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LIQUIDLAUNDRYDETERGENTCAPSULESGUIDELINESONCLPIMPLEMENTATION

Version2.026November2018

Overview

This document provides guidance on theimplementation of Regulation (EU) No 1297/2014of5December2014,amendingtheCLPRegulation(EC) No 1272/2008 with specific measures relatedto liquid consumer laundry detergents in solublepackagingforsingleuse.

It focuses on practical technical measuresconcerning the outer packaging and the solublepackaging(i.e.thecapsuleitself).

DISCLAIMER

Althoughalleffortshavebeenmadetotrytoensurethattheadviceandinterpretationgivenintheseguidelinesiscorrect,A.I.S.E.emphasisesthatitcanacceptnoliabilityforanyerrorsoromissionsorforanylossordamageof any kind arising from their use. These Guidelines have not been endorsed by authorities at the date ofpublication.

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TABLEOFCONTENTS

HISTORYOFTHISDOCUMENT...................................................................................................................3

FOREWORD..............................................................................................................................................4

1.OVERVIEWOFCLPMEASURESFORLLDC...............................................................................................5

2.SCOPEANDDEFINITIONS......................................................................................................................6

3.OUTERPACKAGING...............................................................................................................................6

4.AVERSIVEAGENTINTHESOLUBLEFILM..............................................................................................11

5.CAPSULEINTEGRITY............................................................................................................................12

ANNEXI StudyProtocol:Assessmentoftheeffectivenessofanaversiveagentinsolublefilmforliquidlaundrydetergentcapsules.........................................................................................13

ANNEXII SummaryofIntertekstudyfindings"Assessmentoftheeffectivenessofanaversiveagentinsolublefilmforliquidlaundrydetergentcapsules.......................................................16

ANNEXIII Screeningenvironmentalriskassessmentfordenatoniumbenzoate(exampleofaversiveagent)..........................................................................................................................18

ANNEXIV Capsuleintegritytestprotocol..................................................................................................20

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HISTORYOFTHISDOCUMENT

Date Publication Comments

February2015 LiquidLaundryDetergentCapsulesGuidelinesOnCLPImplementation

Version1.0

Originaldocument

November2018 LiquidLaundryDetergentCapsulesGuidelinesOnCLPImplementation

Version2.0

- Annex IV and Annex V were merged into a newAnnexIVthatcoversthetwocapsuleintegritytests.In this new Annex, (1) the scope of the tests isexpanded to also cover in-market inspections; (2)the pre-conditioning is refined to ensure fullconsistency with the test conditions; (3) statisticalcriteria are put forward appropriate for in-marketinspection; and (4) the statistical criteria fordesignpurposesareremoved.

- Update of the tonnage assumptions for theenvironmental risk assessment of denatoniumbenzoate(AnnexIII).

- Reference to theA.I.S.E. Test Protocol for SuperiorChildImpedingClosuresinsection3.3onclosures.

- Typographicalandlayoutcorrections.

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FOREWORD

TheseGuidelinesaddresstherequirementsofRegulation(EU)No1297/2014(hereunderreferredtoastheSolublePackagingRegulation)1.Allother legislationapplicable todetergentproductsand theirpackagingremainsunchangedthuscontinuestoapply,e.g.

• thenumberofdosesandthenominalquantitytobeindicatedontheouterpackaginginlinewiththe Detergents Regulation (EC) No 648/20042 and provisions of the CLP Regulation (EC) No1272/20083

• classification,labellingandpackagingofdetergentsaccordingtotheCLPRegulation• labellingofallergensaccordingtotheDetergentsRegulation• otherpackagingrequirementsfrome.g.theEUPackagingandWasteDirective,ortheUN‘Orange

Book’ontheTransportofDangerousGoodsconcerningpackaging• theREACHRegulation4• otherapplicablelegislation.

It shouldbeborne inmind that, since all otherCLP requirements concerning classification, labelling andpackagingapplyandsinceintheCLPSolublePackagingRegulationthefilmisconsideredaspackaging,thefilm can be excluded from themixture composition used for deriving classification. In addition, the film(regardedasaspecificformofpackaging)willhavetobearalabelifthemixtureitcontainsishazardous.Specificprovisions for ‘reduced labelling’aswellasa ‘full’ labellingderogationare foreseen inArticle29andAnnexI,Parts1.5.1and1.5.2.oftheCLPRegulation,whichcanbesummarisedasfollows:

• ‘Full’ labelling derogation according to Article 29(2) and Annex I Part 1.5.2.2: when sold to thegeneral public, if the capsule content is less than or equal to 25 mL and if the mixture is notclassifiedinthefollowingcategoriesconcerninghumanhealth:AcuteToxicity(anycategory),Skincorrosion Category 1A/1B/1C, Serious eye damage Category 1, Skin sensitisation Category 1,Respiratory sensitisation Category 1, Specific Target Organ Toxicity Single Exposure ‘STOT SE’ orRepeatedExposure‘STOTRE’(anycategory),CMR1A/1B/2,5AspirationhazardCategory1.

• ‘Reducedlabelling’inlinewithArticle29(1),andCLPAnnexIPart1.5.1:asthecapsulesareinsuchashapeandformandaretoosmalltomeettherequirementsofCLPArticle31(fulllabelling)inthelanguagesoftheMemberStateswhereLLDCareplacedonthemarket,thecapsulesshouldbearatleastthehazardpictogram(s),theproductidentifierandthenameandphonenumberofthesupplier,providedthatallelementsdefinedinCLPArticle17(fulllabellingelements)arelabelledontheouterpackaging.

While the Soluble Packaging Regulation applies only to Liquid Laundry Detergent Capsules classified ashazardous,A.I.S.E.hasputinplaceanewvoluntaryProductStewardshipProgrammetoaddressotherunitdose products such as non-hazardous liquid laundry capsules and liquid detergent capsules other thanlaundry (e.g. automatic dishwasher, floor cleaners, etc.). More information can be found on A.I.S.E.’swebsite: � http://www.aise.eu/our-activities/product-stewardship-programmes/liquid-laundry-detergent-capsules-634/aise-product-stewardship-programme-for-liquid-laundry-detergent-capsules.aspx

Further,A.I.S.E.launchedavoluntaryconsumereducationcampaign‘KeepCapsFromKids’consistingofadedicated multi-lingual website and a communications toolkit (video, web banner, leaflets) aiming atsecuring safe use and storage of liquid laundry detergent capsules. The toolkit is made available to allpartners.

1http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32014R1297&from=EN2http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32004R0648&from=EN3http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2008:353:0001:1355:en:PDF4http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32006R1907&from=en5MixturesclassifiedasCMR1A/1BcannotbesoldtothegeneralpublicanywayunderAnnexXVIIoftheREACHRegulation

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1. OVERVIEWOFCLPMEASURESFORLLDC

Regulation (EU) No 1297/2014 amends Annex II to the CLP Regulation (EC) No 1272/2008 setting out‘Special rules for labelling and packaging of certain substances and mixtures’, by adding a new sectionunder Part 3 ‘Special rules on packaging’ concerning liquid consumer laundry detergents in solublepackagingforsingleuse(referredtoasLiquidLaundryDetergentCapsules=LLDCinthisdocument).

Regulation(EU)No1297/2014alsoamendsArticle35(2)oftheCLPRegulationconcerning‘Packaging’.

Itwaspublishedon6December2014andenteredintoforceon26December2014.

ThefollowingtechnicalmeasuresarerequiredunderRegulation(EU)No1297/2014:

NewCLPrequirementforLLDCs

Outerpackaging:visibilityofcontent

Theouter packaging shall beopaque or obscure so that it impedesthevisibilityoftheproductorindividualdoses.

Outerpackaging:on-packlabelling

The outer packaging shall bear the precautionary statement P102"Keepoutofreachofchildren"atavisibleplaceandinaformatthatattractsattention.

Outerpackaging:closures The outer packaging shall be an easily reclosable, self-standingcontainerandshallbefittedwithaclosurethat

- impedes theabilityof youngchildren toopen thepackagingby requiring coordinated action of both hands with astrength thatmakes itdifficultforyoungchildrentoopenit;andthat

- maintains its functionality under conditions of repeatedopening and closing for the entire life span of the outerpackaging.

Capsulesolublefilm:aversiveagent

The[solublepackaging/capsule]shallcontainanaversiveagentinaconcentrationwhichissafe,andwhichelicitsoralrepulsivebehaviourwithin a maximum time of 6 seconds, in case of accidental oralexposure.

Capsulesolublefilmintegrity:containmentfunction

The[solublepackaging/capsule]shallretainitsliquidcontentforatleast30secondswhenthesolublepackagingisplacedinwaterat20°C;

Capsulesolublefilmintegrity:mechanicalintegrity

The[solublepackaging/capsule]shallresistmechanicalcompressivestrengthofatleast300Nunderstandardtestconditions.

TIMEFRAME:

Themeasuresmustbeinplaceby1June2015.

Forproductsalreadyplaced in themarketby thatdate, shelfwithdrawal isnot required.TheRegulationallowsforatransitionperioduntil31December2015(Article2ofRegulation(EU)No1297/2014).

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2. SCOPEANDDEFINITIONS

Regulation (EU) No 1297/2014 applies to “liquid consumer laundry detergents in soluble packaging forsingleuse”.

‘Detergent’and‘consumerlaundrydetergent’aredefinedinArticle2(1)oftheDetergentsRegulation(EC)No648/2004.Regulation(EU)No1297/2014makesexplicitreferencetothesedefinitions.

This impliesthatsolubleunitdosesof laundrydetergentpossiblysoldtoprofessionalusersdonot fall inthescopeoftheSolublePackagingRegulation.

‘Liquid’isdefinedintheAnnexIPart1.0totheCLPRegulation.

Liquidmeansasubstanceormixturewhich:(i)at50°Chasavapourpressureofnotmorethan300kPa(3bar);(ii)isnotcompletelygaseousat20°Candatastandardpressureof101,3kPa;and(iii) which has a melting point or initial melting point of 20°C or less at a standardpressureof101,3kPa.

Formulti-compartmentproductscontainingseveralproductformsinoneunitdose(e.g.partlyliquid,partlysolid),theEuropeanCommissionhasclarifiedthat,intheabsenceofanyspecificprovisionastoapotentialthresholdquantitytoqualify‘liquid’,thereisnolimit.UnitdosescontaininganyquantityofliquidlaundrydetergentaredeemedtobefallinginthescopeoftheCLPmeasures.

Some‘gels’mayqualifyas‘liquid’underthisdefinition.

‘Hazardous’: since CLP Article 35(2) refers to ‘packaging containing a hazardous substance or mixturessuppliedtothegeneralpublic’, it isunderstoodthatthenewprovisionsapplyonlytohazardousLLDC i.e.detergent mixtures meeting the CLP classification criteria for one or more than one hazard class andcategory. Non-classified detergent mixtures (irrespective whether they contain one or more hazardoussubstances) are neither covered by the requirements of Article 35(2) nor by the Soluble PackagingRegulation.

3. OUTERPACKAGING

Inthiscontext,‘outerpackaging’meansthepackagingunitthatispurchasedbyaconsumerasasingleunit(inmostcasesabox/tuborastand-uppouch)andthatcontainsagivennumberofunitdoses6.

3.1.Visibility

ThisrequirementisdefactoequivalenttotherequirementsfromtheA.I.S.E.ProductStewardshipProgrammeforLLDC.

Note:Forstand-uppouches,itmaybenecessarytomaintainatransparentwindowatthebottomof the pack to allow for production control (e.g. absence of leaks). This is because pouches aresealedduringtheproductionprocessbutneedtobeinspectedfor leakers:thedetectionwindowallows inspecting without the need for destructive testing (opening the pouch to check thus‘destroying’theproduct).Thistransparentwindowmustnotbevisiblewhenthepouchisstandingonahorizontalsurface.Itshouldbenolargerthanrequiredforinspectingleaks.

6Note: ‘outer packaging’ as referred to in Article 33 of CLPmay apply to another layer of packaging such as thetransportpackage.

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Illustrationsofopaqueorobscurepackagingareshownbelow:

3.2.On-packlabelling

TheSolublePackagingRegulationrequirestheprecautionarystatementP102“Keepoutofreachofchildren”tobevisibleandinaformatthatattractsattention.

A.I.S.E.recommendscompaniestocombinetwopractices:

- ensureprimarilythattheP102statementfromtheCLPRegulationisincludedintheCLPlabelandismademoreprominentthantheotherPstatementsand

- repeatasimilarmessageatadifferentplaceontheouterpackaging inanattention-grabbingformat,e.g.P102statementand/ortherelevantA.I.S.E.safeuseicons.

P102STATEMENTINTHECLPLABELAREA:

It should be noted that, under the CLP Regulation, the P102 statement applies to consumerproducts (substances or mixtures), ‘as appropriate’. In the ECHA Guidance on labelling andpackaginginaccordancewithCLP,P102is‘highlyrecommendedforsubstancesandmixturessoldtothegeneralpublic, except for thoseonly classifiedashazardous to theenvironment’. Inaddition,accordingtoArticle32(1)ofCLP,precautionarystatementsshouldbelocatedtogetherwithotherCLPlabelselements(hazardpictograms,signalword,hazardstatements).

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Illustrations of opaque or obscure packaging are shown below:

3.2 On-pack labelling

The Soluble Packaging Regulation requires the precautionary statement P102 “Keep out of reach of children” to be visible and in a format that attracts attention.

A.I.S.E. recommends companies to combine two practices:

- ensure primarily that the P102 statement from the CLP Regulation is included in the CLP label and is made more prominent than the other P statements and

- repeat a similar message at a different place on the outer packaging in an attention-grabbing format, e.g. P102 statement and/or the relevant A.I.S.E. safe use icons.

P102 STATEMENT IN THE CLP LABEL AREA:

It should be noted that, under the CLP Regulation, the P102 statement applies to consumer products (substances or mixtures), ‘as appropriate’. In the ECHA Guidance on labelling and packaging in accordance with CLP, P102 is ‘highly recommended for substances and mixtures sold to the general public, except for those only classified as hazardous to the environment’. In addition,

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It isthereforerecommendedtoapplytheP102statementforallLLDCclassifiedashazardousandtoemphasisetheP102statement intheCLP labelinordertomakeitstandoutversustheotherprecautionarystatements.Thiscanbedoneusingforexampleadifferentcontrastingcolourand/orusingboldorcapitalcharacters.

SAFEUSEINSTRUCTIONSINANATTENTION-GRABBINGFORMAT:

A.I.S.E.recommendsaddinganattention-grabbingsafestoragemessageontoporonfrontoftheouterpackagingintheformofaphraseand/oranicon.

UnderitsProductStewardshipProgrammeforLLDCsfromDecember20127,A.I.S.E.hasdevelopeda set of voluntary safeuse icons8and recommendspresenting these icons visibly, in the formofpatches.ThefollowingrequirementsapplyunderthevoluntaryA.I.S.EPSP:

- Priorityiconsshallbefeaturedinapatchanddisplayedonpackasfollows:o ‘Keepout of reachof children’ (or ‘Keep away from children’ for a limited transition

period, since this has been the text used under the A.I.S.E. PSP commitment), usingofficialtranslationsofP102providedinAnnexIVtotheCLPRegulation;

o ‘Closethelidproperly’or‘Closethebagproperly’(asappropriate),usingofficialA.I.S.E.translations(availablefromwww.aise.eu/end_user_info).

- Minimumsizeoftheicon:20x20mm- Text: the iconshouldbeaccompaniedwith the text fromtheP102statement ‘keepoutof

reachofchildren’or‘keepawayfromchildren’andaminimumsizeof10points(referencefont: Futura Condensed).Multilingual versions of this patch are allowedbut theminimumsize requirements remain valid for all languages. ‘Silent icons’ (icons only, without thecorrespondingtextorwiththetitleonly)areconsideredasanoptionformulti-linguallabels,butthisisnotthepreferredoption.

- Colouroftheicon:blackordarkblue.- Location of the patch displaying the icons: Patch to be placed on pack (as per A.I.S.E.

guidelines and models), with yellow background (reference colour recommended: yellowCMYK:100%).

- Recommended positioning of patch on packaging: on top or front of the pack. Excluded:underneath the outer packaging. In any event, the patch should be readily seen byconsumers.

- General introduction sentence: ‘Handle and store safely’ (or its corresponding translationprovided by A.I.S.E. on the link mentioned above), with a minimum size of 13 points(referencefont:FuturaBold),preferablyincapitalletters.

- Others: patch to include copyright and website reference as follows: copyright ©A.I.S.E.togetherwiththelink:www.keepcapsfromkids.eu(minimumsize:10points–referencefont: Futura Condensed). Since A.I.S.E. previously recommended www.cleanright.eu, thetransition to the new website reference can be progressively implemented by companieswhenupdatingtheirlabels.Thistransitionfrom‘cleanright’to‘keepcapsfromkids’maytakeplaceafter1June2015forpracticalprintingreasons,sincethisisavoluntarymeasure.

7http://www.aise.eu/our-activities/product-stewardship-programmes/liquid-laundry-detergent-capsules-634/aise-product-stewardship-programme-for-liquid-laundry-detergent-capsules.aspx8A.I.S.E.Safeuseiconsareavailableon:www.aise.eu/end_user_info

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FROMPATCHESUSEDUNTIL2014/2015UNDERA.I.S.E.’sPSPFORLLDC

Patchforboxes Patchforstand-uppouches

TONEWPATCHES(tobeusedprogressivelyaspracticallyfeasible)

WITHTITLEANDTEXT

(PREFERREDOPTION)

WITHTITLEONLY SILENT

The A.I.S.E. ‘yellow safety patch’ which has been used since 2013 on packs of liquid laundrydetergentswasprovenextremely successful indelivering inaconsistent,attractiveandpowerfulway the key safe use advice, thanks to the contrasted yellowanddark colours, the size and thelocationrequirements.Theiconsmakeitunderstandablebyavastmajorityofthepopulation.

Therefore,A.I.S.E.recommendsfollowingitsLLDCPSPrequirementsconcerningon-packsafeusecommunication in addition to highlighting the P102 statement in the CLP label area forcompliancewiththeSolublePackagingRegulation.

Although theCLP requirementconcernsonly the ‘Keepoutof reachof children’message,A.I.S.E.advisestocontinuedisplayingthesecondiconrelatedtoclosure(“Closethelidproperly”or“Closethebagproperly”)inlinewiththePSPUsePatchInstructions.OtherA.I.S.Eiconscancontinuetobeusedinotherareasofthelabel,asappropriate.

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3.3.Closures

The closure of the LLDC outer packaging must meet two main requirements that need to bebalanced:

i. impedeyoungchildrenfromopeningthepackagingandii. foradults,alloweasyregularopeningandreclosingafteruse.

Thesefunctionalitiesmustbemaintainedduringthepackaginglifespan.

Inaddition,thepack(i.e.the‘outerpackaging’intheSolublePackagingRegulation)shouldbeself-standingandshouldremainsothroughoutthelifespanofthepack.

With regard to closure design, the Soluble Packaging Regulation refers qualitatively to twoelements:‘requiringcoordinatedactionofbothhands’and‘astrength’foropening.

Theserequirementsapply‘withoutprejudicetotherequirementsofsection3.1[ofAnnexIItoCLP]’whichprescribechild-resistantfasteningsforspecificmixtureclassifications(suchasskincorrosiveproducts). A.I.S.E.’s understanding is that the closure requirements for Soluble Packaging aredifferent fromchild-resistant fastenings insection3.1.andapply independently,withoutconflict.Sosection3.1ofAnnexIIcontinuestoapplyforcertainmixtureclassificationsand,inaddition,thenewsection3.3.appliestoLLDCsregardlessoftheirclassification.

A.I.S.E.suggeststhefollowinginterpretationofSolublePackagingRegulation’srequirements:

- ‘coordinated action of both hands’ for opening: in the lack of clear design description in thelegal text, it isuptoeachcompanytoassessthedesignagainstcompliancewiththisgeneralrequirement. It builds on the fact that the key differentiator between adults and children ismental capacity, logic and dexterity. Coordinationmay include the required use of hands tosecureapacktoenabletheopeningofaclosuresystem(e.g.stand-uppouches).

- ‘with a strength’ for opening: is to be seen in the context of the target age group, namelychildrenbelowtheageof6years.Nostrengthvalueisspecifiedinthelegaltextbutitshouldbesufficientsothattheclosurecannotbeopenedunintentionally(e.g.bysimplytouchingtheouterpackaging).Again,itshouldbeborneinmindthattheykeydifferentiatorbetweenadultsandchildrenisdexterityandlogicratherthanstrength.

- ‘easilyreclosable’:theouterpackagingclosuremustbeabletobeclosedbyadults inasingleaction,suchasbutnot limitedto,onecliptobepushed,agentlepressureonthe lidto lock,onezippertobeactivated.

- ‘maintainsitsfunctionalityunderconditionsofrepeatedopeningandclosing fortheentirelifespan’: the closure system must meet the above criteria on opening and reclosing for thedesignedlifeofthepackaging,whichcorrespondstoatleastthenumberofcapsules/unitdosesintheouterpackaging.

Forinformation,in2017,A.I.S.E.introducedtheTestProtocolforSuperiorChildImpedingClosures,as part of the voluntaryA.I.S.E. Product StewardshipProgrammeFor LiquidDetergentCapsules -2017. This protocol offers a performance standard for ‘child-impeding closures’ that are not fully‘child- resistant’ (in themeaningof ISO8371). WhileCLPandtheSolubleFilmRegulationdonotrequiremeetingsuchperformancecriteria,nevertheless,companiesmayconsiderevaluatingtheirLLDCouterpackagingusingthistestprotocol.

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4. AVERSIVEAGENTINTHESOLUBLEFILM

AccordingtotheSolublePackagingRegulation,thesolublepackaging(i.e.thecapsulewall)mustcontainanaversive agent in a concentration which is safe, and which elicits oral repulsive behaviour within amaximumtimeof6seconds,incaseofaccidentaloralexposure.

Thismeasureisintendedtofurtherreducethechanceofingestionoftheliquidcontentincaseachildleftunattendedhasmanagedtogainaccesstoacapsuleandplacesitinhis/hermouth.

A.I.S.E.hasdevelopedandevaluatedaprotocoltodetermineeffectivelevelsofaversiveagentcontainedinsolublepackagingi.e.inthesolublefilm.TheresultingstudyprotocolisprovidedinAnnexI.

Theobjectivesofthisworkwere:

- Todevelopamethodformeasuringtheoral rejectiontime,asa functionof the levelofaversiveagentinthefilm;

- To prove the concept of effectiveness testing (at different concentrations of aversive agent), inotherwordstoestablisha‘benchmarktest’.

Onegradeoffilmandoneparticularaversiveagentwereselectedforthestudy.

TheA.I.S.E. study has shown that, for the particular aversive agent and film selected, itwas possible todeterminealevelofaversiveagentsufficienttoelicitamedianoralrejectioninlessthan6seconds.Abovethisconcentration,the‘dose-response’curvewasflat,i.e.higherlevelsofaversiveagentwerenotfoundtoleadtolowerrejectiontimes.AsummaryofthestudyfindingsisprovidedinAnnexII.

Forethicalreasons,thestudywasrunonyoungadultsinsteadofchildren.Thisisaconservativeapproach,becauseachild'spalateismuchmoresensitivethanthatofadults.Infantshavearound30,000tastebudsspread throughout theirmouths. By the time adulthood is reached, only about a third of these remain,mostlyonthetongue.ThedecreasingsensitivitytobitternesswithagewasdemonstratedbyMennellaetal.(2005)9.Consequently,itisreasonabletoassumethattheobservedoralrejectiontimeswithyoungadultsaresimilartoorhigherthanwhatmaybeexpectedwithyoungchildren. � It is important tonote that it isup toeachcompany todemonstrateeffectivenessof theaversiveagentchosentotheirownsituation(solublefilm/agents)atdesignstage.Thisisbecause:

- differentaversiveagentsmayleadtodifferenthumanresponsesand- the effective concentration of aversive agent may be affected by the polymer chemical

composition,presenceofotherchemicalsinthefilm,etc.

Itisadvisedtoforeseeasafetymarginsothattheeffectivenessoftheaversiveagentismaintainedduringthewholelifecycleoftheproduct.

Companies will need to document the levels of aversive agent used and the rationale, and keep suchrecordsfor10years(inlinewiththegeneralREACHandCLPrecordkeepingdeadlines).

Further, the Soluble Packaging Regulation requires the effective concentration of aversive agent to besafe.A.I.S.E. recommends todetermine that the concentration chosen is safe in caseof ingestionof theamountoffilmcontainedinonecapsule,bymeansofahumanhealthtoxicologicalriskassessment,basedon thehighest levelof aversiveagent contained in the solublepackagingatany timeof theproduct lifecycleandadaptedtothetargetagegroup(youngchildren,includingbabies).Thesafetydatasheetoftheaversiveagentisausefulsourceoftoxicologicaldatabutmaynotbesufficienttorunafullriskassessment.

Environmentalsafetyshouldalsobedocumented.ItshouldberemindedthattheREACHRegistrationisthemainmechanismtoassessenvironmentalsafetyofsubstancesanddemonstratetheuse issafe (unlessa9JulieA.Mennella,M.YaninaPepino,andDanielleR.Reed.Geneticandenvironmentaldeterminantsofbitterperceptionandsweetpreferences.Pediatrics,2005,115(2),e216-e222

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particularsubstancedoesnotneedtoberegisteredbylaw).AnnexIIIprovidesanexampleofascreeningenvironmentalriskassessmentforoneparticularaversiveagent(denatoniumbenzoate)showingthat,evenunder conservative assumptions, the addition of this bittering agent in unit dose soluble films is of noconcernfromanenvironmentalperspective.

5. CAPSULEINTEGRITY

Two specific requirements apply under the Soluble PackagingRegulation in relation to capsule integrity:mechanicalresistanceandliquidcontainment.

Both themechanical and the containment function tests are understood as ‘design’ tests. They serve asafetypurposeinthequalificationofproducts/validationofprocesses.Theyarenotconsideredasqualitycontroltestssinceitisimpossibleinpracticetotesteverysinglecapsule.

Thesetestsshouldbeperformedonanappropriate,representativenumberofcapsulesatdesignstageandshould be repeated, at the minimum, at every substantial design change in product, film specification,formulationormanufacturingprocess.

The capsules will be tested at least 24 hours after production after having been conditioned in anenvironment with a standard temperature and relative humidity.More details are provided in the testprotocols(AnnexIV).

5.1.Liquidcontainmentfunction

TheSolublePackagingRegulationrequiresthesolublepackagingtoretain its liquidcontentforatleast30secondswhenthecapsuleisincontactwithwater.SomeofthetestingparametersaresetbytheRegulation(water,temperature).

ToA.I.S.E.’sknowledge,nostandardmethodexistsforsuchtypeoftest.

Buildingontheexperiencefromitsmembers,A.I.S.E.hasdevelopedacontainment function testprotocol,whichisprovidedinAnnexIVtothisdocument.

5.2.Mechanicalintegrity

The Soluble Packaging Regulation requires the soluble packaging to resist to a mechanicalcompressionstrengthof300Nunderstandardtestconditions.

A.I.S.E. recommends running adynamometric test: the purpose of such compression test is toassessthemechanicalintegrityofacapsulesubmittedtoacompressivestrength.

Building on the experience from its members, A.I.S.E. has developed a test protocol, which isprovidedinAnnexIVtothisdocument.

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ANNEXI

StudyProtocol:

Assessmentoftheeffectivenessofanaversiveagentinsolublefilmforliquid

laundrydetergentcapsules

Objective

The objective of this test is to determine the effectiveness of a given aversive agent contained in a given solublepackagingfilm.Thedose-responserelationshipofthelevelofaversiveagentwiththeobservedoralrejectiontimeisinvestigated. From this, the level of aversive agent that is expected to lead to a rejection timebelow6 seconds isdetermined.

Generalstudydescription

Theresponseoftestpanelliststotastingwater-solublefilmwithdifferentlevelsofaversiveagentistobeobserved.Fromthis,adose-responserelationshipistobeestablishedthatlinksthedeterringeffect(rejectionofthefilm)withtheleveloftheaversiveagent.

The test panel shall consist of young adults, as a proxy for the target audience for the safetymeasures on liquidlaundrydetergentcapsules(i.e.youngchildren).Therearereliableindicationsthat,especiallyforbittertaste,childrenareusuallymoresensitivethanadults.

Thetestproductisthewater-solublefilmcontaining(differentlevelsof)theaversiveagent.Thefilmshallbeusedinisolationfortasting:actualdetergentcapsulesshallnotbeused,toensurethesafetyofthepanellists.

Eachpanellist,unawareofwhattoexpect,willbegivenasheetofthesolublefilmcontainingagivenlevelofaversiveagent,andwillbeaskedtolickthefilmtoexperiencethetaste.Itwillthenberecordedwhetherthepanellistrejectsthefilmandifso,afterhowmuchtime.Panellistsareonlyallowedtoparticipateonce,toavoidanybiasduetopriorexperiencewithabadtastingsample.

Aconcentrationserieswillbe tested, in tworounds.First, inascreening round,abroadrangeof levelsofaversiveagent in filmshallbeassessed,aswell asanuntreatedblank. Subsequently,basedon the screening round results,suitableaversiveagenttest levelsshallbedefinedforadefinitivetestinground,aimingtorefinethedose-responserelationshipforthoselevelsleadingtoarejectiontimeclosetothetargetofmaximum6seconds.

Testmaterial

Thetestmaterialisacombinationofonespecificwater-solublefilmtypewithonespecificaversiveagent,atdifferentconcentrationlevels.Boththewater-solublefilmandtheaversiveagenttestedshallbeidentifiedinthestudyreportand/or in thestudysponsor’sconfidentialstudyplacementdocumentation. Theresultsof thestudyarespecific tothe type/grade of water-soluble film and the type/grade of aversive agent used. Consequently, results cannot beextrapolatedtosubstantiallydifferentcombinationsoffilmandaversiveagent10.

Preparationofwater-solublefilmtreatedwithaversiveagent

Water-solublefilmswithdifferentlevelsoftheaversiveagentshallbeprepared:

- Screeningtest:untreated(blank)-10ppm-100ppm-1000ppm-10000ppm(*)(**)(*)atoxicologicalsafetyassessmentshallbeconductedpriortothestudy.iftoxicologicalconcernsexistwiththehighestscreeninglevels,analternativeconcentrationserieswithlowerlevelsshouldbeused.(**)arangewithadifferentupperlevelmaybeusedifpre-existinginformationsuggeststhisismoreappropriate.

- Finaltest:6levels(noblank)tobedeterminedbasedontheoutcomeofthescreeningtest

Accuracy of the aversive agent’s levels in the film, and homogeneity of its distribution, shall be ensured by theproducerofthetreatedfilm.

10Itisalsouptoeachcompanytoselecttheaversiveagenttheydeemappropriatefortheirproducts,takingintoaccountthatsomelimitationsofuserelatedtoIntellectualPropertymayapplytocertainaversiveagents,filmsortechnologies.

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Preparationofthefilmsheetsfortastetesting

The treatedwater-soluble films shall be cut into strips of 3cm by 10cm. For each test concentration, at least 12replicatesshallbeprepared.Thestripsoffilmshallthenbeplacedinindividualbags,toensurecontaminationisnotanadditionalvariableforthestudy.

Subsequently,foreachconcentration,thestripsshallbesplitintotwoequalbatches-onebatchformalepanellists,onebatchforfemalepanellists.Thesetsoftestspecimensforfemaleandmalepanellistsshallbekeptseparateandidentifiedassuch.

Thesetestspecimensshallbeindividuallylabelledusingacodingsystemthatlinksthespecimentoitsaversiveagentlevel. Thecodingshallnotdisclose the levelofaversiveagentneither to thepanellists,nor to thepersonsdirectlyhandingthetestspecimenstothepanellists.Thisistoavoidanybias,byapplyingadouble-blindapproach.Forthesame reason, preparation, packing and labelling of the film strips shall be done by different persons than thoseconductingthestudywiththepanellists.

TestPanel

Atestpanelwithasmanyparticipantsas therearetestspecimens (i.e. in total10testconcentrations+oneblank,withminimum12replicateseach,henceatotalofatleast132panellists)isrequiredtoconductthisstudyforonefilm/aversiveagentcombination.

Forethicalconsiderations,thetestpanelshallnotconsistofyoungchildren,butinstead,asaproxy,youngadultsshallbeused. Itshouldbenotedthatthis isexpectedto leadtosomedifference intheresults,asadultstendto ‘think’aboutthebadtastethatishappeningratherthanreactandspititout.Thestudyhasbeendesignedtoeliminateasmuchoftheadults‘overthinking’tothetestaspossible,attemptingtogagea‘true’reactiontime.

Thetestpanelshallconsistofthefollowingindividuals:

- youngadults,intheagegroupof18-25yearsold- equalmixmale/female- exclusioncriteria:

o smokersshallbeexcluded.o panellistswithpriorexperienceontestsofaversiveagentsinthiscontextshallbeexcluded.

Each panellist shall participate to only one single tasting session, to avoid a biased response driven by priorexperience.

TestDesignandInstructions

Thetestshallbeconductedintworounds:

1. ascreeningroundinwhichawiderangeoflevelsoftheaversiveagentisassessed;2. afinalroundinwhichthedose-responserelationclosetotherejectiontimetargetisrefined.

Inthescreeninground,thereshallbe4testconcentrationsinadditiontoablank(untreatedfilm).Inthefinalround,thereshallbe6testconcentrations,andnoblank.Thereshallbeatleast12replicatesforeachconcentration.Hence,intotal,therewillbeatleast132tastingsessions(5x12=60forthescreeninground,and6x12=72forthefinalround).Ifdeemednecessarybasedontheresultsofthescreeninground,ahighernumberofreplicatesmaybeusedforthefinalround.

The levels of aversive agent for the screening round are predetermined. The levels for the final round are to bedefinedbasedonthescreeningresults.Consequently,thefinalroundcanonlybeorganizedseveralweeksafterthescreeninground,toallowforprocessingofthescreeningdata,andforpreparationandshipmentofthefilmandtestspecimens.

Fortheactualtesting,thetestspecimensshallbeprovidedtothepersonconductingthestudyintwobatches:oneforfemalepanellists,andoneformalepanellists.Asoutlineabove,eachofthesebatchesshallcontainanequalnumberofreplicatesforeachtestconcentration.Consequently,everytestconcentrationshallbetestedwithanequalnumberofmalesandfemales,toavoidanypotentialbiasdrivenbythepanellists’gender.

Foreverytastingsession(onepanellist,oneleveloftheaversiveagent)thefollowingmethodshallbefollowed:

1. Thetestshallbeconductedsuchthatparticipatingpanellistscannotsee thereactionofothers in the test,andcannottalktootherswhohavejustcompletedthetest.Thepanellistsshallnotbeinformedaboutthepresenceofanaversiveagent inthesample.Thepersonsprovidingthetestsamplestothepanellistsshallnotbeinformedabouttheleveloftheaversiveagentinthesample.

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2. Thepanellistshalldrinkadefinedsmallamount(50ml)ofstillwater.3. The following exact instructions shall be given to the panellist: “This is a taste test and it iswhatwe call

‘double-blind’,meaningIdonotknowwhattasteyouaregoingtoreceive.Itcouldbeanythingfromaneutralnon-tastetosomethingpleasantorunpleasant,itcouldbesalty,sweet,acidic11,etc.If,whenyouarelickingit,youthinkthetasteisneutralorpleasant,IwantyoutocontinuelickingituntilItellyoutostop.If,whenyouarelickingit,youdiscernthatthetasteissomethingunpleasant,Iwantyoutostoplickingitimmediately.Youaregoingtotakethefilmthatis inthebagandholdit inyourhandsandlickit likeso...”andthenthepanellistwillbeshownhowtoholdandlickthefilm.

4. Atthemomentofcontactofthefilmstripwiththetongue/mouth,atimershallbestarted,andnofurtherinstructionsshallbeprovidedtothepanellist.Eachpanellist’sreactionmaybefilmedforfuturereference.

5. Itshallberecordedwhetherthepanellistrejectedthetestspecimenpriortothestrip’sdissolution inhalf,andifso,exactlyafterhowmanysecondstherejectionoccurred.

6. Participants shall be given something to eat or drink to remove thebad taste. What is to beofferedwilldependontheaversiveagentunderstudy.Forexample,forbitteringagents,strongdarkchocolateisknowntoeffectivelyremovethebittertaste.Inaddition,flavouredlipbalmshallbeofferedincasethebadflavourhastravelledtothelipsofthepanellists.

7. Excludethepanellistfromanyfurtherparticipationtothistestorsimilartestsinthefuture.

Analysisandreportingofresults

Allrawdatacollectedduringthestudyshallbereported,exceptfortheidentitiesofthepanellists(thataretoremainconfidential to the testing laboratory). Note that these identities shall be archived by the testing laboratory forfurtherreference,toavoidtheirparticipationinothersimilarstudiesinthefuture.

Amongthepanellists,itisexpectedthattherewillbeanaturalvariabilityintastereceptorsensitivity,primarilydrivenbygeneticdifferences.Peoplewholacksensitivityinthereceptorsthataretargetedbyaspecificaversiveagent,willexperiencetheaversivetastetoalimitedextent,ifatall(irrespectiveoftheconcentrationoftheaversiveagent).Forexample,inSibert&Frude(1991)12,inatestwherechildrenweregivenorangejuicespikedwithacommonaversiveagent (denatonium benzoate) at a level known to be effective, over 15% of the test subjects showed no evidentresponse.

Theaimofthestudyistodeterminetheappropriateaversivelevelthatleadstooralrejectionwithin6secondsoftheinitialexposure.Fornon-sensitivesubjects,thisrejectiontimecannotbeachieved,irrespectiveofthelevelofaversiveagent used. Consequently, data from non-sensitive subjects should be ignored when determining the appropriatelevel. Hence, the median of the different replicates at a given level shall be used as the relevant metric forcomparisonwiththe6secondtarget.

Bymeansofsuitablestatisticalmethods(tobedeterminedcase-by-case,dependinge.g.onthedistributionshapeandamountofscatterof thedata) itshallbedeterminedwhich levelsofaversiveagenthave ledtoamedianrejectiontimebelowthetargetof6seconds,withatleast90%confidence.Iffeasible(dependingonthequalityofthedata),amathematical dose-response relationship shall also be developed, that allows to determine rejection time as afunction of the aversive agent level. Furthermore, it shall be determined up towhich level of aversive agent theobserved rejection time is not significantly different from the blank; and as of which level of aversive agent theobservedrejectiontimenolongerdecreased.

Thefinaloutcomeofthestudy is thedeterminationofthe lowestaversiveagent level that isexpectedto leadtoamedianrejectiontime(eitherobservedastested;orcalculatedifamathematicaldose-responserelationshipcouldbedeveloped)below6seconds,withatleast90%confidence.

11Theactualdescriptionofthetasteoftheaversiveagentunderstudyshallnotbeusedhere.Forexampleifabitteringagentisused,theword‘bitter’shallnotbementioned;iftheaversiveagenthasanacidictaste,theword‘acidic’shallnotbeused,etc.12Sibert J.R. & Frude N. (1991). Bittering agents in the prevention of accidental poisoning: children's reactions to DenatoniumBenzoate(Bitrex).ArchivesofEmergencyMedicine,1991,8,1-7.

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ANNEXII

SummaryofIntertekstudyfindings:

“AssessmentoftheEffectivenessofanAversiveAgentinSolubleFilmforLiquidLaundryDetergentCapsules”.

ExecutiveSummary

- The proposed test method to assess the effectiveness of an aversive agent in soluble film for liquid laundrydetergentcapsuleswasfoundtobepracticallyfeasible,andtoallowdefininganaversiveagent’seffectivelevelinthecontextofCommissionRegulation(EU)No1297/2014.

- Itisrecommendedtousethemedianoralrejectiontimeastheappropriatemetrictoassesscompliancewiththerequirements. Non-parametric statisticalmethods are needed, because the rejection times between panellistsarenotnormallydistributed.Specifically,acertainpercentageofthepopulationistypicallylessornotsensitivetoagivenaversiveagentduetonaturalvariability(geneticpredisposition),whichleadstoskeweddistributionsandscatteredobservationaldata.This impliesthatasufficientnumberofreplicates(at least12but ideallymore) isrequiredpertestedlevelofaversiveagent,toensurerobustnessoftheresults.

- For one specific grade of PVA film, treated with the bittering agent denatonium benzoate, a dose-responserelationshipwasobservedwithadecreasingrejectiontimeupto220ppm.Therejectiontimeremainedthesamewhentheaversiveagent’slevelwasfurtherincreasedbeyondthislevel.Themedianrejectiontimeforlevels>=220ppmwas2.7seconds,andwasdemonstratedtobesignificantlylessthan6secondswith>95%confidence.

Background

CommissionedbyA.I.S.E.,Intertekcarriedoutastudytomeasurethereactiontimeofyoungadultswhencomingintooral contactwith soluble film treatedwith an aversive agent. The response of the test panellists to tastingwater-soluble film with different levels of aversive agent was observed. From this, a dose-response relationship wasestablishedthatlinksthedeterringeffect(rejectionofthefilm)withtheleveloftheaversiveagent.

Theobjectivesofthisstudyweretwofold:

(1)thedevelopmentofamethodformeasuringtheoralrejectiontimebyyoungadults,asafunctionofthelevelofaversiveagentpresentinwater-solublefilmofdetergentcapsules;and

(2)proofoftheconceptwithonespecificcommonly-usedaversiveagentandonespecificfilm.

For the method development, a pilot study was conducted with internal Intertek employees. Next, through ascreeningstudywith50panellists (5 tested levels,10replicateseach), itwasdeterminedwhatare theappropriatelevelsoftheaversiveagenttobetestedinmoredetail.Afinalstudywasthenconductedwith72panellists(6testedlevels, 12 replicates each). A follow-up study with orange juice that was spiked with the aversive agent, wasconductedafterwardswith10panellists,toassesswhetherthesemayhavebeennon-sensitivetotheaversiveagent.AllthesestudieswereconductedattheIntertekfacilityinOakBrook,IllinoisintheUS.

MethodDevelopment

Overall, it can be concluded that the developed test protocol is practically feasible and that it can be used todeterminetheeffectivelevelofanaversiveagentleadingtorejectionwithinadefinedtimeperiod.

Themostsuitablemethodofdeliverywas foundtobeasheetof film (3x10cm), tobe lickedby thepanellistsuntildiscerningthatthetasteissomethingunpleasant.Clearwordingwasdevelopedtohaveunambiguousinstructionsforthepanellists.Thiswaswellunderstood(withonly1exceptionoutof132panellists).

To rule out anydifferencedue todifferent taste sensitivities betweenmales and females, both genders shouldbeequallyrepresentedandeachgendergroupshouldreceivethesamedistributionofaversiveagentlevelstested.

Theobserved rejection times (especially for those aversive agent levels that lead to a substantial repulsive effect),were found to not follow a normal distribution. Amajority (75-80%)was clustered around a short rejection time,

Page17of21

while the remainder was very scattered. This is directly driven by the biology: genetically, a certain part of thepopulationhasless(orno)effectivereceptorsforthespecificaversivetaste.Assuch,itcanbeanticipatedthatsimilardistributionshapesmaybe foundwithotheraversiveagentsand/orothersoluble films thantheonesused for themethod development. It should be noted that follow-up to assess possible non-sensitivity of panellists with longrejectiontimeswasnotfoundtoaddsubstantialvalue.Instead,appropriatestatisticalmethodsshouldbeusedthatimplicitlytakeintoaccountthe‘biologicaloutliers’.

Asaconsequenceofthenon-normality,theuseofmeanrejectiontimeisnotrelevant.Instead,themedianshouldbeused,asthisisindependentofthedistributionshapeatitsextremes.UsingSignAnalysis(anon-parametricmethod)itcanbeassessedwhethertheobservedmedianissignificantlybelowtherequiredthresholdof6seconds,withagivenlevelofstatisticalconfidence(e.g.90%or95%).

Anotherconsequenceofthenon-normalityisthatasufficientlyhighnumberofreplicatesisrequiredforeachtestedlevel. 12 replicates per level, as applied in the final round of this study, is judged to be aminimum. But a largernumberofreplicatesistobepreferred,toincreasestatisticalrobustness.

ProofofconceptforaspecificPVAfilmcontainingDenatoniumBenzoate

Asaproofofconcept,themethodwasappliedtodeterminetherequiredeffectivelevelofonespecificaversiveagent(abitteringagent:denatoniumbenzoate)selectedbasedonitscommonalityandonespecificpolyvinylalcohol(PVA)filmgrade(MonosolM8630).

Noreductionoftheoralrejectiontimeversusuntreatedfilmwasseenupto10ppmofdenatoniumbenzoateinthefilm.At50ppm,aclearlylowerrejectiontimewasobserved,andthisfurtherdecreasedat110ppmandagainat220ppm,whereamedianvalueoflessthan3secondswasreached.Higherlevelsdidnotcausethemedianrejectiontimetodropfurther13.Thedose-responserelationshipisshowninthebelowchart.Pleasenotethatfortheppmlevelsalogarithmicscalewasused.Thedatashownarefromthefinalstudyexceptthedatapointsinred(screeningstudy).

Theobserveddose-response relationship is statistically supportedby theMann-Whitney test.This shows that the rejection timesatthehigherlevelswerenotsignificantlydifferentfromthoseat220ppm (i.e. flat dose-response beyond 220 ppm). Further, this testshowsthatalltreatmentlevelsinthefinalstudyledtosignificantlylowerrejectiontimesthanthe0ppmblank,andthattherejectiontimeat220ppmwassignificantlylessthanat110ppm.Finallythetestshowsthattherejectiontimeat10ppm(screeninground)wasnotlessthanfortheblank.

Themedianoralrejectiontimefordenatoniumbenzoatelevelsinfilm>=220ppm(inthefinalstudy)wasonaverage2.7seconds.Signanalysisshowsthatforeachofthese levels, themedianwassignificantlybelow6seconds,withaconfidencelevelof>95%.The75thpercentileoftheobservedrejectiontimeswasalsobelow6secondsforalllevels>=220ppm(inthefinalstudy),however,statisticalsignificancecouldnotbedemonstrated.

Itcanbeconcludedthat,forthespecificfilmgradethatwastested,adenatoniumbenzoatelevelof220ppminthefilmisadequatetomeettherequirementsofCommissionRegulation(EU)No1297/2014.

13Tonote:themedianof9.8secondsobservedinthescreeningroundfor1000ppmisjudgedtobeanartifactcausedbythetoolimitednumberofreplicates.Whentheobservedrejectiontimesfor1000ppm(screeninground)andthosefortheverysimilarlevelof960ppm(finalround)aregrouped,themedianis3seconds.

0"

5"

10"

15"

20"

25"

30"

1" 10" 100" 1000" 10000"

level$of$aversive$agent$in$film$(ppm)$

median$oral$rejec6on$6me$(s)$

Page18of21

ANNEXIII

ScreeningenvironmentalriskassessmentforDenatoniumBenzoate(exampleofaversiveagent)

Substanceidentification

Denatoniumbenzoateisasaltofthequaternaryammoniumcationdenatoniumwiththeinertanionbenzoate:

CAS 3734-33-6

Molecularformula C28H34N2O3

Molarmass 446.581

Environmentalproperties

Ecotoxicity

In the European Classification& Labelling notification process (ECHA, 2015), denatoniumbenzoatewas notified asAquaticChronic3(H412)bymostnotifiers.

IntheEUEcolabelDIDLIST(EuropeanCommission,2014),denatoniumbenzoateisincluded(ingredientnr.2604).AstherelevantacuteLC50,avalueof13mg/Lismentioned.Chronicdataareabsent.

Thefollowingecotoxicologaldataarereportedinseveralsafetydatasheets(frommultiplesuppliers)ofdenatoniumbenzoate,and/orinregulatoryreviews(e.g.USCPSC1992;HealthCanada,2011):

• Fish:96hLC50RainbowTrout:>1000mg/L• Invertebrates:96hLC50Shrimp(saltwater):400mg/L• Invertebrates:48hrEC50Daphniamagna:13mg/L• Noeffectsonbacteriaupto150mg/L

ThePredictedNo-EffectConcentration(PNEC)canbederivedfromthe lowestacutedatapoint, in thiscase for thewaterfleaDaphniamagna(which isalsothevalueusedfortheEUecolabel). TheassessmentfactortoextrapolatefromanacuteEC50totheecosystemsafelevelisafactor1000.Hence,thePNEC=13µg/L.

Biodegradability

Theactivecationdenatoniumwasnot foundtobeeitherbiodegradedoradsorbed tosludge inaSemi-ContinuousActivatedSludge(SCAS)study(Corbyetal.,1993).AsaSCAStestsimulatesfateinactualsewagetreatmentplants,itisfairtoassumethatdenatoniumbenzoatewillnotberemovedinsewagetreatment.

Furthermore (cf. CPSC, 1992), in an OECD 301D test, no chemical deterioration of Denatonium benzoate wasobserved. In the Zahn-Wellens test (OECD 302B), a 36% breakdown was found after 28 days. A carbon dioxideproductiontestshowedthatdenatoinumbenzoateispoorlymetabolized(4.5%after28days).

IntheEUEcolabelDIDLIST,denatoniumbenzoateisassumedtobenotremovedinsewagetreatment(DF=1).

Bioaccumulation

Denatoniumbenzoate is highlywater soluble (45 g/L) and has a low octanol/water partitioning coefficient (Kow =0.91)(cf.HealthCanada,2011).Consequently,thereisnoriskforbioaccumulation.

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EnvironmentalRiskAssessment

TonnageEstimate

Denatoniumbenzoateismanufacturedand/orimportedintheEuropeanEconomicAreain100-1000tonnesperyear(ECHAwebsite).Forthepurposeofthisscreeningassessmentonecouldconservativelyassumeatotalof1000tonperyear,whichisequivalentto2000mgpercapitaperyearintheEU(with500millionpeople).

The incremental consumption of denatoniumbenzoate in the context of liquid laundry detergent capsules, can beestimatedasfollows:

- One laundrycapsuleof5cmx5cmwitha film thicknessof100µmhas5x5x0.01x2 sides=0.5cm3ofsolublefilmasouterpackaging.Withadensityof1.3thiscorrespondsto0.65goffilmpercapsule.

- When200[respectively1000]ppmisusedasaversiveagentcontainedinthefilm,thisleadstothepresenceof130[resp.650]µgofdenatoniumbenzoatepercapsule.

- IntheUnitedKingdom,whichistodatethemostmaturemarketforlaundrycapsules,onaverageabout20capsulesaresoldperyearperinhabitant(totalmarket:1150millioncapsules;populationof64million).

- Thiscorrespondsto2.6[resp.13]mgofdenatoniumbenzoatepercapitaperyear.

Consequently,anassessmentoftheassumedcurrenttonnageof1000ton/yearintheEU(=2000mg/cap.year)coversanypotentialincreaseduetotheintroductionofdenatoniumbenzoateinthesolublefilmoflaundrycapsulesattheenvisagedlevels.

RiskAssessment

TheaveragewateruseperpersonperyearintheEUis100-200Lpercapitaperday(EEAwebsite).Conservatively,awateruseof100L/dayisassumed.

Assuming 1000 ton/year in the EU, the concentration of denatonium benzoate in household waste water is 2000mg/cap.yeardividedby365days/yearx100L/cap.day=55µg/L.Asdenatoniumbenzoateisnotremovedinsewagetreatmentplants, this isalso thepredictedconcentration for treatedeffluent. Finally, thePredictedEnvironmentalConcentration(PEC)inriverwater,takingintoaccountastandarddilutionfactorof10,is5.5µg/L.

TheaquaticPNECfordenatoniumbenzoateis13µg/L(derivedfromDaphniamagnaacutedatawithanassessmentfactorof1000).

The PEC/PNEC ratio for denatonium benzoate is 55 / 13 = 0.4 < 1. It should be noted that this is based on aconservativetonnageestimateoftotalconsumption,whichisalsonearlythreeordersofmagnitudehigherthantheexpecteduseofthissubstanceforlaundrycapsules.

Conclusion

Usingconservativeassumptions,especiallyregardingtonnage,thisscreeningassessmentshowsnoconcernswiththeenvironmental safety of denatoniumbenzoate. The incremental useof denatoniumbenzoate as aversive agent inlaundrydetergentcapsules isminimalcomparedtotheassumedtotal tonnage,and isnotanticipatedtonegativelyimpactthisconclusion.

References

Corby,J.,Doi,J.,Conville,J.,Murphy,S.etal.,"BiodegradabilityofaDenatoniumBitterant,"SAETechnicalPaper930587,1993,doi:10.4271/930587.

EuropeanChemicalsAgencyhttp://echa.europa.eu.Accessed7.1.2015and23.11.2018.

EuropeanCommission(2014).DetergentsIngredientsDatabase,version2014.1http://ec.europa.eu/environment/ecolabel/documents/did_list/didlist_part_a_en.pdf

EuropeanEnvironmentAgencyhttp://www.eea.europa.eu/themes/householdsAccessed7.1.2015.

HealthCanada(2011).ProposedRe-evaluationDecisionPRVD2011-15DenatoniumBenzoate08November2011.http://www.hc-sc.gc.ca/cps-spc/alt_formats/pdf/pubs/pest/decisions/rvd2012-06/rvd2012-06-eng.pdf

USConsumerProductSafetyCommission1992.StudyofAversiveAgentshttps://www.cpsc.gov//PageFiles/96066/aversive.pdf

Page20of21

ANNEXIV

Capsuleintegritytestprotocol

Scope

Thisprovidesguidanceonthetestdesign,executionandinterpretationtoevaluatetheintegrityofthecapsuleswhenincontactwithwater,andwhensubjectedtopressure.

Thetestsaresuitableforin-marketcomplianceinspectionsaswellasfortheevaluationofproductandprocessdesignandforqualitycontrolpurposes.

Thetestsarenon-destructive,i.e.eachsampleissubjectedtotheconditionsdefinedinthelegislationasthethresholdforcompliance.Foreachsample,theoutcomeofthetestiseither“pass”or“fail”.Itisallowedtocontinuethetestingbeyondthelegalthreshold,extendingthetestwithadestructivephase,todeterminewhatisthecriticalparametervalueatwhichthetestedcapsulefails.However,thisaspectofthetestisnotpartoftheA.I.S.E.guidanceandthesedataarenotrecommendedforacomplianceassessment.

Sampleconditioningpriortotesting

Sampleconditioningisanimportantmeasuretobeadoptedtoensuretestreproducibility.Therefore,capsulesshallbetestedimmediatelyafterhavingbeenconditionedatatemperatureof20±1°C)andat50±2%RelativeHumidityforatleast24hoursintheoriginalouterpackagingopenedtotheconditioningatmosphere.

Notethatforin-marketproductstesting,onlyproductsthatwereappropriatelytransported,storedandconditionedcan provide relevant and reproducible results according to the accepted international quality standards (see forinstanceASTMstandardD433213).

Capsuleintegritywhenincontactwithwater

A beaker of sufficient capacity is filled with at least 1 L of demineralised water. The water temperature shall bestabilisedat20±1°C.

Onepre-conditionedcapsuleisgentlyintroducedintothebeakeruntil it isentirelysubmerged.Thecapsuleshallbesurroundedbywateronallsides.Incasethedensityissuchthatthecapsuleeitherfloatsorsinks,thecapsuleshallbeplaced insideadevice thatprevents floatingorsinking (e.g.ametalcage,anettingbag,orsimilar)andthatallowsvisualobservation.

A30secondstimershallbestartedassoonasthecapsuleissubmerged.

Thecapsuleshallbecarefullyobservedduring30seconds,foranyvisualevidenceofliquidleavingthecapsule.

Thefollowingpictures illustratetheobservablestagesofcontainment loss(for illustrationonly-visualobservationsmaydifferdependingonthecapsuledesign,coloursizeorshape).

1) Priortoproductreleasewithfullyclosedcontainment.2) Themomentintimewhenfirstreleaseofproductisobserved.3) Furtherprogressofcontentreleaseandairescapesfromthecapsule.

Stage1 Stage2 Stage3

Thecriticalliquidcontentreleasetimeis30seconds.Anindividualcapsulesuccessfullypassesthetestifnoreleaseofliquid content occurred during the 30 seconds of submersion. Optionally, the test can be continued beyond thisduration.

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Capsuleintegritywhensubjectedtopressure

Thedynamometric test shallbeconductedunderconditions thataresimilar to theconditioningatmosphere (roomtemperature/approximately50%RelativeHumidity).

One capsule is subjected to an increasing compression force, between two flat plates of a surface larger than thesurfaceareaofthecapsule,atarateof200-250mm/min.Thiscanbeachievedwithstandardequipmentsuchase.g.Instronmodel5566(seepicturebelow),orequivalent.Duringthetest,thecapsuleistobeplacedinsideatransparentplasticbagtoavoidspillageorsplashes.Itshallbepositionedbetweenthetwoplatesthatapplytheforce,restingonitslargestsurfacearea.

While the capsule is carefully observed, the compression force shall be gradually increased either until 300N isreached,oralowerforceincasethecapsulealreadyreleasesitscontent.

Thecriticalmechanicalcompressionresistanceis300N.Anindividualcapsulesuccessfullypassesthetestifnoreleaseof liquidcontentoccurredduringcompressionuptoa forceof300N.Optionally, thetestcanbecontinuedbeyondthisthreshold.

Statisticalcriteriaforinspectionsusingthecapsuleintegritytests

Forinspections,todeterminewhetherabatchofcapsulesisnon-compliantwiththecapsuleintegritycriteria,A.I.S.E.recommendstoadoptmethodsandqualitycriteriavalidatedaccordingtointernationalproceduresasprovidedbytheISO2859-4standard14withadeclaredqualitylevelof5%non-conformingitems.AtLevel2(i.e.withalimitingnumberof2defects),thisimpliesthatthesamplesizeisn=16.Inotherwords,fromastatisticalpointofview,testresultsfor16samplescontradictthedeclaredqualitylevelifthenumberofdefectsis>2,whilethedeclaredqualitylevelisnotcontradictedifthenumberofdefectsis<=2.

14ISO (2002). Sampling procedures for inspection by attributes— Part4: Procedures for assessment of declared quality levels.ISO2859-4:2002(en).InternationalOrganizationforStandardization,Geneva,Switzerland.