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EN ISO 1736:2000

(Main)

Dried milk and dried milk products - Determination of fat content - Gravimetric method (Reference method) (ISO 1736:2000)

Dried milk and dried milk products - Determination of fat content - Gravimetric method (Reference method) (ISO 1736:2000)

Migrated from Progress Sheet (TC Comment) (2000-07-10): /hall be // at formal vote level (glg/98-02-06)

Milchpulver und Trockenmilcherzeugnisse - Bestimmung des Fettgehaltes - Gravimetrisches Verfahren (Referenzverfahren) (ISO 1736:2000)

Diese Internationale Norm legt das Referenzverfahren für die Bestimmung des Fettgehaltes von Milchpulver und Trockenmilcherzeugnissen fest. Das Verfahren gilt für Milchpulver mit einem Fettgehalt von mindestens 40% (Massenanteil), Vollmilchpulver, teilentrahmtes Milchpulver und Magermilchpulver, Molkenpulver und Butterserumpulver.

Lait sec et produits à base de lait sec - Détermination de la teneur en matière grasse - Méthode gravimétrique (Méthode de référence) (ISO 1736:2000)

Mleko v prahu in suhi mlečni proizvodi - Določevanje maščob - Gravimetrijska metoda (Referenčna metoda) (ISO 1736:2000)

General Information

Status
Withdrawn
Publication Date
29-Feb-2000
Withdrawal Date
14-Oct-2008
ICS
67.100.01 - Milk and milk products in general
Technical Committee
CEN/TC 302 - Milk and milk products - Methods of sampling and analysis
Drafting Committee
CEN/TC 302 - Milk and milk products - Methods of sampling and analysis
Current Stage
9960 - Withdrawal effective - Withdrawal
Start Date
15-Oct-2008
Completion Date
15-Oct-2008
Ref Project
SIST EN ISO 1736:2001 - Dried milk and dried milk products - Determination of fat content - Gravimetric method (Reference method) (ISO 1736:2000)

Relations

Replaced By
EN ISO 1736:2008 - Dried milk and dried milk products - Determination of fat content - Gravimetric method (Reference method)(ISO 1736:2008)
Effective Date
22-Dec-2008

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.YLPHWULMVNDMilchpulver und Trockenmilcherzeugnisse - Bestimmung des Fettgehaltes - Gravimetrisches Verfahren (Referenzverfahren) (ISO 1736:2000)Lait sec et produits a base de lait sec - Détermination de la teneur en matiere grasse - Méthode gravimétrique (Méthode de référence) (ISO 1736:2000)Dried milk and dried milk products - Determination of fat content - Gravimetric method (Reference method) (ISO 1736:2000)67.100.10SURL]YRGLMilk and processed milk productsICS:Ta slovenski standard je istoveten z:EN ISO 1736:2000SIST EN ISO 1736:2001en01-februar-2001SIST EN ISO 1736:2001SLOVENSKI
STANDARD



SIST EN ISO 1736:2001



SIST EN ISO 1736:2001



SIST EN ISO 1736:2001



ReferencenumberISO1736:2000(E)©ISO2000INTERNATIONALSTANDARDISO1736Thirdedition2000-03-01Driedmilkanddriedmilkproducts—Determinationoffatcontent—Gravimetricmethod(Referencemethod)Laitsecetproduitsàbasedelaitsec—Déterminationdelateneurenmatièregrasse—Méthodegravimétrique(Méthodederéférence)SIST EN ISO 1736:2001



ISO1736:2000(E)PDFdisclaimerThisPDFfilemaycontainembeddedtypefaces.InaccordancewithAdobe'slicensingpolicy,thisfilemaybeprintedorviewedbutshallnotbeeditedunlessthetypefaceswhichareembeddedarelicensedtoandinstalledonthecomputerperformingtheediting.Indownloadingthisfile,partiesacceptthereintheresponsibilityofnotinfringingAdobe'slicensingpolicy.TheISOCentralSecretariatacceptsnoliabilityinthisarea.AdobeisatrademarkofAdobeSystemsIncorporated.DetailsofthesoftwareproductsusedtocreatethisPDFfilecanbefoundintheGeneralInforelativetothefile;thePDF-creationparameterswereoptimizedforprinting.EverycarehasbeentakentoensurethatthefileissuitableforusebyISOmemberbodies.Intheunlikelyeventthataproblemrelatingtoitisfound,pleaseinformtheCentralSecretariatattheaddressgivenbelow.©ISO2000Allrightsreserved.Unlessotherwisespecified,nopartofthispublicationmaybereproducedorutilizedinanyformorbyanymeans,electronicormechanical,includingphotocopyingandmicrofilm,withoutpermissioninwritingfromeitherISOattheaddressbeloworISO'smemberbodyinthecountryoftherequester.ISOcopyrightofficeCasepostale56CH-1211Geneva20Tel.+41227490111Fax+41227341079E-mailcopyright@iso.chWebwww.iso.chPrintedinSwitzerlandii©ISO2000–AllrightsreservedSIST EN ISO 1736:2001



ISO1736:2000(E)©ISO2000–AllrightsreservediiiContentsPageForeword.iv1Scope.12Normativereference.13Termanddefinition.14Principle.15Reagents.26Apparatus.27Sampling.38Preparationoftestsample.39Procedure.49.1Testportion.49.2Blanktests.49.3Preparationoffat-collectingvessel.49.4Determination.510Calculationandexpressionofresults.710.1Calculation.710.2Expressionofresults.711Precision.711.1Interlaboratorytest.711.2Repeatability.811.3Reproducibility.812Testreport.8AnnexA(informative)Notesonprocedures.9AnnexB(informative)Alternativeprocedureusingfat-extractiontubeswithsiphonorwash-bottlefittings.11Bibliography.14SIST EN ISO 1736:2001



ISO1736:2000(E)iv©ISO2000–AllrightsreservedForewordISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISOmemberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcommittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhastherighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,inliaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission(IEC)onallmattersofelectrotechnicalstandardization.InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3.DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting.PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote.AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectofpatentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.InternationalStandardISO1736waspreparedbyTechnicalCommitteeISO/TC34,Agriculturalfoodproducts,SubcommitteeSC5,Milkandmilkproducts,incollaborationwiththeInternationalDairyFederation(IDF)andAOACInternational,andwillalsobepublishedbytheseorganizations.Thisthirdeditioncancelsandreplacesthesecondedition(ISO1736:1985),whichhasbeentechnicallyrevised.AnnexesAandBofthisInternationalStandardareforinformationonly.SIST EN ISO 1736:2001



INTERNATIONALSTANDARDISO1736:2000(E)©ISO2000–Allrightsreserved1Driedmilkanddriedmilkproducts—Determinationoffatcontent—Gravimetricmethod(Referencemethod)WARNING—TheuseofthisInternationalStandardmayinvolvehazardousmaterials,operationsandequipment.Thisstandarddoesnotpurporttoaddressallthesafetyproblemsassociatedwithitsuse.Itistheresponsibilityoftheuserofthisstandardtoestablishsafetyandhealthpracticesanddeterminetheapplicabilityofregulatorylimitationspriortouse.1ScopeThisInternationalStandardspecifiesthereferencemethodforthedeterminationofthefatcontentofdriedmilkanddriedmilkproducts.Themethodisapplicabletodriedmilkwithafatcontentof40%(massfraction)ormore,driedwhole,driedpartiallyskimmed,anddriedskimmedmilk,driedwhey,driedbuttermilkanddriedbutterserum.NOTEWhenthepowdercontainshardlumpswhichdonotdissolveinammoniasolutionorcontainsfreefattyacidsinsignificantquantities,noticeablebyadistinctsmell,theresultofthedeterminationwillbetoolow.WithsuchproductsrecourseshouldbemadetoamethodusingtheWeibull-Berntropprinciple(seeISO8262-3).2NormativereferenceThefollowingnormativedocumentcontainsprovisionswhich,throughreferenceinthistext,constituteprovisionsofthisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,thispublicationdonotapply.However,partiestoagreementbasedonthisInternationalStandardareencouragedtoinvestigatethepossibilityofapplyingthemostrecenteditionofthenormativedocumentindicatedbelow.Forundatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIECmaintainregistersofcurrentlyvalidInternationalStandards.ISO3889,Milkandmilkproducts—Determinationoffatcontent—Mojonnier-typefatextractionflasks.3TermanddefinitionForthepurposesofthisInternationalStandard,thefollowingtermanddefinitionapplies.3.1fatcontentofdriedmilkanddriedmilkproductsmassfractionofsubstancesdeterminedbytheprocedurespecifiedinthisInternationalStandardNOTEThefatcontentisexpressedasamassfraction,inpercent[formerlygivenas%(m/m)].4PrincipleAnammoniacalethanolicsolutionofatestportionisextractedwithdiethyletherandlightpetroleum.Thesolventsareremovedbydistillationorevaporation.Themassofthesubstancesextractedisdetermined.NOTEThisisusuallyknownastheRöse-Gottliebprinciple.SIST EN ISO 1736:2001



ISO1736:2000(E)2©ISO2000–Allrightsreserved5ReagentsUseonlyreagentsofrecognizedanalyticalgrade,unlessotherwisespecified,anddistilledordemineralizedwaterorwaterofequivalentpurity.Thereagentsshallleavenoappreciableresiduewhenthedeterminationiscarriedoutbythemethodspecified(see9.2.2).5.1Ammoniasolution,containingamassfractionofNH3ofapproximately25%(20=910g/l).NOTEIfammoniasolutionofthisconcentrationisnotavailable,amoreconcentratedsolutionofknownconcentrationmaybeused(see9.4.2).5.2Ethanol(C2H5OH),orethanoldenaturedbymethanol,containingavolumefractionofethanolofatleast94%.(SeeA.5.)5.3CongoredsolutionDissolve1gofCongoredinwaterina100mlone-markvolumetricflask(6.14).Dilutetothemarkwithwater.NOTETheuseofthissolution,whichallowstheinterfacebetweenthesolventandaqueouslayerstobeseenmoreclearly,isoptional(see9.4.4).Otheraqueouscoloursolutionsmaybeusedprovidedthattheydonotaffecttheresultofthedetermination.5.4Diethylether(C2H5OC2H5),freefromperoxides(seeA.3),containingnomorethan2mg/kgofantioxidants,andcomplyingwiththerequirementsfortheblanktest(see9.2.2,A.1andA.4).NOTETheuseofdiethylethercouldleadtohazardoussituations.Duetoexpectedchangesinsafetyregulations,studiesareongoingtoreplacediethyletherbyanotherreagentprovidedthatitdoesnotaffecttheendresultofthedetermination.5.5Lightpetroleum,withanyboilingrangebetween30°Cand60°Cor,asequivalent,pentane(CH3[CH2]3CH3)withaboilingpointof36°Candcomplyingwiththerequirementsfortheblanktest(see9.2.2,A.1andA.4).NOTETheuseofpentaneisrecommendedbecauseofitshigherpurityandconstantquality.5.6MixedsolventShortlybeforeuse,mixequalvolumesofdiethylether(5.4)andlightpetroleum(5.5).6ApparatusWARNING—Sincethedeterminationinvolvestheuseofvolatileflammablesolvents,allelectricalapparatusemployedshallcomplywithlegislationrelatingtothehazardsinusingsuchsolvents.Usuallaboratoryequipmentand,inparticular,thefollowing.6.1Analyticalbalance,capableofweighingtothenearest1mg,withareadabilityof0,1mg.6.2Centrifuge,capableofholdingthefat-extractionflasksortubes(6.6)andcapableofspinningatarotationalfrequencyof500min–1to600min–1toproducearadialaccelerationof80gto90gattheouterendoftheflasksortubes.NOTETheuseofthecentrifugeisoptionalbutrecommended(see9.4.7).6.3Distillationorevaporationapparatus,fordistillingthesolventsandethanolfromtheboilingorconicalflasks,orevaporatingfrombeakersanddishes(see9.4.14)atatemperaturenotexceeding100°C.SIST EN ISO 1736:2001



ISO1736:2000(E)©ISO2000–Allrightsreserved36.4Dryingoven,electricallyheated,withventilationport(s)fullyopen,capableofbeingmaintainedatatemperatureof102°C2°Cthroughoutitsworkingspace.Theovenshallbefittedwithasuitablethermometer.6.5Waterbath,capableofbeingmaintainedatatemperatureof65°C5°C.6.6Mojonnier-typefat-extractionflasks,asspecifiedinISO3889.NOTEItisalsopossibletousefat-extractiontubes,withsiphonorwash-bottlefittings,butthentheprocedureisdifferent.ThealternativeprocedureisgiveninannexB.Thefat-extractionflasksshallbeprovidedwithgoodqualitycorksorstoppersofanothermaterial[e.g.siliconerubberorpolytetrafluoroethylene(PTFE)]unaffectedbythereagentsused.Barkcorksshallbeextractedwiththediethylether(5.4),keptinwateratatemperatureof60°Cormoreforatleast15min,andshallthenbeallowedtocoolinthewatersothattheyaresaturatedwhenused.6.7Rack,forholdingthefat-extractionflasks(ortubes)(6.6).6.8Washbottle,suitableforusewiththemixedsolvent(5.6).Aplasticswashbottleshallnotbeused.6.9Fat-collectingvessels,suchasboilingflasks(flat-bottomed),ofcapacities125mlto250ml,conicalflasks,ofcapacity250ml,ormetaldishes.Ifmetaldishesareused,theyshallbeofstainlesssteel,flat-bottomedwithadiameterof80mmto100mmandaheightofapproximately50mm.6.10Boilingaids,fat-free,ofnon-porousporcelainorsiliconcarbide(optionalwhenmetaldishesareused).6.11Measuringcylinders,ofcapacities5mland25ml.6.12Pipettes,graduated,ofcapacity10ml.6.13Tongs,madeofmetal,forholdingflasks,beakersordishes.6.14Volumetricflask,one-mark,ofcapacity100ml.7SamplingSamplingisnotpartofthemethodspecifiedinthisInternationalStandard.ArecommendedsamplingmethodisgiveninISO707.Itisimportantthatthelaboratoryreceiveasamplewhichistrulyrepresentativeandhasnotbeendamagedorchangedduringtransportorstorage.Storethesamplesatatemperatureofbetween2°Cand6°Cfromthetimeofsampling.8PreparationoftestsampleThoroughlymixthetestsamplebyrepeatedlyrotatingandinvertingthesamplecontainer.Ifnecessary,transferallofthetestsampletoanairtightcontainerofapproximatelytwicethevolumeofthetestsampletoallowthisoperationtobecarriedout.SIST EN ISO 1736:2001



ISO1736:2000(E)4©ISO2000–Allrightsreserved9ProcedureNOTE1Ifitisrequiredtocheckwhethertherepeatabilitylimit(11.2)ismet,carryouttwosingledeterminationsinaccordancewith9.1to9.4.NOTE2Analternativeprocedureusingfat-extractiontubeswithsiphonorwash-bottlefittings(seenotein6.6)isgiveninannexB.9.1TestportionMixthetestsample(clause8)bygentlystirringorrotatingandinvertingthecontainerseveraltimes.Immediatelyweightothenearest1mg,directlyorbydifference,inafat-extractionflask(6.6)oneofthefollowingtestportions:a)about1gofdriedhigh-fatmilk,ofdriedwholemilkorofdriedbutterserum;b)about1,5gofdriedpartiallyskimmedmilk;c)about1,5gofdriedskimmedmilk;d)about1,5gofdriedwhey;e)about1,5gofdriedbuttermilk.Transferthetestportionascompletelyaspossibleintothelower(small)bulbofthefat-extractionflask.9.2Blanktests9.2.1BlanktestformethodCarryoutablanktestsimultaneouslywiththedeterminationusingthesameprocedureandsamereagents,butreplacingthedispersedtestportionin9.4.1by10mlofwater(seeA.2).Ifthevalueobtainedintheblanktestregularlyexceeds1,0mg,checkthereagentsifthishasnotbeenrecentlydone(9.2.2).Correctionsofmorethan2,5mgshouldbementionedinthetestreport.9.2.2BlanktestforreagentsTotestthequalityofthereagents,carryoutablanktestasspecifiedin9.2.1.Additionallyuseanemptyfat-collectingvessel,preparedasspecifiedin9.3,formasscontrolpurposes.Thereagentsshallleavenoresiduegreaterthan1,0mg(seeA.1).Iftheresidueofthecompletereagentblanktestisgreaterthan1,0mg,determinetheresidueofthesolventsseparatelybydistilling100mlofthediethylether(5.4)andlightpetroleum(5.5),respectively.Useanemptyfat-collectingvessel,preparedforcontrolpurposesasdescribedabove,toobtaintherealmassofresiduewhichshallnotexceed1,0mg.Veryoccasionally,thesolventsmaycontainvolatilematterwhichisstronglyretainedinfat.Ifthereareindicationsofthepresenceofsuchsubstances,carryoutblanktestsonallthereagentsandforeachsolventusingafat-collectingvesselwithabout1gofanhydrousbutterfat.Ifnecessary,redistilsolventsinthepresenceof1gofanhydrousbutterfatper100mlofsolvent.Usethesolventsonlyshortlyaftertheredistillation.Replaceunsatisfactoryreagentsandsolvents,orredistilsolvents.9.3Preparationoffat-collectingvesselDryafat-collectingvessel(6.9)withafewboilingaids(6.10)intheoven(6.4)setat102°Cfor1h.NOTE1Boilingaidsaredesirabletopromotegentleboilingduringthesubsequentremovalofsolvents,especiallywhenusingglassfat-collectingvessels;theiruseisoptionalwithmetaldishes.SIST EN ISO 1736:2001



ISO1736:2000(E)©ISO2000–Allrightsreserved5Protectthefat-collectingvesselfromdustandallowittocooltothetemperatureoftheweighingroom(glassfat-collectingvesselforatleast1h;metaldishforatleast30min).NOTE2Toavoidinsufficientcoolingorundulylongcoolingtimes,thefat-collectingvesselshouldnotbeplacedinadesiccator.Usetongs(6.13)toplacethefat-collectingvesselonthebalance.Weighthefat-collectingvesseltothenearest1,0mg.NOTE3Tongsshouldpreferablybeusedtoavoid,inparticular,temperaturevariations.9.4Determination9.4.1Carryoutthedeterminationwithoutdelay.Addabout10mlofpreheatedwatera
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