Designation:D95−13´1ManualofPetroleumMeasurementStandards(MPMS),Chapter10.5
StandardTestMethodfor
WaterinPetroleumProductsandBituminousMaterialsbyDistillation1ThisstandardisissuedunderthefixeddesignationD95;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval.
ThisstandardhasbeenapprovedforusebyagenciesoftheU.S.DepartmentofDefense.
ε1NOTE—IPinformationwasremovededitoriallyinSeptember2013.
1.Scope*
1.1Thistestmethodcoversthedeterminationofwaterintherangefrom0to25%volumeinpetroleumproducts,tars,andotherbituminousmaterialsbythedistillationmethod.
NOTE1—Volatilewater-solublematerial,ifpresent,maybemeasuredaswater.
1.2Thespecificproductsconsideredduringthedevelop-mentofthistestmethodarelistedinTable1.ForbituminousemulsionsrefertoTestMethodD244.Forcrudeoils,refertoTestMethodD4006(APIMPMSChapter10.2).
NOTE2—Withsometypesofoil,satisfactoryresultsmaybeobtainedfromTestMethodD1796(APIMPMSChapter10.6).
1.3ThevaluesstatedinSIunitsaretoberegardedasthestandard.Thevaluesinparenthesesareforinformationonly.1.4Thisstandarddoesnotpurporttoaddressallofthesafetyconcerns,ifany,associatedwithitsuse.Itistheresponsibilityoftheuserofthisstandardtoestablishappro-priatesafetyandhealthpracticesanddeterminetheapplica-bilityofregulatorylimitationspriortouse.Forspecifichazardstatements,seeSection6.2.ReferencedDocuments
2.1ASTMStandards:2D235SpecificationforMineralSpirits(PetroleumSpirits)(HydrocarbonDryCleaningSolvent)
ThistestmethodisunderthejurisdictionofASTMCommitteeD02onPetroleumProducts,LiquidFuels,andLubricantsandtheAPICommitteeonPetroleumMeasurement,andisthedirectresponsibilityofSubcommitteeD02.02/COMQ,thejointASTM-APICommitteeonHydrocarbonMeasurementforCustodyTransfer(JointASTM-API).
CurrenteditionapprovedMay1,2013.PublishedJuly2013.Originallyapprovedin1921.Lastpreviouseditionapprovedin2010asD95–05(2010).DOI:10.1520/D0095-13E01.2ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.ForAnnualBookofASTMStandardsvolumeinformation,refertothestandard’sDocumentSummarypageontheASTMwebsite.
1D244TestMethodsandPracticesforEmulsifiedAsphaltsD1796TestMethodforWaterandSedimentinFuelOilsbytheCentrifugeMethod(LaboratoryProcedure)(APIMPMSChapter10.6)
D4006TestMethodforWaterinCrudeOilbyDistillation(APIMPMSChapter10.2)
D4057PracticeforManualSamplingofPetroleumandPetroleumProducts(APIMPMSChapter8.1)
D4177PracticeforAutomaticSamplingofPetroleumandPetroleumProducts(APIMPMSChapter8.2)
D5854PracticeforMixingandHandlingofLiquidSamplesofPetroleumandPetroleumProducts(APIMPMSChap-ter8.3)
E123SpecificationforApparatusforDeterminationofWaterbyDistillation2.2APIStandards:3MPMSChapter8.1ManualSamplingofPetroleumandPetroleumProducts(ASTMPracticeD4057)
MPMSChapter8.2AutomaticSamplingofPetroleumandPetroleumProducts(ASTMPracticeD4177)
MPMSChapter8.3MixingandHandlingofLiquidSamplesofPetroleumandPetroleumProducts(ASTMPracticeD5854)
MPMSChapter10.2DeterminationofWaterinCrudeOilbytheDistillationMethod(ASTMTestMethodD4006)MPMSChapter10.6TestMethodforWaterandSedimentinFuelOilsbytheCentrifugeMethod(LaboratoryProce-dure)(ASTMTestMethodD1796)
PublishedasManualofPetroleumMeasurementStandards.AvailablefromAmericanPetroleumInstitute(API),1220L.St.,NW,Washington,DC20005-4070,http://www.api.org..
3*ASummaryofChangessectionappearsattheendofthisstandard
Copyright©ASTMInternational,100BarrHarborDrive,POBoxC700,WestConshohocken,PA19428-2959.UnitedStates
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D95−13´1NOTE4—Itisrecommendedtouseawideboilingrangesolventwith10%boilingbelow100°Ctohelptoensureanevendistillationrate.
3.Terminology
3.1Definitions:
3.1.1bituminousmaterial,n—inpetroleumtechnology,ablackordark-coloredveryviscousliquidorsemi-solidcom-posedprincipallyofhighmolecularweightcondensedaromatic,ornaphtheniccompounds,orboth.4.SummaryofTestMethod
4.1Thematerialtobetestedisheatedunderrefluxwithawater-immisciblesolvent,whichco-distillswiththewaterinthesample.Condensedsolventandwaterarecontinuouslyseparatedinatrap,thewatersettlinginthegraduatedsectionofthetrapandthesolventreturningtothestill.5.SignificanceandUse
5.1Aknowledgeofthewatercontentofpetroleumproductsisimportantintherefining,purchase,sale,andtransferofproducts.
5.2Theamountofwaterasdeterminedbythistestmethod(tothenearest0.05or0.1volume%,dependingonthetrapsizeused)maybeusedtocorrectthevolumeinvolvedinthecustodytransferofpetroleumproductsandbituminousmate-rials.
5.3Theallowableamountofwatermaybespecifiedincontracts.
6.Solvent-CarrierLiquid
6.1Awater-immisciblesolvent-carrierliquidthatismis-cibleinthematerialbeingtested(seeTable1)shallbeused.6.1.1AromaticSolvent—Thefollowingaromaticsolventsareacceptable:
6.1.1.1IndustrialGradeXylene—(Warning—Flammable.Vaporharmful.)
6.1.1.2Ablendof20volume%industrialgradetolueneand80volume%industrialgradexylene.(Warning—Flammable.Vaporharmful.)
6.1.1.3PetroleumNaphthaorCoalTarNaphtha,freeofwater,yieldingnotmorethan5%distillatesat125°C(257°F)andnotlessthan20%at160°C(320°F)andwitharelativedensity(specificgravity)notlowerthan0.8545at15.56/15.56°C(60/60°F).(Warning—Extremelyflammable.Harm-fulifinhaled.Vaporsmaycausefire.)
6.1.2PetroleumDistillateSolvent—Apetroleumdistillatesolventcontainingatleast2%(V/V)aromaticsandwithaninitialboilingpoint(IBP)greaterthan80°C(176°F);andafinalboilingpoint(FBP)below250°C(482°F)shallbeused.
NOTE3—ExamplesofsuitablesolventsincludeTypesIandIVandClassesAandBofSpecificationD235.
TABLE1TypeofSolvent-CarrierLiquidtoUseVersusMaterialto
BeTested
TypeofSolvent-CarrierLiquid
AromaticPetroleumdistillateVolatilespirits
MaterialtobeTested
asphalt,bitumen,tar,andrelatedproductsfueloil,lubricatingoil,lubricatingoiladditives
greases
6.1.3VolatileSpiritsSolvent—Thefollowingvolatilespiritssolventsareacceptable:
6.1.3.1PetroleumSpirit,withaboilingrangefrom100to120°C(212to248°F).(Warning—Flammable.Vaporharm-ful.)
6.1.3.2Iso-octane,of95%purityorbetter.(Warning—Extremelyflammable.Harmfulifinhaled.Vaporsmaycausefire.)
6.2SolventBlank—ThewatercontentofthesolventshallbedeterminedbydistillinganequivalentamountofthesamesolventusedforthetestsampleinthedistillationapparatusandtestingasoutlinedinSection10.TheblankshallbedeterminedtothenearestscaledivisionandusedtocorrectthevolumeofwaterinthetrapinSection11.7.Apparatus
7.1General—Theapparatuscomprisesaglassormetalstill,aheater,arefluxcondenser,andagraduatedglasstrap.Thestill,trap,andcondensermaybeconnectedbyanysuitablemethodthatproducesaleakproofjoint.PreferredconnectionsaregroundjointsforglassandO-ringsformetaltoglass.TypicalassembliesareillustratedinFig.1,Fig.2,andFig.3.Thestillsandtrapsshouldbechosentocovertherangeofmaterialsandwatercontentsexpected.Onassembly,careshallbetakentopreventthejointsfromfreezingorsticking.Alwaysapplyaverythinfilmofstopcockgreasetopreventtheglasswarejointsfromseizing.
7.2Still—Aglassormetalvesselwithashortneckandsuitablejointforaccommodatingtherefluxtubeofthetrapshallbeused.Vesselsof500,1000,and2000-mLnominalcapacityhaveprovedsatisfactory.
7.3Heater—Asuitablegasburnerorelectricheatermaybeusedwiththeglassstill.Agasringburnerwithportsontheinsidecircumferenceshallbeusedwiththemetalstill.Thegasringburnershallbeofsuchdimensionsthatitmaybemoved
FIG.1TypicalAssemblywithGlassStill
2
D95−13´1ogy(NIST)4traceableequipment.Verificationshallbewithatraceable5mLMicroBuretteorMicroPipette,readabletothenearest0.01mL.
9.1.1InstylesA,B,C,andD,asspecifiedinTable2(Table1inSpecificationE123),eachsubdivision(thatis,0.1mLthrough1.0mL)intheconicalportionofthetubeshallbeverified.Thereafter,eachmajorsubdivision(thatis,2.0mL,3.0mL,4.0mL,anduptothetotalvolumeofthetrap)shallbeverified.
9.1.2InstylesEandF,asspecifiedinTable2,eachmajorsubdivision(0.1mL,1.0mL,2.0mL,4.0mL,and5.0mLinthecaseofStyleE;0.05mL,0.5mL,1.0mL,1.5mL,and2.0mLinthecaseofStyleF)shallbeverified.
9.2Theentireglasswareassemblyshallbeverifiedpriortofirstuseandataregularfrequencythereafterasfollows.9.2.1Put400mLofdry(0.02%watermaximum)xyleneorthesolventtobeutilizedintheanalysisofunknownsamplesintotheapparatusandtestinaccordancewithSection10.Whencomplete,discardthecontentsofthetrapandaddthevolumeofwaterasspecifiedasfirsttestinTable3directlytothedistillationflaskandtestinaccordancewithSection10.9.2.2Repeatthetestin9.2.1,andaddthevolumespecifiedassecondtestinTable3directlytotheflask.TheassemblyoftheapparatusissatisfactoryonlyifthetrapreadingsarewithinthetolerancesspecifiedinTable3.
9.3Areadingoutsidethepermissiblelimitssuggestsamalfunctionresultingfromvaporleaks,toorapidboiling,inaccuraciesincalibrationofthetrap,oringressofextraneousmoisture.Eliminatethesefactorsbeforerepeatingtheverifica-tion.
10.Procedure
NOTE6—Theprecisionofthistestmethodwillbeaffectedbywaterdropletsadheringtosurfacesintheapparatusandthereforenotsettlingintothewatertraptobemeasured.Tominimizetheproblem,allapparatusmustbecleanedchemicallyatleastdailytoremovesurfacefilmsanddebris,whichhinderfreedrainageofwaterinthetestapparatus.Morefrequentcleaningisrecommendedifthenatureofsamplesbeingruncausespersistentcontamination.
FIG.2Two-millilitreReceiverShowingAlternativeConnectionsto
GlassStill
upanddownthevesselwhentestingmaterialsthatarelikelytofoamorsolidifyinthestill.
7.4Glassware—DimensionsanddescriptionsoftypicalglasswareforuseinthistestmethodareprovidedinSpecifi-cationE123.
NOTE5—Insteadofstandardizingonaparticularapparatusspecifica-tionwithrespecttodimensionsandstyle,agivenapparatuswillbedeemedsatisfactorywhenaccurateresultsareobtainedbythestandardadditiontechniquedescribedinSection9.
8.Sampling
8.1Samplingisdefinedasallstepsrequiredtoobtainanaliquotofthecontentsofanypipe,tank,orothersystemandtoplacethesampleintothelaboratorytestcontainer.OnlyrepresentativesamplesobtainedasspecifiedinPracticesD4057(APIMPMSChapter8.1)andD4177(APIMPMSChapter8.2)shallbeusedforthistestmethod.
8.2Thesizeofthetestportionshouldbebasedontheexpectedwatercontentofthesample,suchthatthewateryielddoesnotexceedthecapacityofthetrap(unlessatrapwithastopcockisusedpermittingexcesswatertobewithdrawnintoagraduatedcylinder).
8.3PracticeD5854(APIMPMSChapter8.3)containsinformationonsamplingandhomogenizationefficiencyofunknownmixers.ThistestmethodshouldnotbefollowedwithoutstrictadherencetoPracticeD5854(APIMPMSChapter8.3).9.Verification
9.1Theaccuracyofthegraduationmarksonthetrapshallbecertifiedorverified,usingonlynationalorinternationalstandards,suchasNationalInstituteofStandardsandTechnol-3
10.1Measureasuitableamountofsampletoanaccuracyof61%andtransferittothestill.
10.2Measureordinaryliquidsamplesinagraduatedcylin-derofanappropriatesize.Rinsethematerialadheringtothecylinderwithone50-mLandtwo25-mLportionsofthesolvent-carrierliquid(seeSection6andTable1).Drainthecylinderthoroughlyafterthesampletransferandeachrinsing.10.3Weighsolidorviscousmaterialsdirectlyintothestillandadd100mLoftheselectedsolvent-carrierliquid.Incasesofmaterialwithalow-watercontentwhenlargesamplesmustbeused,asolvent-carrierliquidvolumeinexcessof100mLmaybenecessary.
10.4Glassbeadsorotherboilingaidsmaybeadded,ifnecessary,toreducebumping.
10.5Assemblethecomponentsoftheapparatus,asillus-tratedinFig.1,Fig.2,andFig.3,choosingthetrapin
NationalInstituteofStandardsandTechnology(NIST),100BureauDr.,Stop1070,Gaithersburg,MD20899-1070,http://www.nist.gov.
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D95−13´1NOTE1—Trapshallbe15to16mmininsidediameter.
FIG.3TypicalAssemblieswithMetalStill
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D95−13´1TABLE2SpecificationsandSizesofTraps
Description
SmallestScaleDivision,mL0.10.20.10.20.20.10.050.10.05
StyleABCDE
TopofGraduatedTubeSTJointSTSTSTST
JointJointJointJoint
BottomofGraduatedTubeConicalConicalConicalConicalRound
BottomofVaporTubeSTJointSTJointPlainPlainSTJoint
SizeofTrap
mL
1025252555102
RangemL0to1.0>1.0to10.00to1.0>1.0to251.0to250to5.00to5.00to10.00to2.0
ScaleErrorMaximum,
mL0.050.10.050.10.10.050.0250.10.025
FSTJointRoundSTJoint
TABLE3PermissibleLimitsinMillilitres
CapacityofReceiverat20°CRoundtrap
225(0.05mLsubdivisions)5(0.05mLsubdivisions)5(0.1mLsubdivisions)5(0.1mLsubdivisions)
1010Conicaltrap
1010
2525
VolumeofWaterAddedtoFlaskat
20°C
11.914.5
PermissibleLimitsforRecoveredWaterat
20°C
1±0.051.9±0.051±0.054.5±0.05
1stTest2ndTest1stTest2ndTest
10.7Whentheevolutionofwateriscomplete,allowthetrapandcontentstocooltoroomtemperature.Dislodgeanydropsofwateradheringtothesidesofthetrapwithaglassorpolytetrafluoroethylene(PTFE)rodorothersuitablemeansandtransferthemtothewaterlayer.Readthevolumeofthewaterinthetraptothenearestscaledivision.
10.8Asolventblankshallbeestablished,asoutlinedin6.2.11.Calculation
11.1Calculatethewaterinthesample,asweightorvolumepercent,inaccordancewiththebasisonwhichthesamplewastaken,asfollows:
11.1.1Water,%(V/V)=
1stTest2ndTest
14.5
1±0.14.5±0.1
1stTest2ndTest595±0.19±0.1
~Volumeinwatertrap,mL!2~Waterinsolventblank,mL!Volumeintestsample,mL3100
(1)
1stTest2ndTest1stTest2ndTest
191224
1±0.19±0.212±0.224±0.2
11.1.2Water,%(V/m)=
~Volumeofwaterintrap,mL!2~Waterinsolventblank,mL!Massoftestsample,g3100
(2)
12.Report
accordancewiththeexpectedwatercontentofthesampleandmakingallconnectionsvaporandliquidtight.Ifametalstillwitharemovablecoverisused,insertagasketofheavypaper,moistenedwithsolvent,betweenthestillbodyandthecover.Thecondensertubeandtrapmustbechemicallycleantoensurefreedrainageofwaterintothebottomofthetrap.Insertaloosecottonpluginthetopofthecondensertopreventcondensationofatmosphericmoistureinsideit.Circulatecoldwaterthroughthejacketofthecondenser.
10.6Applyheattothestill,adjustingtherateofboilingsothatcondenseddistillatedischargesfromthecondenserattherateoftwotofivedropspersecond.Ifthemetalstillisused,startheatingwiththeringburnerabout76mm(3in.)abovethebottomofthestillandgraduallylowertheburnerasthedistillationproceeds.Continuedistillationuntilnowaterisvisibleinanypartoftheapparatusexceptinthetrapandthevolumeofwaterinthetrapremainsconstantfor5min.Ifthereisapersistentringofwaterinthecondensertube,carefullyincreasetherateofdistillationorcutoffthecondenserwaterforafewminutes.
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12.1Reporttheresultsasthewatercontenttothenearest0.05%ifthe2-mLreceiverhasbeenusedandtothenearest0.1%ifthe10-mLor25-mLreceiverhasbeenusedandtothenearestsubdivisionifa5-mLreceiverhasbeenusedwitha100-mLor100-gsample.13.PrecisionandBias
13.1Precision—Thecriteriadescribedin13.1.1and13.1.2shouldbeusedtojudgetheacceptabilityofresultswhenusingthe10or25-mLtraps.Theprecisionwhenusingthe2-mLtrapora5–mLtraphasnotbeenestablished.
NOTE7—PracticeD6300wasnotusedinobtainingprecisiondata.
13.1.1Repeatability—Thedifferencebetweensuccessivetestresults,obtainedbythesameoperatorwiththesameapparatusunderconstantoperatingconditionsonidenticaltestmaterial,would,inthelongrun,inthenormalandcorrectoperationofthetestmethod,exceedthevaluesinTable4inonlyonecaseintwenty.
TABLE4Precision
TypeRepeatability
WaterCollected,
mL
0.0–1.01.1–25
Difference,mL
0.1
0.1mLor2%ofthemean,whicheverisgreater
0.2
0.2mLor10%ofthemean,whicheverisgreater
D95−13´1would,inthelongrun,inthenormalandcorrectoperationofthetestmethod,exceedthevaluesinTable4inonlyonecaseintwenty.
13.2Bias—Asthereisnoacceptedreferencematerialsuit-ablefordeterminingbiasfortheproceduredescribedinthistestmethodformeasuringwaterinpetroleumproductsandbituminousmaterialsbydistillation,nostatementaboutbiasismade.14.Keywords
14.1bituminousmaterials;distillation;petroleumproducts;solventcarrierliquid;waterbydistillation;watercontent
Reproducibility
0.0–1.01.1–25
13.1.2Reproducibility—Thedifferencebetweentwosingleandindependenttestresultsobtainedbydifferentoperatorsworkingindifferentlaboratoriesonidenticaltestmaterial,
SUMMARYOFCHANGES
SubcommitteeD02.02hasidentifiedthelocationofselectedchangestothisstandardsincethelastissue(D95–05(2010))thatmayimpacttheuseofthisstandard.
(1)AddedSpecificationD235tosubsection2.1.(2)Updated6.1,6.1.2,andTable1.
(3)AddedNote3andNote4.
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