GB/T 19719-2005 首饰 镍释放量的测定 光谱法

ICS39.060

Y88

NATIONALSTANDARD

OFTHEPEOPLE'SREPUBLICOFCHINA

中华人民共和国国家标准

GB/T19719-2005

Jewellery-Determinationofthereleaseofnickel-

Methodofspectrometry

首饰镍释放量的测定光谱法

IssuedonMarch23,2005ImplementedonSeptember1.2005

JointlyissuedbytheGeneralAdministrationofQualitySupervision,Inspectionand

Quarantine(AQSIQ)andtheStandardizationAdministration(SAC)

ofthePeople'sRepublicofChina

GB/T19719-2005

Foreword

ThisstandardisrevisedfromthestandardofEN1811:1998<Referencetestmethodfor

releaseofnickelfromproductsintendedtocomeintodirectandprolongedcontactwiththe

skin.>(Englishversion).

Inordertobereferredeasily,thisstandardisamendedoneditasthefollowing:

a)"ThisEuropeanStandard"isreplacedby"ThisStandard";

b)","usedasperiodisreplacedby".";

c)"cm3"isreplacedby"mL";

d)Deletetheforewordoftheinternationalstandard;

e)AddtheinformativeannexEforguidance.

TheannexA,B,C,D,EandFareinformativeannex.

ThisstandardisproposedbyChinaNationalLightIndustryCouncil.

Thisstandardisunderthejurisdictionofstandardizationtechnicalcommitteeof

jewelry(SAC/TC256).

Draftingorganizationofthisstandard:Nationaljewelryqualitysupervisionandinspection

center,NationalCneterofQualitySupervision&InspectiononGold-Sliver

Products(Nanjing)andNationalCneterofQualitySupervision&InspectiononGold-Sliver

Products(Shanghai)

Chiefdraftingstaffofthisstandard:LiWujun,WangDonghui,FangMingwu,FanJifang,,

LiYupeng,LiSuqing.

GB/T19719-2005

Jewelry–Determinationofthereleaseofnickel-Methodofspectrometry

1.Scope

ThisGBStandardspecifiesamethodforsimulatingthereleaseofnickelfromarticlesin

ordertodeterminewhethersuchitemsreleasenickelatarategreaterthan0.5

2

mg/cm/week.

Thisstandardisapplicabletotheclause4.3.2ofGB11887-2002,whichisaboutthe

jewelrycontainingnickel,andalsoapplicabletothearticlewhichprolongedcontactwith

theskin.

2.NormativeReference

Thefollowingdocumentsarenecessarywhenthistextisapplied.Fordatedreference,only

thedatededitionappliestothisstandard.Forundatedreferences,thelatesteditionofthe

normativedocument(includingalltheamendments)isapplicabletothisstandard.

GB11887-2002Jewelry-finenessofthepreciousmetalandnamingmethod(ISO

9202:1991.NEQ).

3.Principle

Theitemtobetestedfornickelreleaseisplacedinanartificialsweattestsolutionforone

week.Theconcentrationofdissolvednickelinthesolutionisdeterminedbyatomic

absorptionspectrometry,inductively-coupledplasmaspectrometryorotherappropriate

analyticalmethod.Thenickelreleaseisexpressedinmicrogramspersquarecentimeterper

2

week(mg/cm/week).

4.Reagents

Exceptwhereindicated,allreagentsshallbeofrecognizedproanalysis,p.a.,gradeor

betterandshallbefreeofnickel.Andthewaterisdeionizedandaeratedwater.

4.1Sodiumchloride.

4.2Urea

4.3Deionizedwater,theelectricalconductivityisnotlessthan1µs/cm

4.4.DL-Lacticacid,r=1.21g/ml,>88%(m/m).

4.5Ammoniasolution,r=0.91g/ml,25%(m/m).

4.6Nitricacid.

4.7Diluteammoniasolution,1%(m/m).Transfer10mlofammoniasolution(4.5)intoa

250mlbeakercontaining100mlofdeionizedwater.Stirandcooltoroomtemperature.

Transferthesolutiontoa250mlvolumetricflaskandmakeuptovolumewithdeionized

water.

4.8Dilutenitricacid,approximately5%(m/m).Transfer30mlofnitricacid(4.6)intoa

500mlbeakercontaining350mlofdeionizedwater.Stirandcooltoroomtemperature.

Transferthesolutiontoa500mlvolumetricflaskandmakeuptovolumewithdeionized

water.

4.9Degreasingsolution.Dissolve5gofananionicsurface-activeagentsuchassodium

dodecylbenzenesulfonateorsodiumalkylarylsulfonatein1000mlwater.An

appropriately-diluted,neutral,commercially-availabledetergentmaybeused.

4.10Waxorlacquer(suitableforelectroplatingpurposes)capableofprotectingasurface

fromnickelrelease.Thewaxorlacquershallbeshowntopreventnickelreleasefroma

nickel-releasingsurfacewhenoneormorecoatsofthewaxorlacquerareappliedinthe

samemannerasonatestsample,andtestedfornickelreleaseaccordingtoclause6(see

annexC).

5Apparatus

5.1ApH-meter,accurateto0.02pH.

5.2Ananalyticalspectrometer,capableofdetectingaconcentrationof0.01mgnickelper

litre.Theinstrumentshall,afteroptimization,meettheperformancecriteriagivenin5.2.1

and5.2.2.Itisrecommendedthateitheraninductively-coupledplasma-opticalemission

spectrometeroranelectrothermalexcitationatomicabsorptionspectrometerisused.

5.2.1MinimumprecisionThestandarddeviationof10measurementsoftheabsorptionofa

fullmatrixcalibrationsolutioncontaining0.05mgnickelperlitreshallnotexceed10%.

5.2.2LimitofdetectionThelimitofdetectionshallbeconsideredastwicethestandard

deviationof10measurementsoftheabsorbanceofafullmatrixsolutioncontainingnickel

ataconcentrationlevelselectedtogiveanabsorbancejustabovethatofthezero

calibrationsolution.Thelimitofdetectionofnickelinamatrixsimilartothefinaltest

solutionshallbebetterthan0.01mg/l.

5.3Thermostaticallycontrolledwater-bathoroven,capableofmaintainingatemperature

of(30±2)℃.

5.4Avesselwithlid,bothcomposedofanon-metallic,nickel-freeandnitric-acid-resistant

material,suchasglassand/orpolypropyleneand/orpolytetrafluoroethyleneand/or

polystyrene.Thesampleshallbesuspendedintheliquidbyaholdermadefromthesame

materialsaslistedabove,soastominimizecontactofthesamplearea(6.1.1)withthe

wallsandbaseofthevessel.Thesizeandshapeofvesselandholdershallbechosensoas

tominimizethevolumeoftestsolutionrequiredtocompletelycovertheobjecttobetested.

Inordertoremoveanytraceofnickel,thevesselandholdershallbepre-treatedbybeing

storedinasolutionofdilutenitricacid(4.8)foratleast4h.Afteracidtreatment,rinsethe

vesselandholderwithdeionizedwateranddry.

6Samples

6.1Samplearea

6.1.1Definitionofsamplearea

Onlythesurface(s)ofanitemthatcomesintodirectandprolongedcontactwiththeskin

shallbeanalyzed.Inthisstandardsuchsurfacesaredefinedassamplearea.

6.1.2Determinationofsamplearea

Determinationofthesamplearea(a)insquarecentimetresisachievedbymarkingthe

contourofthesampleareaassumingthattheitemiswornorusedasintended(seeannex

C).Inordertoachievetherequireddegreeofanalyticalsensitivity,aminimumsamplearea

of0.2cm2shallbetested.Ifnecessary,identicalitemsmaybetreatedtogethertoobtainthis

minimumarea.

6.1.3Areasotherthansampleareas

Inordertopreventreleaseofnickelfromareasotherthanthesamplearea,suchareasshall

beremovedorprotectedfromthetestsolution.Thismaybeachievedafterdegreasing(see

6.2)by,forexample,theapplicationofoneormorecoatingsofawaxorlacquerwhichhas

beenshowntoprotectfromnickelrelease(4.10).AnnexCgivesguidanceonthecoatingof

protectedareaspriortotesting.Whereitisnotfeasibletoremoveorprotectallareasother

thanthesamplearea,forexamplewithcertainwatchbracelets,suchunprotectedsurfaces

shallbeconsideredaspartofthesamplearea.NOTEIf,whennon-significantsurfacesare

consideredtobepartofthesamplearea,thenickelreleasefromtheitemisfoundtobe

unacceptable,considerationshouldbegiventodismantlingtheitemandtestingany

internalcomponentsfornickelrelease.Ifthenickelreleasefromsuchinternalcomponents

issignificantitmightbeappropriatetotesttheexternalcomponentsontheirown,

assumingthattheyareavailable,orthematerialsfromwhichtheitemhasbeen

manufactured(seeannexD).

6.2SamplepreparationGentlyswirlthesamplefor2minindegreasingsolution(4.9)at

roomtemperature.Rinsethoroughlywithdeionizedwateranddry.Afterdegreasing,items

shouldbehandledwithplasticforcepsorcleanprotectivegloves.

NOTEThiscleaningstageisintendedtoremoveextraneousgreaseandskinsecretionsdue

tohandling,butnotanyprotectivecoatings.However,itwillalsosubstantiallyremoveany

nickelcontaminationthatmightbepresentonthesurfaceoftheitem.Ifthereisa

requirementtodeterminethisnickelthecleaningstageshouldbeomitted.However,it

shouldbeappreciatedthatomissionofthiscleaningstagemightitselfaffectthenickel

releasefromtheitem.

6.3Referencedisc

Asaqualitycontrolcheck,thenickelreleasefromareferencediscmaybedetermined(see

annexB).

Ifused,itisimportantthatbothsidesofareferencediscareabradedbeforeeachtest.A

minimumof0.05mmshallbeabradedfromeachsurfaceusingwetemerypaperNo.600

followedbyNo.1200.Thediscisthendegreasedinthesa