1、A Referencenumbe r ISO18917:1999(E) INTERNATIONAL STANDARD ISO 18917 Firstedition 19990601 PhotographyDeterminationofresidual thiosulfateandotherrelatedchemicalsin processedphotographicmaterials Methodsusingiodineamylose,methylene blueandsilversulfide PhotographieDterminationduthiosulfatersidueletda
2、utresproduits chimiquesdanslesproduitsphotographiquestraitsMthodesliode amylose,aubleudemthylneetausulfuredargentISO18917:1999(E) ISO1999 Allrightsreserved.Unlessotherwisespecified,nopartofthispublicationmaybereproducedorutilizedinanyformorbyan ymeans,electronic ormechanical,includingphotocopyingand
3、microfilm,withoutpermissioninwritingfromthepublisher. InternationalOrganizationforStandardization Casepostale56 CH1211Genve20 Switzerland Internet isoiso.ch PrintedinSwitzerland ii Contents 1Scope 1 2Normativereferences . .1 3Generalrequirements. .2 4Iodineamylosemethod .3 5Methylenebluemethod .7 6S
4、ilverdensitometricmethod 11 AnnexA (informative) Appraisalofkeepingcharacteristics 16 AnnexB (informative) Guidanceintheselectionoftestmethod.17 AnnexC (informative) Preparationfor0,2mol/lsodiumhydroxidesolution18 AnnexD (informative) Preparationof1,000mol/lsodiumthiosulfatesolution 19 Bibliography2
5、1ISO ISO18917:1999(E) iii Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommi
6、tteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnongovernmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. DraftInternation
7、alStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. InternationalStandardISO18917waspreparedbyTechnicalCommitteeISO/TC42, Photography. Thisfirsteditioncancelsandreplacesthese
8、condeditionofISO417(ISO417:1993)whichhasbeentechnically revised.Asinthesecondedition,itincludestheiodineamyloseandmethyleneblueprocedures,butthereactant levelshavebeenmodifiedtoprovidemorereproducibleresults. AnnexesA,B,CandDofthisInternationalStandardareforinformationonly.ISO18917:1999(E) ISO iv In
9、troduction ThisInternationalStandardisoneofaseriesofspecificationsonphotographicprocessing.Individualswithouta workingknowledgeofanalyticalchemistrymayoccasionallyusethisInternationalStandard.Hazardwarningshave thereforebeengivenusingasystemofsymbolswithlettercodesdesignatingthenatureofthehazard.Mor
10、e detailedinformationregardinghazards,handlinganduseofthesechemicalsmayalsobeavailablefromthe manufacturer. Determinationofresidualthiosulfateanditsdecompositionproductsisofuseinappraisingtheadequacyofwashing andthereforethepermanenceofthesilverimageonphotographicfilms,platesandpapers.Inadequatewash
11、ing cancausealossinimagedensityandtheformationofstaininlowdensityareas.Thesedeleteriouseffectsare acceleratedbyimproperstorageconditions. Determinationofresidualthiosulfateandrelatedcompounds,byitself,isnotsufficienttoinsurethepermanenceof photographicrecords.Longtermorarchivalstoragerequirespropera
12、ttentiontoenclosurematerials,storage environment,andthelike.TheseconsiderationsarespecifiedinISO3897,ISO5466,ISO6051andISO10602.INTERNATIONALSTANDARD ISO ISO18917:1999(E) 1 PhotographyDeterminationofresidualthiosulfateandother relatedchemicalsinprocessedphotographicmaterialsMethods usingiodineamylos
13、e,methyleneblueandsilversulfide 1Scope 1.1 ThisInternationalStandardspecifiestestmethodsforthedeterminationofresidualthiosulfateandother relatedchemicalsinprocessedphotographicmaterials. 1.2 ThisInternationalStandardappliestosilverhalide/gelatinproductsthathavebeenprocessedwithafinal thiosulfatefixi
14、ngbathandawaterwash.ThisInternationalStandarddoesnotapplytostabilisedblackandwhite products,thermallyprocessedfilms,orinstanttypeproducts.TheproceduresgiveninthisInternationalStandard measureresidualthiosulfate,andthesilverdensitometricmethodmeasuresresidualrelatedpolythionatematerials aswell. Measu
15、rementscarriedoutbytheproceduresinthisInternationalStandardmay,withinthelimitationsstated inannexesAandB,correlatewiththeimagestabilitiesofprocessedphotographs. 1.3 Filmorplateswithphotographicsensitivelayersonbothsides,orwithaphotographicsensitivelayeronone sideandagelatinbackinglayeronthereversesi
16、de,maycontainapproximatelytwiceasmuchthiosulfateafter processingassampleshavingacoatingononesideonly.Thissituationwillbetrueformaterialsforwhichresidual thiosulfateisdeterminedbytheiodineamyloseormethyleneblueprocedures. NOTE Forthemethodofreportingsuchresults,seefigure1,example2. 1.4 Theiodineamylo
17、se canbeusedwithfibrebasedpaper,resincoatedpaper,filmsandplates.Itisthemethod tobeusedwithfilmsandpaperscontainingincorporateddevelopingagents. 1.5 Themethylenebluemethodcanbeusedwithfibrebasedpaper,resincoatedpaper,filmsandplatesbutnot withfilmsandpapercontainingincorporateddevelopingagents. 1.6 Th
18、esilversulfidedensitometricmethodmeasuresthiosulfates,polythionatesandallotherresidualchemicals inaprocessedproductthatreactwithsilveriontoformasilver“stain“undertheconditionsofthetest. 1.7 Atabulatedsummary ofmethods,scope,etc.isgiveninannexB. 2Normative references Thefollowingnormativedocumentscon
19、tainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthese publicationsdonotapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthem
20、ostrecenteditionsofthenormativedocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIEC maintainregistersofcurrentlyvalidInternationalStandards . ISO53:1995, PhotographyDensitymeasurements Part3: Spectralconditions. ISO103491:1992, Phot
21、ographyPhotographicgradechemicalsTestmethods Part1: General.ISO18917:1999(E) ISO 2 3General requirements 3.1 Safetyandhazardconcerns 3.1.1Handling Reagentsshallbehandledinconformitywithhealthandsafetyprecautionsasshownoncontainersorasgivenin othersourcesofsuchinformation.Properlabellingofpreparedrea
22、gentsincludeschemicalname,dateof preparation,expirationdate,restandardizationdate,nameofpreparer,andadequatehealthandsafetyprecautions. Thedischargeofreagentsshallconformtoapplicableenvironmentalregulations. 3.1.2Hazard warnings Someofthechemicalsspecifiedinthetestproceduresarecaustic,toxicorotherwi
23、sehazardous.Safelaboratory practiceforthehandlingofchemicalsrequirestheuseofsafetyglassesorgoggles,rubberglovesandother protectiveapparelsuchasfacemasksorapronswhereappropriate.Specificdangernoticesaregiveninthetextfor particularlydangerousmaterials,butnormalprecautionsarerequiredduringtheperformanc
24、eofanychemical procedureatalltimes. Thefirsttimethatahazardousisnotedinthetestprocedure,thehazardshallbeindicatedbytheword“DANGER” followedbyasymbolconsistingofanglebrackets“ “containingaletterwhichdesignatesthespecifichazard.A doublebracket“ “shallbeusedforparticularlyperiloussituations. Insubseque
25、ntstatementsinvolvinghandlingofthesehazardousmaterials,onlythehazardsymbolconsistingofthe bracketsandletter(s)shallbedisplayed.Furthermore,foragivenmaterial,thehazardsymbolsshallbeusedonly onceinasingleparagraph. DetailedwarningsforhandlingchemicalsandtheirdilutedsolutionsarebeyondthescopeofthisInte
26、rnational Standard. Employersshallprovidetrainingandhealthandsafetyinformationinconformancewithlegal requirements. ThehazardsymbolsystemusedinthisInternationalStandardisintendedtoprovideinformationtotheusersandis notmeantforcompliancewithlegalrequirementsforlabelling,asthesevaryfromcountrytocountry.
27、 Itisstronglyrecommendedthatanyoneusingthesechemicalsobtainfromthemanufacturerpertinent informationaboutthehazards,handling,useanddisposalofthesechemicals. 3.1.3 Hazardinformationcodesystem B Harmfulifinhaled.Avoidbreathingdust,vapour,mistorgas.Useonlywithadequateventilation. C Harmfulifcontactoccur
28、s.Avoidcontactwitheyes,skinorclothing.Washthoroughlyafterhandling. S Harmfulifswallowed.Washthoroughlyafterhandling.Ifswallowed,obtainmedicalattentionimmediately. S Maybefatalifswallowed.Ifswallowed,obtainmedicalattentionimmediately. F Willburn.Keepawayfromheat,sparks,andopenflame.Usewithadequateven
29、tilation. O Oxidizer.Contactwithothermaterialmaycausefire.Donotstorenearcombustiblematerials. Theflammablewarningsymbol, F ,shallnotbeusedforquantitiesofcommonsolventsunder1litre.ISO ISO18917:1999(E) 3 3.2Reagents Reagentsusedinthetestproceduresshallbecertifiedreagentgradechemicalsandshallmeetapprop
30、riate standardsorbechemicalsofpurityacceptablefortheanalysis. NOTE FurtherdetailsaregiveninISO63531,ISO63532andISO63533(seebibliography). Wheneverwaterisspecifiedwithoutotherqualifiersinthetestprocedures,onlydistilledwaterorwaterofatleast equalpurityshallbeused. 3.3Glassware Allglasswaresubjecttohea
31、tingshallbeofheatresistantborosilicateglass. 1) PipettesandothervolumetricglasswareshallmeetthevolumerequirementsofClassAorClassBglasswareas specifiedinISO103491. 4Iodineamylose method 4.1Use Theiodineamylosemethodisapplicabletothedeterminationofresidualthiosulfateionsinfilmandresincoated photograph
32、icpapercontainingincorporateddevelopingagents.Theprocedurecoverstherangefrom0,002 m g/cm 2 to0,40 m g/cm 2 .Themethodisalsoapplicabletomeasuringresidualthiosulfateioninfibrebasedpaper,filmand plates.Thismethodmeasuresonlythiosulfateionsandgivesresultscomparabletothoseobtainedbythe methylenebluemetho
33、d. Themethodgivesresultsthatcorrelatewellwithacceleratedkeepingtestsofseveralprocessedmicrofilmsandis applicabletocolouraswellasblackandwhiteproducts. 4.2Principle Theeluent(4.4.4)isaddedtothesampletoextractresidualthiosulfate,tetrathionateandpentathionateions. Formalinisaddedtoformacomplexwithanysu
34、lfiteionpresent.Iodineisaddedtoanamylose(fractionatedlinear potatostarch)indicatortoformabluecolouredsolution.Thethiosulfateintheeluent,whenaddedtotheiodine amylosesolution,willreactwiththeiodineandproportionatelyreducetheintensityofthebluecolour.Thelossin colourcorrespondstothethiosulfateconcentrat
35、ion. 4.3Chemical reactions a)Starch (C 6 H 10 O 5 ) n +I 2 (inKIsolution) Bluecolouredsolution b) Bluecolouredsolution+ SO 23 2- Decreaseinbluecolourintensity 4.4Reagents 4.4.1Potassium iodate,c(KIO 3 )=0,000017mol/l(0,00357g/l) Preparea0,0167mol/lsolutionofpotassiumiodatebyweighing0,357gofpotassium
36、iodate(DANGER: O )and placingitina100mlonemarkvolumetricflask,makinguptothemarkwithwaterandmixingwell.Pipette1,0mlof the0,0167mol/lpotassiumiodatesolutionintoa1litreonemarkvolumetricflask,makinguptothemarkwith water. 1) Pyrex isanexampleofsuitableglasswareavailablecommercially.Thisinformationisgiven
37、fortheconvenienceof usersof thisInternationalStandardanddoesnotconstituteanendorsementbyISOofthisbrand.ISO18917:1999(E) ISO 4 4.4.2Formate buffer,pH2,0 Add,fromagraduatedcylinder,110mlofformicacid(HCO 2 H)(8890%)(DANGER: C B S F )toa1litre onemarkvolumetricflaskcontaining500mlto600mlofwater,andmakeu
38、ptothemarkwithwater.UsingapH meter,adjustthesolutiontopH2,0 0,1at21Cwith10mol/lsodiumhydroxidesolution(4.4.8)(DANGER: C ) fromadroppingpipette. 4.4.3Formate buffer,pH2,8 Pipette10,0mlofpH2,0formatebuffer(4.4.2)intoa1litreonemarkvolumetricflaskandmakeuptothemarkwith water. 4.4.4Eluent Dissolve1,0g 0,
39、1gofpotassiumiodide(KI)and1,0g 0,1gofpotassiummonohydrogenphosphatetrihydrate (K 2 HPO 4 3H 2 O)anddiluteto1litrewithwater.UsingapHmeter,adjusttopH8,5at21 Cbyadding0,5mol/l sulfuricacid(4.4.9)dropbydropfromadroppingpipette. 4.4.5 Cadmiumiodideamylosereagent (CdI 2 amylose) NOTE Batchesshouldbelimite
40、dto1litrevolumes. Addanddissolve11,0g 1gofcadmiumiodide(CdI 2 )(DANGER:Carcinogen 2) )in400mlofwater,andboil gentlyfor15min.Addafurther400mlofwaterandheattoboiling.Continueboilingandslowlyadd,whilestirring, 5,0gofamylose 3) .Boilandstirfor5min.Continueboilingandslowlyadd,withstirring,5,0gofacidwashe
41、d analyticalfilteraid 4) .Boilandstirfor5min. Whilethesolutionisstillhot,filteritunderahighvacuum,usingaBuchnerfunnel(4.5.1.5)withthefineporosity filterpaper (4.5.1.6)intoa1litrevacuumflask.Transferthefiltratetoa1litrevolumetricflask.Rinsethevacuum flaskwithwaterandaddtherinsingstothevolumetricflask
42、.Diluteto1litrewithwater. 4.4.6Sodium thiosulfate,c(Na 2 S 2 O 3 )=0,1000mol/l(15,8g/l) Commerciallyavailableanalysedreagentsolutionsarerecommended.AnnexDprovidesaprocedureforthe preparationofstandardsodiumthiosulfatesolutionusingsodiumthiosulfatepenthahydrate(Na 2 S 2 O 3 5H 2 O). 4.4.7Formalin(DANGER: B C S ) 4.4.8Sodium hydroxide,c(NaOH)=10mol/l(DANGER: C ) Thissolutionmaybepreparedfromsodiumhydroxide(DANGER: C ). 4.4.9Su
