞ Tested detergent pass performance test if:

the performance in all four soil classes is > reference detergent

☞ Tested detergent fail performance test if:

the performance in one or more soil classes is < reference detergent

Part 4. Supplement to performance test no. 2. Modification of standard EN 502 42.

If the washing effect is tested in accordance with standard EN 50242:1998 for functional testingof dishwashers for domestic use, the following amendments shall apply:

• The tests should be carried out at 55°C ± 2°C with cold pre-wash without detergent.

• The machine used in the test must be connected to cold water and must hold 12 place settingswith a washing index of between 3.35 and 3.75.

• The machines drying programme should be used, but only the cleanliness of the dishes should beassessed.

• A weak acidic rinsing agent in accordance with the standard (formula III) should be used.

• The rinsing agent setting should be between 2 and 3.

• The dosage of dishwashing detergent should be as recommended by the manufacturer.

• Three attempts should be carried out at a water hardness in accordance with the standard. Anattempt consists of five washes where the result is read after the fifth wash without the dishesbeing cleaned between the washes.

• The result should be better than or identical to the reference detergent after the fifth wash.

Recipe for the reference detergent (Detergent B IEC 436)* and rinsing agent (formula III), seeAppendix B in the standard EN 50242:1998.

* The tensides are to be stored in a cool place in watertight containers not exceeding 1 kg and are tobe used within three months.

Annex 3

1. Detergent Ingredient Database (DID-list)

2. Approach for handling ingredients which are not listed in theDID-list

NOEC = no effect concentration; LTE = long term effect; LF = loading factor; an NBO = anaerobically non biodegradable; a NBO = aerobically non biodegradable; SI = soluble inorganics; II = insolubleinorganics; THOD = theoretical oxigen demand; Y = yes; CF = correction factor.

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1. DID-list (Detergent Ingredients Database - for ecolabel calculations only)revised edition 29.09.98 (rev. 28.03.95; first edition: 08.07.94)

Ingredients DID No. NOEC 1 LTE LF an NBO a NBO SI II THOD

Anionic surfactants

C 10-13 LAS (Na ø 11.5-11.8. C14 1 %) 2 0.12 0.12 0.05 Y, CF = 1.5 O O O 2.3

C 14/17 alk. sulfonate 3 0.27 0.27 0.03 Y, CF = 0.75 O O O 2.5

C 8/10 Alkylsulfate 4 EC50= 2.9 0.15 0.02 O O O O 1.9

C 12-15 AS 5 0.1 0.1 0.02 O O O O 2.2

C 12-18 AS 6 LC50 = 3 0.15 0.02 O O O O 2.3

C 16/18 FAS 7 0.55 0.55 0.02 O O O O 2.5

C 12-15 A 1-3 EO sulphate 8 0.15 0.15 0.03 O O O O 2.1

C 16/18 A 3-4 EO sulphate 9 no valid data 0.1 0.03 O O O O 2.2

C 8 Dialkylsulfosuccinate 10 LC50 = 7.5 0.4 0.5 Y, CF = 1.5 O O O 2

C 12/14 sulpho-fat.-acid methylester 11 EC50 = 5 0.25 0.05 Y, CF = 0.75 O O O 2.1

C 16/18 sulpho-fat.-acid methylester 12 0.15 0.15 0.05 Y, CF = 0.75 O O O 2.3

C 14/16 alpha olefine sulphonate 13 LC50 = 2.5 0.13 0.05 Y, CF = 0.75 O O O 2.3

C 14-18 alpha olefine sulphonate 14 LC50 = 1.4 0.07 0.05 Y, CF = 2.0 O O O 2.4

soaps (C12 - 22) 15 EC0 = 1.6 1.6 0.05 O O O O 2.9

Nonionic surfactants

C 9/11 A >3-6 EO lin. or mono br. 16 EC50=3.3 0.7 0.03 O O O O 2.4

C 9/11 A > 6-9 EO lin. or mono br. 17 EC50=5.4 1.1 0.03 O O O O 2.2


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C 12-15 A 2-6 EO lin. or mono br. 18 0.18 0.18 0.03 O O O O 2.5

C 12-15 (Avg. C6-9 EO lin. ormono br.

19 0.24 0.24 0.03 O O O O 2.3

C 12-15 (Avg. C>14) A >6-9 EO 20 0.17 0.17 0.03 O O O O 2.3

C 12-15 A >9-12 EO 21 LC50 = 0.8 0.3 0.03 O O O O 2.2

C 12-15 A 20-30 EO 22 EC50 = 13 0.65 0.05 O O O O 2

C 12-15 A > 30 EO 23 LC50 = 130 6.5 0.75 O Y O O 0*

C 12/18 A 0-3 EO 24 no data 0.01 0.03 O O O O 2.9

C 12-18 A 9 EO 25 0.2 0.2 0.03 O O O O 2.4

C 16/18 A 2-6 EO 26 0.03 0.03 0.03 O O O O 2.6

C 16/18 A > 9-12 EO 27 LC50 = 0.5 0.05 0.03 O O O O 2.3

C 16/18 A 20-30 EO 28 EC50 = 18 0.36 0.05 O O O O 2.1

C 16/18 A > 30 EO 29 LC50 = 50 2.5 0.75 O Y O O 0*

C 12/14 Glucose Amide 30 4.3 4.3 0.03 O O O O 2.2

C 16/18 Glucose Amide 31 0.116 0.116 0.03 O O O O 2.5

C 12/14 Alkylpolyglucoside 32 1 1 0.03 O O O O 2.3

Amphoteric surfactants

C 12-15 Alkyl dimethylbetaine 33 0.03 0.03 0.05 Y, CF= 2.5 O O O 2.9

C12-18 Alkyl amidopropylbetaine 34 0.03 0.03 0.05 Y,CF = 2.5 O O O 2.8

Sud controllers

Silicone 35 EC0 = 241 4.82 0.4 Y,CF = 0.75 Y O O 0.0

Paraffin 36 no data 100 0.4 O Y O O 0*


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Fabric Softening

Glycerol 37 LC50 > 5-10gl 1000 0.13 O O O O 1.2

Builders

Phosphate as STPP 2 38 1000 0.6 O O Y O 0.0

zeolite A 39 120 120 0.05 O O O Y 0.0

Citrate 40 EC50 = 85 85 0.07 O O O O 0.6

Polycarboxylates and related derivates 41 124 124 0.4 Y, CF = 0.1 Y O O 0*

Clay 42 1000 0.05 O O O Y 0.0

Carbonate /bicarbonate 43 LC50 = 250 250 0.8 O O Y O 0.0

fatty acid (C >=14) 44 EC0=1.6 1.6 0.05 O O O O 2.9

Silicate 45 EC50 > 1000 1000 0.8 O O Y O 0.0

NTA 46 19 19 0.13 O O O O 0.6

Polyaspartic acid. Na salt 47 125 12.5 0.13 Y,. CF=0.1 O O O 1.2

Bleaching

Perborate mono (as borate) 48 1 - 10 6 1 O O Y O 0.0

Perborate tetra (as borate) 49 1 - 10 6 1 O O Y O 0.0

Percarbonate (see carbonate) 50 LC50 = 250 250 0.8 O O Y O 0.0

TAED 51 EC0 = 500 EC0 = 500 0.13 O O O O 2.0

Solvents

C 1-C4 alcohols 52 LC50 = 8000 100 0.13 O O O O 2.3

Monoethanolamine 53 0.78 0.78 0.13 O O O O 2.4


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Diethanolamine 54 0.78 0.78 0.13 O O O O 2.3


Triethanolamine 55 0.78 0.78 0.13 O O O O 2

Miscellaneous

Polyvinylpyrrolidon PVP / PVNO / PVPVI 56 EC50 > 100 100 0.75 Y, CF = 0.1 Y O O 0*

Phosphonates 57 7.4 7 0.4 Y, CF = 0.5 Y O O 0*

EDTA 58 LOEC = 11 11 1 Y, CF = 0.1 Y O O 0*

CMC 59 LC50 > 250 250 0.75 Y, CF = 0.1 Y O O 0*

Na sulphate 60 EC50 = 2460 1000 1 O O Y O 0.0

Mg Sulphate 61 EC50 = 788 800 1 O O Y O 0.0

Na chloride 62 EC50 = 650 650 1 O O Y O 0.0

Urea 63 LC50>10000 100 0.13 O O O O 2.1

maleic acid 64 LC50 = 106 2.1 0.13 O O O O 0.8

malic acid 65 LC50 = 106 2.1 0.13 O O O O 0.6

Ca formiate 66 100 0.13 O O O O 2.0

Silica 67 100 0.05 O O O Y 0.0

High MW polymers PEG > 4000 68 100 0.4 O Y O O 0*

Low MW polymers PEG < 4000 69 100 0.13 O O O O 1.1

Cumenesulfonate 70 LC50 = 66 6.6 0.13 Y, CF = 0.25 O O O 1.7

Xylenesulfonate 71 LC50 = 66 6.6 0.13 Y, CF = 0.25 O O O 1.6


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Toluene sulfonates 72 LC50 = 66 6.6 0.13 Y, CF = 0.25 O O O 1.4

Na-/Mg-/KOH 73 100 1 O O Y O 0.0

Enzymes 74 LC50 = 25 25 0.13 O O O O 2.0

Perfume formulation as used 75 LC50 = 2-10 0.02 0.1 Y, CF = 3.0 Y O O 0*

Dyes 76 LC50 = 10 0.1 0.4 Y, CF = 3.0 Y O O 0*

Starch 77 no data 250 0.1 O O O O 0.97

Zn Phthalocyanine Sulfonate 78 0.16 0.016 0.07** Y, CF=2.5 Y O O 0*

Anionic Polyester (Soil release polymer) 79 EC50=310 310 0.4 Y,CF=0.1 Y O O 0*

Iminodisuccinate 80 23 2.3 0.13 Y,CF=0.25 O O O 1.1

Optical brighteners = FWA

FWA 1 3 81 LC0 = 10 1.0 0.4 Y, CF = 1.5 Y O O 0*

FWA 5 4 82 3.13 3.13 0.4 Y, CF = 0.5 Y O O 0*

Additional ingredients

C12-18 Alkyl Aminoxides 83 0.08 0.08 0.05 Y,CF = 2.5 O O O 3.2

Glycereth (6-17EO) cocoate 84 EC50=32 1.6 0.05 O O O O 2.1

C12-18 Phosphate esters 85 EC50=38 1.9 0.05 Y,CF = 0.25 O O O 2.3 Footnote explanations1 measured.2 phosphat = additional nutrification potential must be added using a nutrification limit of 0.13 mg P / l. resp. 0.51 mg/l STPP. according to CDV eutro:= dosage (STPP) x

LF (STPP) x 1000 / 0.51.3 FWA 1 = Disodium 4.4'-bis (4-anilino-5-morpholino-1.3.5-triazin-2-yl)amino stilbene-2.2'-disulfonate.4 FWA 5 = Disodium 4.4'-bis(2-sulfostryryl)biphenyl.0* ThOD for aerobically non degradable organic substances is set to zero.** rapid photodegradation.

2. How to deal with ingredients which are not in listed in the DID-list The Technical Guidance Document (TGD) in support of Council Regulation 793/93/ EEC andCouncil Directive 67/548/EEC for the Risk Assessment of new and existing chemicals provide theframework how to deal with toxicity data and removal data. The principles of Risk Assessment havealready been taken into account when establishing the DID-list for laundry detergents (UBA, 1997)and the Guidance document for the award of the community Eco-label to laundry detergents (EEC,1995) and therefore should also be the basis for the following approach:

If a substance is not in the DID-list, the following data have to be used for calculating the scores:

Table 3: Data-set which have to be provide for substances which are not listed in die DID-list

1. Chemical identity (name, structure-formula, CAS-number)2. Sorption tendency (log POW)3. Biodegradability data (aerobic and anaerobic)4. Toxicity data (long term and/or acute)

ad 3. Biodegradability data1. aerobically degradable organic substances

The assessment of the aerobic degradation potential of a substance should be done according to theOECD-test-guidelines for ready biodegradability (OECD 301 A - F) or inherent degradability(OECD 302 A - C). For surfactants also the ISO-Headspeace-CO2-method for the assessment of theultimate biodgradability of surfactants which is currently EU-ring-tested could be used (EEC, 1998b).However, tests which measure CO2-development or O2-consumption should be preferred to testswhich measured DOC-removal.

On the basis of the test results the substance should be classified in the following categories:

• ready biodegradable• inherent biodegradable• non biodegradable

According to this classification a loading factor is defined for each substance (see 1.1 and 1.2).

1.1 loading factors for non-surfactants

The loading factor for non surfactants has to be assessed according to table 4:

Table 4: loading factors for organic substances (non-surfactants).

Substance low sorption

log KOW 0 - 2

medium sorption

log KOW 2 - 4

high sorption