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ASME BPVC.

V-2017 ARTICLE 24,SE-165/SE-165M

STANDARD PRACTICEFOR LIQUIDPENETRANT


EXAMINATIONFOR GENERAL INDUSTRY

SE-165/SE-165M

(Identicalwith ASTM SpecificationE165/E165M-12.)

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ARTICLE 24,SE-165/SE-165M ASME BPVC.V-2017

Standard Practicefor
LiquidPenetrantExamination forGeneral Industry

1. Scope therefore,eachsystemshallbe usedindependentlyoftheothe


Combining valuesfrom the two systemsmay resultin non
1 .1 Thispracticecoversproceduresforpenetrantexamina-tionof
conformance withthestandard.
materialsPenetranttestingisa. nondestructivetesting method
fordetectingdiscontinuitiesthatareopentothesurface 1 .5 This standard does not purport to address all of the safety
suchascracks,seams,laps,coldshuts,shrinkage,laminations, concerns,if any, associatedwith its use. It is the responsibilityof the
throughleaks,or lackoffusionand isapplicabletoin-process, final,and user ofthisstandardto establishappro-priatesafetyand
maintenancetestingItcan. be effectivelyusedinthe examinationof healthpracticesand determinethe applica
nonporous,metallicmaterials,ferrousand nonferrousmetals,and of bilityofregulatorylimitationspriorto use.
nonmetallicmaterialssuchas non-porous glazedor
fullydensifiedceramics,as wellas certain nonporousplastics,and 2. Referenced Documents
glass. 2. 1 ASTM Standards:
1 .2 Thispracticealsoprovidesa reference: D129 Test Method forSulfurin PetroleumProducts(Gen-
1 .2.1By which a liquidpenetrantexaminationprocess eralHigh PressureDecompositionDeviceMethod)
recommended or requiredby individualorganizationscan be E516 Practicefor TestingThermal ConductivityDetecto Used
reviewedtoascertainitsapplicabilityand completeness. inGas Chromatography
1 .2.2Foruseinthepreparationofprocessspecificationsand D808 TestMethod forChlorineinNew and Used Petroleu
proceduresdealingwiththe liquidpenetrantestingof parts and Products(High PressureDecompositionDeviceMethod)
materialsAgreement. by thecustomerrequestingpenetrant D1193 SpecificationforReagentWater
inspectionisstronglyrecommended. Allareasof thispractice may be D1552 TestMethod forSulfurinPetroleumProducts(High
open toagreementbetween thecognizantengineering TemperatureMethod)
organizationand the supplier,or specificdirectionfrom the D4327 TestMethod forAnions inWater by SuppressedIon
cognizantengineeringorganization. Chromatography
1 .2.3For usein theorganizationof facilitiesand personnel E433 ReferencePhotographsfor Liquid PenetrantInspec tion
concernedwithliquidpenetrantesting.
E543 SpecificationforAgenciesPerformingNondestructi
1 .3 This practicedoes not indicateor suggestcriteriafor
Testing
evaluationof theindicationsobtainedby penetrantestingIt. shouldbe
pointedout,however,thatafterindicationshave been found,they E1208 Practicefor FluorescentLiquid PenetrantTestin Using
theLipophilicPost-EmulsificationProcess
must be interpretedor classifiedand then evaluated.For
thispurpose theremust be a separatecode, standard,or a E1209 Practicefor FluorescentLiquid PenetrantTestin Using
theWater-WashableProcess
specificagreement to define the type,size, location,and directionof
indicationsconsideredacceptable, and E1210 Practicefor FluorescentLiquid PenetrantTestin Using
thoseconsideredunacceptable. theHydrophilicPost-EmulsificationProcess
E1219 Practicefor FluorescentLiquid PenetrantTestin Using
1 .4 Units— The values statedin eitherSI unitsor inch-pound theSolvent-RemovableProcess
unitsare to be regardedseparatelyas standard.The valuesstatedin E1220 PracticeforVisiblePenetrantTestingUsing Solvent
each system may not be exactequivalents; Removable Process
E1316TerminologyforNondestructiveExaminations
E1417 PracticeforLiquidPenetrantTesting

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ASME BPVC.V-2017 ARTICLE 24,SE-165/SE-165M

E1 41 8Practicefor VisiblePenetrantTestingUsing the 5. Significanceand Use


Water-WashableProcess 5.1Liquidpenetrantestingmethodsindicatethepresenc
E2297 GuideforUse ofUV-A andVisibleLightSourcesand locationand,toa limitedextent,thenatureand magnitudeof
MetersusedintheLiquidPenetrantand MagneticParticle the detecteddiscontinuitiesEach. of the variouspenetra
Methods methods has been designedforspecificusessuch as criti
2.2ASNT Document: serviceitems,volume ofparts,portabilitylocalizedareasof
SNT-TC-1A Recommended Practicefor Nondestructive examinationThe. method selectedwilldepend accordinglyon
TestingPersonnelQualificationand Certification thedesignand servicerequirementsofthepartsor materia
ANSI/ASNT CP-189StandardforQualificationand Certifi- beingtested.
cationofNondestructiveT stingPersonnel
2.3MilitaryStandard: 6. Classificationof PenetrantMaterialsand Methods
MIL-STD-410 NondestructiveT stingPersonnelQualifica- 6.1Liquidpenetrantexaminationmethods and typesare
tionand Certification classifiedin accordancewithMIL-I-25135and AMS 2644 as
2.4APHA Standard: listedin Table1 .
429Method fortheExaminationofWater and Wastewater
6.2FluorescentPenetrantTesting(Type 1)—Fluoresce
2.5AIA Standard:
NAS-410 Certificationand Qualificationof Nondestructive penetrantestingutilizespenetrantsthatfluorescebrillian
TestPersonnel when excitedby blacklight(UVA). The sensitivityoffluores
centpenetrantsdependson theirabilityto be retainedin th
2.6SAE Standards:
varioussizediscontinuitiesduringprocessing,and then to
AMS 2644InspectionMaterial,Penetrant
bleedout intothedevelopercoatingand produceindicatio
QPL-AMS-2644 QualifiedProductsofInspectionMaterials, thatwillfluoresce.Fluorescentindicationsare many time
Penetrant brighterthantheirsurroundingswhen viewed underappropr
3. Terminology ateblacklightillumination.
6.3VisiblePenetrantTesting(Type 2)— Visiblepenetra
3.1The definitionsrelatingtoliquidpenetrantexamination, testingusesa penetranthatcan be seenin visiblelightThe.
which appearinTerminologyE1316,shallapplyto theterms
usedin thispractice. penetrantisusuallyred,sothatresultantindicationsproducea
definitecontrastwiththewhitebackgroundofthedevelope
4. Summary of Practice Visiblepenetrantindicationsmust be viewed underadequat
4.1Liquidpenetrantmay consistof visibleor fluorescent whitelight.
material.The liquidpenetrantis appliedevenly over the
surfacebeingexaminedand allowedtoenteropendiscontinui- 7. Materials
tiesAftera. suitabledwelltime,theexcesssurfacepenetrantis 7.1LiquidPenetrantTestingMaterialsconsistof fluores
removed.A developerisappliedto draw the entrappedpen- cent or visiblepenetrants,emulsifiers(oil-baseand water
etrantoutofthediscontinuityand stainthedeveloperThe. test base),removers (waterand solvent),and developers(dr
surfaceisthenexaminedtodeterminethepresenceorabsence powder,aqueousandnonaqueous)A. familyofliquidpenetra
ofindications. examinationmaterialsconsistsoftheapplicablepenetrantand
emulsifier,as recommended by themanufacturerAny. liqui
N OTE 1 —The developermay be omittedby agreementbetween the penetrant,removerand developerlistedin QPL-25135/QPL-
contractingparties.
N OTE 2—Fluorescentpenetrantexaminationshallnotfollowa visible AMS2644 can be used,regardlessofthemanufacturerInte.
penetrantexaminationunlesstheprocedurehasbeen qualifiedinaccor- mixingofpenetrantsand emulsifiersfrom differentmanufac
dance with 10.2,because visibledyes may cause deterioration turersisprohibited.
quenchingoffluorescentdyes.
N OTE 3—Refer to9.1forspecialrequirementsforsulfur,halogenand
4.2Processingparameters,such as surfaceprecleaning, alkalimetalcontent.
penetrantdwelltimeand excesspenetrantremovalmethods, N OTE 4—While approvedpenetrantmaterialswillnotadverselyaffec
aredependenton thespecificmaterialsused,thenatureofthe common metallicmaterials,some plasticsorrubbersmay be swollenor
partunderexamination,(thatis,size,shape,surfacecondition, stainedby certainpenetrants.
alloy)and typeofdiscontinuitiesexpected. 7.2Penetrants:

TABLE 1 Classificationof PenetrantExaminationTypes and


Methods
Type I—FluorescentPenetrantExamination
Method A—Water-washable (seeTest Method E1 209)
Method B—Post-emulsifiable,lipophilic(seeTest Method E1 208)
Method C—Solvent removable(seeTestMethod E1 219)
Method D—Post-emulsifiable,hydrophilic(seeTestMethod E1 210)
Type II—VisiblePenetrantExamination
Method A—Water-washable (seeTest Method E1 41 8)
Method C—Solvent removable(seeTestMethod E1 220)

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7. 2.1Post-EmulsifiablePenetrantsare insolublein water and 7. 5.1Dry Powder Developers—Dry powder developersare


cannot be removed with water rinsingalone.They are used assupplied,thatis,free-flowing,non-cakingpowder (se
formulatedto be selectivelyremoved from thesurfaceusinga 8. 8.1)Care. shouldbe takennotto contaminatethedevelope with
separateemulsifier.Properly applied and given a proper fluorescentpenetrant,as the contaminateddevelope speckscan
emulsificationtime,the emulsifiercombines with the excess appearas penetrantindications.
surfacepenetrantoform a water-washablemixture,which can be 7. 5.2AqueousDevelopers—Aqueous developersare nor mally
rinsedfrom thesurface,leavingthesurfacefreeofexcessive suppliedasdry powder particlestobe eithersuspende
fluorescentbackground.Properemulsificationtime must be (watersuspendable)or dissolved(watersoluble)inwater.The
experimentallyestablishedand maintained to ensure that over- concentration,useand maintenanceshallbe inaccordancewith
emulsificationdoes not resultinlossof indications. manufacturer’srecommendations.Water solubledeveloper
7. 2.2Water-WashablePenetrantsare formulatedto be di- shallnotbe used withType 2 penetrantsor Type 1,Method A
rectlywater-washablefrom the surfaceof thetestpart,aftera penetrants.
suitablepenetrantdwelltime.Becausethe emulsifieris“built-
N OTE 5—Aqueous developersmay causestrippingof indicationsifnot
in,”water-washablepenetrantscan be washed outof disconti- properlyappliedand controlledThe. procedureshould be qualifiedin
nuitiesifthe rinsingstep istoo long or too vigorous.It is accordancewith 10.2.
thereforextremelyimportanttoexercisepropercontrolinthe removal
of excesssurfacepenetrantto ensureagainstover-washing.Some 7. 5.3NonaqueousWet Developers—Nonaqueous wet devel
penetrantsare lessresistantto overwashing than others,so opersare suppliedas suspensionsof developerparticlesin a
cautionshouldbe exercised. nonaqueous solventcarrierready for use as supplie
Nonaqueous, wet developersare sprayed on to form a thi
7. 2.3Solvent-RemovableP netrantsare formulatedso that
coatingon thesurfaceofthepartwhen dried.Thisthincoatin
excesssurfacepenetrantcan be removed by wipinguntilmost of
servesas the developingmedium.
the penetranthas been removed. The remaining traces shouldbe
removed with the solventremover (see8.6.4)To. preventremoval N OTE 6—This type of developerisintendedforapplicationby spray only.
of penetrantfrom discontinuities,careshould be taken to avoid the
use of excesssolvent.Flushingthe surfacewith solventtoremove
7. 5.4LiquidFilm Developersare solutionsor colloid
theexcesspenetrantisprohib-itedas
suspensionsof resins/polymerin a suitablecarrier.These
thepenetrantindicationscouldeasilybe washed away. developerswillform a transparentortranslucentcoatingon the
7. 3 Emulsifiers: surfaceof the part.Certaintypes of film developermay be
7. 3.1LipophilicEmulsifiersareoil-miscibliquidsusede to strippedfrom the partand retainedfor recordpurposes(se
emulsifythe post-emulsifiedpenetranton the surfaceof the 8. 8.4).
part,renderingitwater-washableThe. individualcharacteris-ticsof
theemulsifierand penetrant,and the geometry/surface roughnessof 8. Procedure
the partmaterialcontributeto determiningthe emulsificationtime.
8.1 The following processingparameters apply to both
fluorescentand visiblepenetrantestingmethods.
7. 3.2HydrophilicEmulsifiersare water-miscibleliquids used to
emulsifythe excesspost-emulsifiedpenetranton the surfaceof 8. 2 TemperatureLimits—The temperatureof the penetran
thepart,renderingitwater-washableThese. water-base materialsand the surfaceof the partto be processedshallbe
emulsifiers(detergent-typeremovers) are suppliedas between 40°and 125°F[4°and 52°C]ortheproceduremust be
concentratestobe dilutedwithwaterand usedasa dip orspray. The qualifiedatthe temperatureused as describedin10.2.
concentration,useand maintenanceshallbe inaccordance with
8. 3 ExaminationSequence—Final penetrantexaminatio
manufacturer’srecommendations.
shallbe performed afterthe completionof alloperationstha could
7. 3.2.1Hydrophilicemulsifiersfunctionby displacingthe
cause surface-connectediscontinuitiesor operation thatcould
excesspenetrantfilm from the surfaceof the partthrough
expose discontinuitiesnot previouslyopen to the surface.Such
detergentactionThe. forceofthewatersprayorair/mechanical
operationsinclude,but are not limitedto
agitationin an open dip tank providesthe scrubbingaction
grinding,welding,straightening,machining,and heattreatin
whilethedetergentdisplacesthefilm ofpenetrantfrom thepart
Satisfactoryinspectionresultscan usuallybe obtainedon
surface.The individualcharacteristicsof the emulsifierand
surfacesin the as-welded,as-rolled,as-cast,as-forged,or
penetrant,and the geometry and surfaceroughnessof thepart
ceramicsinthe densifiedcondition.
materialcontributeto determiningthe emulsificationtime.
Emulsificationconcentrationshallbe monitoredweekly using a 8. 3.1SurfaceTreatment—Finalpenetrantexaminationmay be
suitablerefractometer. performedpriortotreatmentsthatcan smear thesurfacebu not by
themselvescause surfacediscontinuitiesSuch. trea ments
7. 4 SolventRemovers—Solventremovers functionby dis- include,butarenotlimitedto,vaporblasting,deburrin
solvingthe penetrant,making itpossibleto wipe the surface sanding,buffing,sandblasting,orlappingPerformanceoffinal.
cleanand freeof excesspenetrant. penetrantexaminationaftersuch surfacetreatmentsnecess
7. 5 Developers—Developersform a translucentor white tatesthatthepart(s)be etchedtoremove smeared metal from the
absorptivecoatingthataidsin bringingthe penetrantout of surfacepriorto testingunlessotherwiseagreed by the
surfacediscontinuitiesthroughblottingaction,thusincreasing the contractingpartiesNote. thatfinalpenetrantexaminationshal
visibilityof theindications. always precedesurfacepeening.

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N OTE 7—Sand or shotblastingcan closediscontinuitiessoextremecare shouldbe conductedpriorto use.Electrostaticsprayapplic tioncan


should be taken to avoid masking discontinuitiesUnder. certain eliminateexcessliquidbuild-upof penetranton the part,minimize
circumstances,however, gritblastingwith certainair pressuresand/or
mediums may be acceptablewithoutsubsequentetchingwhen agreedby overspray,and minimize the amount of pen-
the contractingparties. etrantenteringhollow-coredpassageswhich might serveas
N OTE 8—Surface preparationof structuralor electronicceramicsfor penetrantreservoirs,causingseverebleedoutproblemsdurin
penetranttestingby grinding,sand blastingand etchingis not recom- examination.Aerosol spraysare convenientlyportableand
mended becauseof thepotentialfordamage. suitableforlocalapplication.
8. 4 PrecleaningThe— successofany penetrantexamination
N OTE 1 0—With sprayapplications,itisimportantthattherebe prope
procedureisgreatlydependentupon the surroundingsurface and
ventilationThis. isgenerallyaccomplishedthroughtheuseof a properl
discontinuitybeing free of any contaminant(solidor liquid)thatmight designedsprayboothand exhaustsystem.
interferewiththepenetrantprocessAllparts. or areasof partstobe
examined must be cleanand dry before the 8. 5.1PenetrantDwell Time— After application,allow ex
penetrantisapplied.Ifonlya sectionof a part,such as a cesspenetranto drainfrom the part(careshouldbe takento
weld,includingthe heataffectedzone isto be examined,all preventpoolsof penetrantfrom forming on the part),whil
contaminantsshallbe removed from the areabeingexamined as allowingfor properpenetrantdwell time (seeTable 2).The
defined by the contractingparties“Clean”. isintendedto mean lengthof time the penetrantmust remain on thepartto allo
thatthesurfacemust be freeofrust,scale,weldingflux, weld properpenetrationshouldbe as recommended by thepenetra
spatter,grease,paint,oilyfilms, dirt,and so forth,that might manufacturer.Table 2,however,providesa guideforselecti of
interferewith the penetrantprocess.All of thesecon- penetrantdwelltimesfora varietyof materials,forms,and typesof
taminantscanpreventthepenetrantfrom enteringdiscontinui- discontinuitiesUnlessotherwisespecified,the. dwel
ties(seeAnnex on Cleaningof Partsand Materials). time shallnot exceed the maximum recommended by the
manufacturer.
8. 4.1DryingafterCleaning—Itisessentialthatthe surface of
partsbe thoroughlydry aftercleaning,sinceany liquid 8. 6 PenetrantRemoval
residuewillhinderthe entranceof the penetrantDrying. may be 8. 6.1Water Washable (MethodA):
accomplishedby warming the partsin dryingovens,with
8. 6.1 .Removal1 of Water Washable Penetrant—After the
infraredlamps,forcedhotair,orexposuretoambienttempera-ture.
requiredpenetrantdwell time,the excess penetranton the
surfacebeingexamined must be removed withwater.Itcan be
N OTE 9—Residues from cleaningprocessessuch as strongalkalies, removed manually with a coarsespray or wiping the par
picklingsolutionsand chromates,inparticular,may adverselyreactwith the surfacewith a dampened rag, automaticor semi-automat water-
penetrantand reduceitssensitivityand performance.
sprayequipment,orby waterimmersion.Forimmersion
8.5 PenetrantApplicationAftertheparthas— been cleaned, rinsing,partsare completelyimmersed in the waterbathwith airor
dried,and is within the specified temperaturerange,the mechanicalagitation.
penetrantisappliedto the surfaceto be examined so thatthe (a)The temperatureofthewatershallbe maintainedwithi the
entirepartor area under examinationiscompletelycovered rangeof 50° to 100°F [10°to38°C].
withpenetrantApplicationmethods. includedipping,brushing, (b)Spray-rinsewaterpressureshallnotexceed40 psi[275
flooding,or spraying.Small partsare quiteoftenplaced in kPa].When hydro-airpressurespray guns are used,the ai
suitablebasketsand dippedintoa tank ofpenetrantOn. larger pressureshouldnotexceed 25 psi[172kPa].
parts,and thosewith complex geometries,penetrantcan be
appliedeffectivelyby brushingorsprayingBoth. conventional and N OTE 11 —Overwashing should be avoided.Excessivewashing can
cause penetrantto be washed out of discontinuitiesWith. fluorescen
electrostaticspray guns are effectivemeans of applying penetrantmethods performthemanual rinsingoperationunder blackligh
liquidpenetrantsto thepartsurfacesNot. allpenetrantmate-rialsare so that it can be determined when the surfacepenetranthas been
suitablefor electrostaticspray applicationso, tests adequatelyremoved.

TABLE 2 Recommended Minimum DwellTimes


Type of Dwell TimesA (minutes)
Material Form Discontinuity Penetrant Developer
B C

Aluminum, magnesium, steel, castingsand welds cold shuts,porosity,lackoffusion, 5 10


brass cracks (allforms)
and bronze,titaniumand
high-temperaturealloys
wrought materials—extrusions, laps,cracks (allforms) 10 10
forgings,plate
Carbide-tippedtools lackof fusion,porosity,cracks 5 10
Plastic allforms cracks 5 10
Glass allforms cracks 5 10
Ceramic allforms cracks, porosity 5 10
A
For temperature range from 50° to 1 25°F [10° to 52°C].For temperaturesbetween 40° and 50°F [4.4°and 10°C],recommend a minimum dwelltime of20 minutes.
B
Maximum penetrantdwelltime inaccordance with8.5..1
C
Development time beginsas soon as wet developercoatinghas driedon surfaceof parts(recommended minimum). Maximum development time inaccordance with
8.8.5.

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8. 6.1 .2Removalby Wiping(MethodC)— After therequired penetrantcontamination in the hydrophilicemulsifier bath


penetrant dwell time, the excess penetrantis removed by wiping therebyextendingitslife.Itisnot necessaryto prerinsea par ifa
with a dry,clean,lint-freecloth/towelThen. use a clean lint- spray applicationof emulsifieris used.
freecloth/towellightlymoistened with water or solventto remove 8. 6.3.2PrerinsingControls—Effectiveprerinsingisaccom-
theremaining tracesof surfacepenetrantas determined by plishedby manual, semi-automated,or automated water spray
examinationunder black lightfor fluorescentmethods and rinsingof thepart(s)The. water spraypressureshallnotexceed 40
visiblelightfor visiblemethods. psi[275kPa] when manual or hydro airsprayguns are used
8. 6.2LipophilicEmulsification(MethodB): When hydro-airpressurespray guns are used,theairpressur
8. 6.2.1ApplicationofLipophilicEmulsifier—After the re-quired shallnot exceed 25 psi[172kPa].Water freeof contaminants
penetrantdwell time, the excesspenetranton the part must be thatcould clogspray nozzlesor leavea residueon the part(s
emulsified by immersing or flooding thepartswith the isrecommended.
requiredemulsifier (the emulsifier combines with the excess 8. 6.3.3ApplicatiofEmulsifiern—The residualsurfacepen-
surfacepenetrantand makes the mixture removable by water etranton part(s)must be emulsified by immersing thepart(s)in
rinsing)Lipophilicemulsifiershallnot. be appliedby sprayor brush an agitatedhydrophilicemulsifier bath or by spraying the
and the part or emulsifier shallnot be agitatedwhile being part(s)with water/emulsifiersolutionsthereby renderingthe
immersed. After applicationof the emulsifier,the parts shallbe remaining residualsurface penetrantwater-washable for the
drained and positionedin a manner thatpreventsthe final rinsestationThe. emulsificationtimebeginsas soon as the
emulsifierfrom poolingon the part(s). emulsifierisapplied.The lengthof time thattheemulsifieris
8. 6.2.2EmulsificationTime— The emulsificationtime be-ginsas allowed to remain on a partand in contactwith the penetran is
soon as theemulsifierisapplied.The lengthof time that dependent on the type of emulsifier employed and the
theemulsifierisallowedto remain on a partand incontactwith surfaceroughness.The emulsificationtime should be deter
thepenetrantisdependent on the type of emulsifieremployed and mined experimentallyfor each specificapplicationThe. sur face
thesurfaceroughness.Nominal emulsificationtime should finish (roughness of the part is a significantfactorin
be as recommended by the manufacturer.The actualemulsifi- determiningthe emulsificationtime necessaryfor an emulsi fier.
cation time must be determined experimentallyfor each Contact emulsificationtime should be kept to the leas
specificapplicationThe. surfacefinish (roughness)of thepart isa possibletime consistentwith an acceptablebackground and
significantfactorin theselectionof and in the emulsifica-tion time shallnot exceed two minutes.
of an emulsifier.Contact time shallbe kept to the minimum time 8. 6.3.4Immersion—For immersion application,partsshal be
to obtainan acceptablebackground and shall not exceed completely immersed in the emulsifier bath.The hydro-
threeminutes. philicemulsifierconcentrationshallbe as recommended by the
8. 6.2.3PostRinsing—Effectivepostrinsingof the emulsi-fied manufacturerand thebath or partshallbe gentlyagitatedby ai or
penetrantfrom the surface can be accomplished using mechanically throughoutthe cycle.The minimum time to
eithermanual, semi-automated,or automated waterimmersion or obtainan acceptablebackground shallbe used,but the dwell
spray equipment or combinationsthereof. time shallnotbe more thantwo minutes unlessapproved by the
8. 6.2.4Immersion—For immersion post rinsing,parts are contractingparties.
completelyimmersed in the waterbath with airor mechanical 8. 6.3.5SprayApplicationFor— spray applications,allpar
agitationThe. amount of time the partisin the bath shouldbe surfaces should be evenly and uniformly sprayed with a
the minimum requiredto remove the emulsified penetrant.In water/emulsifiersolutionto effectivelyemulsify the residua
addition,the temperaturerange of the water should be 50 to penetranton part surfacesto render it water-washable.The
100°F [10 to 38°C].Any necessarytouch-up rinseafteran concentrationof theemulsifierfor sprayapplicationshouldbe in
immersion rinseshallmeet the requirementsof 8.6.2.5. accordancewith themanufacturer’ srecommendations,but i
8. 6.2.5Spray PostRinsing—Effectivepost rinsingfollow-ing shallnot exceed 5 %. The water spraypressureshouldbe les
emulsificationcan also be accomplished by eithermanual or than 40 psi[275 kpa].Contactwith theemulsifiershallbe kept
automaticwater sprayrinsing.The water temperatureshall be to the minimum time to obtainan acceptablebackground and
between 50 and 100°F [10 and 38°C]. The water spray shallnot exceed two minutes.The water temperatureshallbe
pressureshallnot exceed 40 psi[275 kPa] when manual spray maintainedbetween 50 and 100°F [10 and 38°C].
guns are used.When hydro-airpressurespray guns are used, the 8. 6. 3 . 6Post-Rinsing of Hydrophilic Emulsifie Penetrants—
airpressureshouldnot exceed 25 psi [172kPa]. Effective post-rinsingof emulsified penetran from thesurfacecan
8. 6.2.6RinseEffectivenessIf— the emulsificationand final be accomplished using eithermanual or automated water
rinsestepis not effective,as evidencedby excessiveresidual spray,water immersion, or combination thereof.The
surfacepenetrantafteremulsificationand rinsing;thoroughly totalrinsetime shallnot exceed two minutes regardlessof
recleanand completely reprocessthepart. thenumber of rinsemethods used.
8. 6.3HydrophilicEmulsification(MethodD): 8. 6.3.7ImmersionPost-RinsingIf— an agitatedimmersion
8. 6.3.1Applicatiofn HydrophilicRemover— Followingthe rinseisused,theamount of time the part(s)is(are)in thebath
requiredpenetrantdwell time,thepartsmay be prerinsedwith water shallbe the minimum required to remove the emulsified
priorto the applicationof hydrophilicemulsifier.This prerinseallows penetrantand shallnot exceed two minutes.In addition,the
for the removal of excess surface penetrant from the parts prior temperaturerange of the water shallbe within50 and 100°F [10
to emulsificationso as to minimize and 38°C]. Be aware that a touch-up rinse may be

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necessaryafterimmersion rinse,butthe totalwash time still compressedairnotexceeding5 psi[34 kPa].Dry developer


shallnotexceed two minutes. shallnotbe used with Type IIpenetrant.
8.6.3.8SprayPost-RinsingEffectivepost— -rinsingfollow- 8.8.2AqueousDevelopers(FormsB andC)— Water solubl
ing emulsificationcan also be accomplished by manual, developers(Form B) are prohibitedfor use with Type 2
semi-automatic,or automaticwater spray.The water spray penetrantsor Type 1,Method A penetrantsWater. suspendabl
pressureshallnot exceed 40 psi[275 kPa] when manual or developers(Form C) canbe usedwithboth Type 1 and Type 2
hydro airsprayguns are used.When hydro-airpressurespray penetrantsAqueous. developersshallbe appliedto the par
guns are used,the airpressureshallnot exceed 25 psi[172 immediatelyafterthe excesspenetranthas been removed and
kPa].The watertemperatureshallbe between 50 and 100°F priorto drying.Aqueous developersshallbe preparedand
[10 and 38°C].The spray rinsetime shallbe lessthan two maintainedinaccordancewith themanufacturer’sinstructio
minutes,unlessotherwisespecified. and appliedinsucha manner astoensurecomplete,even,par
8.6.3.9RinseEffectivenessIfthe— emulsificationand final coverage.Aqueous developersmay be appliedby sprayin
rinsestepsarenoteffective,as evidencedby excessiveresidual flowing, or immersing the partin a prepareddeveloperbath
surfacepenetrantafteremulsificationand rinsing,thoroughly Immerse the partsonly long enough to coat allof the par
reclean,and completelyreprocessthe part. surfaceswith thedevelopersinceindicationsmay leachouti
8.6.4Removal of Solvent-RemovableP netrant(Method the partsare leftin the bath too long.After the partsare
C)— Afterthe requiredpenetrantdwelltime,the excesspen- removed from the developerbath,allow the partsto drain
etrantis removed by wiping with a dry, clean,lint-free Drainallexcessdeveloperfrom recessesand trappedsection
cloth/towelThen. use a clean,lint-freecloth/towelightly toeliminatepoolingof developer,which can obscurediscon
moistened with solventremover to remove the remaining tinuitiesDry. the partsin accordancewith 8.7.The drie
tracesof surfacepenetrant.Gentlewiping must be used to developercoatingappearsas a translucentor whitecoatingon
avoidremoving penetrantfrom any discontinuityOn. smooth thepart.
surfaces,an alternatemethod of removal can be done by 8.8.3NonaqueousWet Developers(FormsD and E)— Afte
wiping with a clean,dry cloth.Flushing the surfacewith the excesspenetranthas been removed and the surfacehas
solventfollowingthe applicationof thepenetrantand priorto been dried,apply nonaqueous wet developerby sprayingin
developingisprohibited. sucha manner astoensurecompletepartcoveragewitha thin
8.7 Drying—Regardlessof thetypeand method ofpenetrant even film of developer.The developershallbe appliedin a
used,dryingthe surfaceof the part(s)is necessarypriorto manner appropriateto the type of penetrantbeing used.For
applying dry or nonaqueous developersor followingthe visibledye,the developermust be appliedthicklyenough to
applicationof the aqueous developer.Drying time willvary providea contrastingbackground.For fluorescentdye, the
withthetypeofdryingusedand thesize,nature,geometry,and developermust be appliedthinlyto produce a transluce
number of partsbeingprocessed. coveringDippingorflooding. partswithnonaqueousdevelop
8.7.1DryingParameters—Components shallbe airdriedat room
temperatureor in a dryingoven. Room temperature dryingcanbe
aidedby theuseof fans.Oven temperatureshall not exceed 160°F
[71°C].Drying time shallonly be that necessaryto adequatelydry
the part.Components shallbe removed from the oven
afterdrying.Components shouldnot be placedin the oven with
pooled water or pooled aqueous solutions/suspensions.

ersisprohibited,becausethesolventactionof thesetypesof
developerscan flush or dissolvethepenetrantfrom withinthe
discontinuities.
N OTE 12—The vaporsfrom thevolatilesolventcarrierin thedevelope
may be hazardous.Properventilationshouldbe providedatalltimes,but
especiallywhen thedeveloperisappliedinsidea closedarea.

tappingthe part,or by blowing with low-pressuredry,clean,


8.8 DeveloperApplicationThere— are various modes of
effectiveapplicatiofn thevarioustypesofdeveloperssuchas ersisprohibited,becausethesolventactionof thesetypesof
dusting,immersing,floodingor spraying.The developerform, the
partsize,configuration,and surfaceroughnesswillinflu-ence the
choiceof developerapplication.
8. 8.1Dry PowderDeveloper(Form A)— Dry powder devel-
opersshallbe appliedafterthepartisdry in sucha manner as
toensurecompletecoverageoftheareaofinterestPartscan. be
immersed in a containerof dry developeror in a fluid bed of dry
developer.They can also be dusted with the powder
developerthrougha hand powder bulb or a conventionalor
electrostaticpowder gun. Itiscommon and effectiveto apply
dry powder in an encloseddust chamber, which createsan
effectiveand controlledustcloud.Other means suitedtothe
sizeand geometry of thespecimenmay be used,providedthe
powder isappliedevenlyovertheentiresurfacebeingexam-
ined.Excessdeveloperpowder may be removed by shakingor
8.8.4LiquidFilm Developers—Apply by sprayingas rec maximum permitteddevelopingtimesshallbe fourhours fo dry
ommended by themanufacturer.Spray partsinsucha manner powder developer(Form A), two hours for aqueous
astoensurecompletepartcoverageoftheareabeingexamined with a developer(Forms B and C), and one hour for nonaqueous
thin,even film of developer. developer(Forms D and E).
8. 8.5DevelopingTime— The lengthoftimethedeveloperi 8.9 InspectionAftertheapplicabledevelopmenttime,per—
toremain on thepartpriorto inspectionshallbe notlessthan ten form inspectionofthepartsundervisibleorultravioletlightas
minutes.Developing time beginsimmediatelyafterthe applicationof appropriateItmay. be helpfultoobservethebleedoutdurin
dry powder developeror as soon as the wet (aqueousor thedevelopment time as an aidininterpretingindications.
nonaqueous)developercoatingisdry (thatis,the water or 8. 9.1UltravioletLightExamination—Examine partsteste with
solventcarrierhas evaporatedto dryness).The Type 1 fluorescentpenetrantunder black lightin a

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darkenedarea.Ambient lightshallnot exceed2 fc [21 .5lx]. The processescan bake the developeronto the part.A suitab
measurement shallbe made witha suitablevisiblelight technique,such asa simplewaterrinse,waterspray,machine
sensorattheinspectionsurface. wash,solventsoak,or ultrasoniccleaningmay be employed
(seeAnnex A1 forfurtherinformationon postcleaning)Iti.
N OTE 1 3—Because the fluorescentconstituentsin the penetrantwill
eventuallyfadewithdirectexposureto ultravioletlights,directexposure ofthe
recommended thatifdeveloperemovalisnecessary,itshoul be
partundertestto ultravioletlightshouldbe minimizedwhen not carriedoutaspromptlyaspossibleafterexaminationsotha
removingexcesspenetrantorevaluatingindications. thedeveloperdoes notadhereto thepart.
8.9.1 .BlackLightLevelControl1—Blacklightshallpro-videa 9. SpecialRequirements
minimum lightintensityof1000 µW/cm 2 ,ata distance of 15
9.1Impurities:
in.[38.1cm].The intensityshallbe checked dailyto 9.1 .1When usingpenetrantmaterialson austeniticstainle
ensuretherequiredoutput(seeGuide E2297 formore infor- steels,titanium,nickel-baseor otherhigh-temperaturealloy
mation).Reflectorsand filtershallalsobe checkeddailyfor theneed torestricertainimpuritiessuch as sulfur,halogen and
cleanlinessand integrityCracked. or broken ultravioletfilters alkalimetalsmust be consideredThese. impuritiesmay cause
shallbe replacedimmediately.Sincea dropinlinevoltagecan embrittlementor corrosion,particularlyat elevate
causedecreasedblacklightoutputwithconsequentinconsis- temperaturesAny. suchevaluationshallalsoincludeconside
tentperformance,a constant-voltagetransformershouldbe ationof the form in which the impuritiesarepresent.Some
usedwhen thereisevidenceof voltagefluctuation. penetrantmaterialscontainsignificantamounts of theseimpu-
N OTE 1 4—Certain high-intensityblacklightsmay emit unacceptable ritiesin theform of volatileorganicsolventsthatnormall
amounts of visiblelight,which can cause fluorescentindicationsto evaporatequicklyand usuallydo not causeproblems.Other
disappearCareshouldbe. takento onlyusebulbssuitableforfluorescent materialsmay containimpurities,which arenot volatileand may
penetrantestingpurposes.
reactwiththepart,particularlyinthepresenceofmoistur or
8.9.1 .BlackLightWarm2-Up— Unlessotherwisespecified by elevatedtemperatures.
themanufacturer,allowthe blacklightto warm up fora minimum of 9.1 .2Because volatilesolventsleavethe surfacequickl
five minutespriorto use or measurement of its intensity. withoutreactionundernormal examinationprocedures,pen-
etrantmaterialsare normally subjectedto an evaporati
8.9.1 .VisualAdaptation3—Personnelexaminingpartsafter procedureto remove the solventsbefore the materialsare
penetrantprocessingshallbe in thedarkenedareaforatleast one analyzedfor impuritiesThe. residuefrom thisprocedurei
minute beforeexamining parts.Longer times may be thenanalyzedinaccordancewithTestMethod D1552 or Tes
necessaryundersome circumstancesPhotochromicor. tinted Method D129 decompositionfollowedby TestMethod E516
lenseshallnotbe worn duringtheprocessingand examination of Method B (TurbidimetricMethod) forsulfurThe. residuemay
parts. alsobe analyzedby Test Method D808 or Annex A2 on Methods
8.9.2VisibleLightExamination—Inspectpartstestedwith Type 2 forMeasuringTotalChlorineContentinCombustibl
visiblepenetrantundereithernaturalor artificialvisible light.Proper LiquidPenetrantMaterials(forhalogensotherthan fluorine and
illuminationis requiredto ensure adequate Annex A3 on Method for Measuring Total Fluorin Content in
sensitivityoftheexaminationA. minimum lightintensityatthe CombustibleLiquid PenetrationMaterials(fo fluorine)An.
examinationsurfaceof 100 fc [1076lx]isrequired(seeGuide E2297 alternativeprocedure,Annex A4 on Determina tionof Anions by
formore information). Ion Chromatography,providesa singl instrumentaltechniquefor
8.9.3Housekeeping—Keep the examinationarea free of rapidsequentialmeasurement of common anionssuch as
interferingdebris,includingfluorescentresiduesand objects. chloride,fluoride,and sulfateAlkal. metalsin the residueare
8.9.4IndicationVerificationFor— Type 1 inspectionsonly, itis determinedby flame photometry
common practiceto verifyindicationsby wiping the indicationwitha atomicabsorptionspectrophotometry,or ion chromatograph
solvent-dampenedswab or brush,allowing theareatodry,and (seeASTM D4327).
redevelopingthearea.Redevelopmenttime shallbe a minimum of
ten minutes,exceptnonaqueous redevelopmenttimeshouldbe a N OTE 1 5—Some currentstandardsrequireimpuritylevelsofsulfurand
halogensto not exceed 1 % of any one suspectelement.This leve
minimum of threeminutes.If however, may be unacceptablefor some applications,o the actua
theindicationdoesnotreappear,theoriginalindicationmay be maximum acceptableimpuritylevelmustbe decidedbetweensupplierand
consideredfalseThisproceduremay. be performedup totwo useron a caseby casebasis.
timesfor any givenoriginalindication. 9.2Elevated-TemperatureTesting—Where penetrantesti is
8.9.5Evaluation—All indicationsfound duringinspection shallbe performed on partsthatmust be maintainedat elevate
evaluatedin accordancewith acceptancecriteriaas temperatureduringexamination,specialpenetrantmateria and
specified.ReferencePhotographsof indicationsarenotedin E433). processingtechniquesmay be requiredSuch. examinatio
requiresqualificationin accordancewith10.2and themanu-
8.10PostCleaning—Post cleaningisnecessarywhen re- facturer’srecommendationsshallbe observed.
sidualpenetrantor developercouldinterferewith subsequent
10. Qualificationand
processingor with servicerequirements.It is particularly
Requalification 1 0.1PersonnelQualificationWhen— requiredby the
customer,allpenetranttestingpersonnelshallbe qualifie
importantwhere residualpenetranttestingmaterialsmight certifiedinaccordancewitha writtenprocedureconformingto
combine withotherfactorsinservicetoproducecorrosionand
priorto vapor degreasingor heattreatingthe partas these

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ASME BPVC.V-2017 ARTICLE 24,SE-165/SE-165M

the applicableditionof recommended PracticeSNT-TC-1 A, 10. 3NondestructiveTestingAgency Qualification—If a


ANSI/ASNT CP-1 89,NAS-41 0, or MIL-STD-41 0. nondestructivetestingagency as describedinPracticeE543 is
10. 2 ProcedureQualification—Qualificationof procedures using used to perform the examination,the agency shouldmeet the
times, conditions,or materialsdifferingfrom those requirementsof PracticeE543.
specifiedinthisgeneralpracticeor fornew materialsmay be 10. 4 Requalificationmay be requiredwhen a change or
performed by any of severalmethods and shouldbe agreed upon substitutionismade inthetypeof penetrantmaterialsorinthe
by thecontractingpartiesA. testpiececontainingone or more procedure(see10.2).
discontinuitiesof the smallestrelevantsizeisgenerally
used.When agreed upon by the contractingparties,the test
11.Keywords
piecemay containrealor simulateddiscontinuities,providing
itdisplaysthecharacteristicsofthediscontinuitiesencountered 11 .1fluorescentliquidpenetranttesting;hydrophilicemul-
inproductexamination. sification;lipophilicemulsification;liquidpenetranttestin
10.2.1Requalificationof the procedureto be used may be nondestructivetesting;solventremovable;visibleliquidpen-
requiredwhen a change is made to the procedureor when etranttesting;water-washable;post-emulsified;black ligh
materialsubstitutionismade. ultravioletlight;visiblelight

ANNEXES

(MandatoryInformation)

A1. CLEANING OF PARTS AND MATERIALS

A1.1 ChoiceofCleaningMethod A1 .1 .1 .3Vapor Degreasing—Vapor degreasingis a pre


ferredmethod of removing oilor grease-typesoilsfrom the
A1 .1 .1The choiceofa suitablecleaningmethod isbasedon
surfaceof partsand from open discontinuitiesIt.willnot
suchfactorsas:(1) typeofcontaminanttobe removed sinceno
remove inorganic-typesoils(dirt,corrosion,salts,etc.),and
one method removes allcontaminantsequallywell;( 2) effect
may notremove resinoussoils(plasticcoatings,varnish,paint
of the cleaningmethod on the parts;(3) practicalityof the
etc.)Because. of the shortcontacttime,degreasingmay not
cleaningmethod forthe part(forexample,a largepartcannot completelyclean out deep discontinuitiesand a subsequen
be put intoa small degreaseror ultrasonicleaner);and ( 4) solventsoak isrecommended.
specificcleaningrequirementsof thepurchaserThe. following
A1 .1 .1 .4AlkalineCleaning:
cleaningmethods are recommended:
(a)Alkaline cleanersare nonflammable water solutio
A1 .1 .1 .1DetergentCleaning—Detergentcleanersare non- containing speciallyselected detergents for wetting
flammable water-solublecompounds containingspeciallyse- penetrating,emulsifying,and saponifyingvarioustypes of
lectedsurfactantsfor wetting,penetrating,emulsifying,and soilsHot. alkalinesolutionsarealsoused forrustremoval and
saponifyingvarioustypesof soils,such as grease and oily descalingto remove oxide scale which can mask surfac
films,cuttingand machiningfluids,and unpigmented drawing discontinuitiesAlkalinecleanercompounds. must be used in
compounds, etc.Detergentcleanersmay be alkaline,neutral,or accordancewith the manufacturers’recommendations.Part
acidicin nature,but must be noncorrosiveto the item being cleaned by the alkalinecleaningprocess must be rinse
inspectedThe. cleaningpropertiesofdetergentsolutionsfacili- completelyfreeof cleanerand thoroughlydried priorto the
tatecomplete removal of soilsand contaminationfrom the penetranttestingprocess (parttemperatureat the time of
surfaceand void areas,thus preparingthem to absorb the penetrantapplicationshallnot exceed125°F [52°C].
penetrant.Cleaningtime shouldbe as recommended by the (b)Steam cleaningisa modificationof the hot-tankalka
manufacturerof thecleaningcompound. linecleaningmethod, which can be used for preparationof
A1 .1 .1 .2SolventCleaning—There are a varietyof solvent large,unwieldypartsItwillremove. inorganicsoilsand many
cleanersthatcan be effectivelyutilizedtodissolvesuchsoilsas organicsoilsfrom thesurfaceofparts,butmay not reachtothe
grease and oily films, waxes and sealants,paints,and in bottom ofdeep discontinuities,and a subsequentsolventsoak
general,organicmatter.These solventshouldbe residue-free, isrecommended.
especiallywhen used as a hand-wipesolventor as a dip-tank A1 .1 .1 .5UltrasonicCleaning—Thismethod addsultrason
degreasingsolventSolventcleanersarenot. recommended for agitationtosolventor detergentcleaningto improve cleanin
theremoval of rustand scale,weldingflux and spatter,and in efficiencyand decreasecleaningtime.Itshouldbe used with
general,inorganicsoilsSome. cleaningsolventsareflammable waterand detergentifthesoiltobe removed isinorganic(rus
and can be toxic.Observe allmanufacturers’instructionsand dirt,salts,corrosionproducts,etc.),and withorganicsolventi
precautionarynotes. thesoiltobe removed isorganic(greaseand oilyfilms, etc.

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Afterultrasoniccleaning,partsmust be rinsedcompletelyfree of Acid solutions/etchantsare also used routinelyto remove


cleaner,thoroughlydried,and cooled to at least125°F smeared metal thatpeens over surfacediscontinuitiesSuch.
[52°C],beforeapplicationof penetrant. etchantshouldbe usedinaccordancewiththemanufacturers
A1 .1 .1 .Paint6 Removal— Paint films can be effectively recommendations.
removed by bond release solvent paint remover or disintegrating-
N OTE A1 .1 —Etched partsand materialsshouldbe rinsedcompletel
typehot-tankalkalinepaintstrippersIn. most cases,thepaintfilm must freeofetchants,thesurfaceneutralizedand thoroughlydriedby heatprio
be completelyremoved toexposethe surfaceofthemetal.Solvent- toapplicationofpenetrantsAcidsand. chromatescan adverselyaffectthe
typepaintremoverscanbe ofthe high- fluorescenceoffluorescentmaterials.
viscositythickenedtypeforsprayorbrushapplicationor canbe oflow N OTE A1 .2—Whenever thereisa possibilityofhydrogenembrittlemen
viscositytwo-layertypefordip-tankapplication. Both typesof as a resultofacidsolution/etching,thepartshouldbe baked at a suitab
temperatureforan appropriatetimetoremove thehydrogenbeforefurthe
solventpaintremovers are generallyused at processingAfterbaking,thepartshallbe. cooledto a temperaturebelow
ambienttemperatures,as receivedHot.-tankalkalinestrippers 125°F[52°C]beforeapplyingpenetrants.
shouldbe usedinaccordancewith themanufacturer’sinstruc-
A1 .1 .1 .AirFiringofCeramics9—Heatingofa ceramicpar in a
tionsAfterpaintremoval,thepartsmust. be thoroughlyrinsed to
clean,oxidizingatmosphere is an effectiveway of removing
remove allcontaminationfrom the void openings,thor-oughly
moistureorlightorganicsoilor both.The maximum
dried,and cooled to at least125°F [52°C] before applicationof
temperaturethatwillnotcausedegradationofthepropertiesof
penetrant.
theceramicshouldbe used.
A1 .1 .1 .MechanicalCleaningand7 SurfaceConditioning— Metal-
removingprocessessuch as filing,buffing,scraping, A1.2 PostCleaning
mechanicalmilling,drilling,reaming,grinding,liquidhoning,
sanding,lathecutting,tumble or vibratorydeburring,and A1 .2.1Removal of Developer—Dry powder developercan be
abrasiveblasting,includingabrasivessuch as glassbeads, effectivelyremoved with an airblow-off(freeof oil)or i canbe
sand,aluminum oxide,ligno-cellulosepellets,metallicshot, etc.are, removed withwaterrinsingWet. developercoatingscan be
oftenused to remove such soilsas carbon,rustand scale,and removed effectivelyby waterrinsingor waterrinsingwith
detergenteitherby hand or with a mechanicalassist(scru
foundry adheringsands,as well as to deburror producea
brushing,machine washing,etc.)The. solubledevelopercoat
desiredcosmeticeffecton thepart.These processes
ingssimplydissolveoffof thepartwith a waterrinse.
may decreasethe effectivenessof the penetranttestingby
smearingor peeningovermetal surfacesand fillingdisconti- A1 .2.2Residualpenetrantmay be removed throughsolven
nuitiesopen to thesurface,especiallyfor softmetalssuchas action.Solventsoaking(15 min minimum), and ultrason
aluminum,titanium,magnesium,and berylliumalloy. solventcleaning(3 min minimum) techniquesare recom-
A1 .1 .1 .Acid8 Etching—Inhibitedacid solutions(pickling mended. In some cases,itisdesirabletovapor degrease,then
solutions)are routinelyused for descalingpart surfaces. followwith a solventsoak.The actualtime requiredin the
Descalingisnecessarytoremove oxidescale,which can mask vapordegreaserand solventsoakwilldepend on thenatureof
surfacediscontinuitiesand preventpenetrantfrom entering. thepartand shouldbe determinedexperimentally.

A2. METHODS FOR MEASURING TOTAL CHLORINE CONTENT IN COMBUSTIBLE LIQUID


PENETRANT MATERIALS

A2.1 Scopeand Application titrimetricallyeitheragainstsilvernitratewith the end poin


A2.1 .1These methods coverthedeterminationof chlorine in detectedpotentiometrically(Method A) or coulometrical with
theend pointdetectedby currentflow increase(Method B).
combustibleliquidpenetrantmaterials,liquidor solidIts. range of
applicabilityis 0.001 to 5 % usingeitherof the
alternativetitrimetricproceduresThe. proceduresassume that A2.2.1 .1Safety—Strictadherenceto allof the provisio
bromine or iodinewillnot be present.Iftheseelementsare prescribedhereinafterensuresagainstexplosiveruptureof the
present,theywillbe detectedand reportedaschlorineThe. full bomb, or a blow-out,providedthebomb isof properdesig and
amount of theseelements willnot be reported.Chromate constructionand in good mechanical condition.It i
interfereswith theprocedures,causinglow or nonexistentend desirable,however,thatthebomb be enclosedin a shieldof
points.The method is applicableonly to materialsthatare steelplateat least1⁄2 in.[12.7mm] thick,or equivale protectionbe
totallycombustible. providedagainstunforeseeablecontingencies

A2.2 Summary ofMethods A2.3 Apparatus

A2.2.1The sample isoxidizedby combustionin a bomb A2.3.1Bomb, havinga capacityof notlessthan300 mL, so
containingoxygen underpressure(seeA2.2.1 .1)The. chlorine constructedthatit willnot leak during the test,and tha
compounds thusliberatedare absorbedin a sodium carbonate quantitativerecoveryof the liquidsfrom the bomb may be
solutionand the amount of chloridepresentis determined readilyachieved.The innersurfaceofthebomb may be made

622
ASME BPVC.V-2017 ARTICLE 24,SE-165/SE-165M

ofstainlessteelor any othermaterialthatwillnotbe affected by A2.5.2.3Placethealuminum dishon a hotplatein a fume hood.


thecombustionprocessor productsMaterialsusedin. the bomb
assembly,such as the head gasket and leadwire A2.5.2.4Let thematerialevaporateuntilthedishisnearl dry.
insulation,shallbe resistanttoheatand chemicalaction,and shallnot
undergoany reactionthatwillaffectthe chlorine contentof A2.5.2.5Placethedishintoa preheatedoven from 194°F
theliquidinthebomb. [90°C]to212°F [100°C]for10 minutes.
A2.3.2Sample Cup,platinum,24 mm inoutsidediameterat A2.5.2.6Take thedishoutof theoven and allowto cool.
thebottom,27 mm inoutsidediameteratthetop,12 mm in A2.5.2.7Reweigh thedishand recordweight.
heightoutsideand weighing10 to 11 g,opaque fusedsilica, wide- N OTE A2.3— For Cleaners—If theresidueislessthan50 ppm, repor
theresidueweight.Iftheweightisgreaterthan50 ppm, proceedwiththe bomb
formwith an outsidediameterof 29 mm at thetop,a heightof 19 mm, procedure.
and a 5-mL capacity(Note 1),or nickel (Kawin capsuleform),top
diameterof 28 mm, 15 mm in height,and 5-mL capacity. A2.6 Decomposition
A2.6.1Reagentsand Materials:
N OTE A2.1 —Fused silicacruciblesare much more economicaland A2.6.1 .Oxygen,1freeof combustiblematerialand haloge
longer-lastingthanplatinumAftereachuse,theyshouldbe. scrubbedout compounds,availableata pressureof 40 atm [4.05MPa].
withfine,wet emery cloth,heatedtodullredheatovera burner,soaked
inhotwaterfor1 h,thendriedand storedina desiccatorbeforereuse. A2.6.1 .Sodium2 Carbonate Solution(50 g Na 2CO 3/L)—
Dissolve50 g ofanhydrousNa CO 3 or 58.5g ofNa 2 CO · O)
2 32

A2.3.3FiringWire,platinum,approximatelyNo. 26 B & S gage. or 135g of Na 2 CO 3·10H2 O inwaterand diluteto 1 L.


A2.6.1 .White3 Oil,refined.
A2.3.4IgnitionCircuit(NoteA2.2),capableof supplying A2.6.2Procedure:
sufficientcurrentoignitethenylonthreador cottonwicking
A2.6.2.1Preparationof Bomb and Sample— Cut a pieceof
withoutmeltingthewire.
firingwireapproximately100 mm inlength.Coilthemiddle
N OTE A2.2—The switchintheignitioncircuitshouldbe ofa typethat section(about20 mm) and attachthefreeendstotheterminal
remainsopen,exceptwhen heldinclosedpositionby theoperator. Arrangethecoilsothatitwillbe aboveand toone sideof the
A2.3.5Nylon Sewing Thread,or CottonWicking,white. samplecup.Place5 mL ofNa 2CO 3 solutioninthebomb (Note
A2.4),placethecoveron thebomb and vigorouslyshakefor15 s
A2.4 Purityof Reagents todistributhesolutionovertheinsideof thebomb. Open
A2.4.1Reagentgradechemicalsshallbe used in alltests. thebomb, placethesample-filledsamplecup in thetermina
Unlessotherwiseindicated,itisintendedthatallreagentshall holder,and inserta shortlengthof threadbetweenthefirin
conform to thespecificationsof theCommittee on Analytical wireand thesample.Use of a sampleweightcontainingove
Reagents of the American Chemical Society,where such 20 mg of chlorinemay cause corrosionof the bomb. The
specificationsare availableOthergradesmay. be used pro- sampleweightshouldnotexceed0.4g iftheexpectedchlori
contentis2.5% orabove.Ifthesampleissolid,notmore than
videditisfirstascertainedthatthe reagentisof sufficiently
highpuritytopermititsusewithoutlesseningtheaccuracyof 0.2g shouldbe used.Use 0.8g ofwhiteoilwithsolidsamples
thedetermination. Ifwhiteoilwillbe used(NoteA2.5),add ittothesamplecup
by means of a dropperatthistime (seeNote A2.6 and Note
A2. 4.2Unlessotherwiseindicated,referencestowatershall
A2.7).
be understoodtomean refereegradereagentwaterconforming
toSpecificationD1193. N OTE A2.4—After repeateduseofthebomb forchlorinedeterminatio
a film may be noticedon the innersurface.This dullnessshouldbe
A2.5 Sample Preparation removed by periodicpolishingof thebomb. A satisfactorymethod for
doingthisistorotatethebomb ina latheatabout300 rpm and polishthe
A2. 5.1Penetrants,Developers,Emulsifiers,MagneticOils: insidesurfacewithGritNo. 2/0or equivalentpapercoatedwitha ligh
A2. 5.1 .1Weigh 50 g of testmaterialintoa 150-mm petri machineoiltopreventcutting,and thenwitha pasteofgrit-freechromic
dish. oxideandwater.Thisprocedurewillremove allbutverydeeppitsandput
A2. 5.1 .2Placethe150-mm petridishintoa 194°F[90°C]to a highpolishon thesurfaceBeforeusingthebomb,. itshouldbewashed
with soap and water to remove oilor pasteleftfrom the polishi
212°F[100°C]oven for60 minutes. operationBombs. with porousor pittedsurfacesshouldneverbe used
A2. 5.1 .3Allow thetestmaterialto coolto room tempera- becauseof thetendencyto retainchlorinefrom sample tosample.Itis
ture. recommended tonotuse more than1 g totalof sample and whiteoilor
otherchlorine-freecombustiblematerial.
A2. 5.2SolventCleaners: N OTE A2.5—If thesampleisnotreadilymisciblewithwhiteoil,some
A2. 5.2.1Take thetareweightof an aluminum dish. othernonvolatile,chlorine-freecombustiblediluentmay be employedin
A2. 5.2.2Weigh 100g ofthecleanerintothealuminum dish. place of white oil.However, the combined weight of sample and
nonvolatilediluentshallnot exceed 1 g. Some solidadditivesare
relativelyinsoluble,butmay be satisfactorilyburnedwhen coveredwith
a layerofwhiteoil.
N OTE A2.6—The practiceofrunningalternatelysampleshighand low
inchlorinecontentshouldbe avoidedwheneverpossibleItisdifficultto.
rinsethe lasttracesof chlorinefrom thewallsof the bomb and the
tendencyforresidualchlorinetocarryoverfrom sample tosample has
been observedin a number of laboratoriesWhen. a sample high in

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ARTICLE 24,SE-165/SE-165M ASME BPVC.V-2017

chlorinehas preceded one low in chlorinecontent,the teston the low- A2.7.3Collectionof Chlorine Solution—Remove the sample cup
chlorinesampleshouldberepeatedand one orbothofthelow values withcleanforcepsand placein a 400-mL beaker Wash down
thusobtainedshouldbeconsideredsuspectiftheydo notagreewithinthe
limitsofrepeatabilityof thismethod. thewallsof thebomb shellwitha fine streamof methanolfrom a
wash bottle,and pourthewashingsintothe beaker.Rinseany
A2.6.2.2Addition of Oxygen— Place the sample cup in residueintothebeaker.Next,rinsethebomb coverand
positionand arrangethenylonthread,or wispofcottonsothat theend terminalsintothebeaker.Finally,rinsebothinsid and outsideof
dipsintothesample.Assemble thebomb and tighten thesample crucibleintothebeaker.Washings shouldequalbut
thecoversecurelyAdmit. oxygen (seeNote A2.7)slowly(to notexceed100 mL. Add methanolto make 100 mL.
avoidblowingthe sample from the cup) untila pressureis
reachedas indicatedin TableA2.1 .
A2.7.4Determinationof Chlorine—Add 5 mL of H 2 SO 4
N OTE A2.7—It isrecommended tonotadd oxygen orignitethesample (1:2)to acidifythesolution(solutionshouldbe acidtolitmu and
ifthe bomb has been jarred,dropped,ortilted.
clearof white Na 2 CO 3 precipitate)Add. 100 mL of
A2.6.2.3Combustion— Immerse thebomb in a cold-water acetone.Placetheelectrodesinthesolution,starthestirrer(i
bath.Connecttheterminalstotheopen electricalcircuitClose. mechanicalstirreristobe used),and begintitrationIftitrat.
thecircuito ignitethesample.Remove thebomb from the bath ismanual,setthepH meteron theexpandedmillivoltscaleand
afterimmersion for at leastten minutes.Releasethe pressureata notethereadingAdd. exactly0.1mL ofAgNO 3 solutionfrom
slow,uniformratesuchthattheoperationrequires notlessthan1 min. theburet.Allow a few secondsstirring;then recordthenew
Open thebomb and examinethecontents. Iftracesof unburnedoilor millivoltreading.Subtractthe secondreadingfrom thefirst
sootydepositsarefound,discard thedetermination,and Continuethetitration,notingeach amount ofAgNO 3 soluti and
thoroughlycleanthebomb beforeagain puttingitin use (NoteA2.4).
theamount of differencebetween thepresentreadingand
thelastreading.Continueadding0.1 -mLincrements,making
readingsand determiningdifferencesbetweenreadingsuntila
A2.7 Analysis,Method A, PotentiometricTitrationProce-dure
maximum differencebetween readingsisobtainedThe. tota
amount ofAgNO 3 solutionrequiredtoproducethismaximum
A2. 7.1Apparatus: differentialistheend point.Automatictitratorscontinuous
A2. 7.1 .1SilverBilletElectrode. stirthesample,add titrant,measure thepotentialdifferenc
A2. 7.1 .2Glass Electrode,pH measurement type. calculatethedifferential,and plotthedifferentialon a chart The
A2. 7.1 .3Buret,25-mL capacity,0.05-mLgraduations. maximum differentialistakenas theend point.
A2. 7.1 .4MillivoltMeter, or expanded scalepH meter ca-
pableof measuring0 to 220 mV. N OTE A2.9—For maximum sensitivity,0.00282N AgNO
3 solutionmay
N OTE A2.8—An automatictitratorishighlyrecommended inplaceof be usedwiththeautomatictitratorThisdilutereagentshouldnotbe. used
itemsA2.7.1 .and3 A2.7.1 .4Repeatabilityand. sensitivityofthe method withlargesamples orwhere chlorinecontentmay be over0.1% sinc
aremuch enhancedby theautomaticequipmentwhilemuch tediouseffort thesetestswillcauseend pointsof10 mL orhigher.The largeamount of
isavoided. waterused in such titrationsreducesthe differentialbetween reading
making theend pointverydifficultto detectFor. chlorinecontentsover 1 %
A2.7.2Reagentsand Materials:
insamplesof0.8g orlarger,0.282N AgNO 3 solutionwillbe require to
A2.7.2.1Acetone,chlorine-free. avoidexceedingthe10-mL waterdilutionlimit.
A2.7.2.2Methanol,chlorine-free.
A2.7.2.3SilverNitrate Solution(0. 0282N)— Dissolve A2.7.5Blank— Make blankdeterminationswiththeamount of
4. 79106 0.0005g of silvernitrate(AgNO 3) in water and white oilused but omittingthe sample.(Liquidsample
diluteto1 L. normallyrequireonly0.15to 0.25g of whiteoilwhilesolid
require0.7to0.8g.)Follownormal procedure,making two or
A2.7.2.4Sodium ChlorideSolution(0. 0282N)— Dry a few grams
threetestrunsto be suretheresultsarewithinthelimitsof
of sodium chloride(NaCl) for 2 h at 130 to 150°C, weigh out1
.64806 0.0005g of thedriedNaCl, dissolvein water,and diluteto1 repeatabilityforthetestRepeatthisblankprocedurewhenever. new
L. batchesof reagentsor whiteoilareused.The purposeof
theblankrun isto measure thechlorinein thewhiteoil,the
A2.7.2.5SulfuricAcid (1 + 2)— Mix 1 volume of concen-
reagents,and thatintroducedby contamination.
tratedsulfuricacid(H2 SO 4 , sp.gr 1 .84)with 2 volumes of water.
A2.7.6StandardizationSilvernitratesolutionsarenotper—
manentlystable,so thetrueactivityshouldbe checkedwhen
thesolutionisfirstmade up and then periodicallyduringthe lifeof
thesolutionThisisdone. by titrationf a known NaCl solutionas
TABLE A2.1 Gauge Pressures
follows:Preparea mixtureof theamounts of the
Capacity of Bomb, Gauge Pressure, atm [MPa]
chemicals(Na2CO 3 solution,H 2SO 4 solution,acetone,and
mL minA max
methanol)specifiedforthetestPipetin5..0mL of 0.0282N-NaCl
300 to350 38 [3.85] 40 [4. 05]
350 to400 35 [3.55] 37 [3. 75] solutionand titratetotheend point.Prepareand titrat
400 to450 30 [3.04] 32 [3. 24] similarmixtureofallthechemicalsexcepttheNaCl solutio
450 to500 27 [2.74] 29 [2. 94] thusobtaining reagentblankreading.Calculatethenormalit of
A
The minimum pressures are specified to providesufficientoxygen forcomplete theAgNO 3 solutionas follows:
combustion and the maximum pressures presenta safetyrequirement.
5.03 N N aCl
N A gNO 3 5 (A2. 1)
VA 2 VB

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ASME BPVC.V-2017 ARTICLE 24,SE-165/SE-165M

where: equipmentmanufacturer.Gentlyheatwithcontinuousmixing
N AgNO3 = normalityof theAgNO 3 solution, untilthegelatiniscompletelydissolved.
N NaCl = normalityof theNaCl solution, A2.8.3.2Divideintoaliquotseachsufficientforone day’
VA = millilitresofAgNO 3 solutionusedforthetitra- analyses(Thirtymillilitresisenough. forapproximatelyeleve
tionincludingtheNaCl solution,and titrationsKeep.) the remainderin a refrigerator,but do not
VB = millilitresofAgNO 3 solutionusedforthetitra- freeze.The solutionwillkeep for aboutsix months in the
tionof thereagentsonly. refrigeratorWhen. readyto use,immerse theday’saliquotin
A2. 7.7CalculationCalculatethechlorinecontentof— the hotwaterto liquefythegelatin.
sample as follows: A2.8.3.3GlacialAceticAcid-NitricAcidSolution—A typi
~VS2 VB!3 N 3 3.545 calratiois12.5to1 (12.5partsCH 3 COOH to1 partHNO 3)
Chlorine,weight% 5 W
(A2. 2) A2.8.3.4Mix enough gelatinsolutionand of aceticacid
nitricacidmixturefor one titration(A. typicalmixtureis2.
where: mL of gelatinsolutionand 5.4 mL of acetic-nitricaci
VS = millilitresofAgNO 3 solutionused by thesample, mixture.)
VB = millilitresofAgNO 3 solutionused by theblank,
N OTE A2.11 —The solutionmay be premixed ina largerquantityfor
N = normalityof theAgNO 3 solution,and convenience,butmay notbe useableafter24 h.
W = grams of sample used.
A2.8.3.5Run atleasthreeblankvaluesand takean averag
A2. 7.8Precisionand Accuracy:
accordingto theoperatingmanual of thetitratorDetermin.
A2. 7.8.1The followingcriteriashouldbe used forjudging
separateblanksforbothfive dropsofmineraloiland 20 drop
theacceptabilityof results:
of mineraloil.
A2.7.8.1 .Repeatability1Resultsby— the same analyst
shouldnot be consideredsuspectunlessthey differby more A2.8.4Titration:
than0.006% or10.5% of thevaluedetermined,whicheveris A2.8.4.1Weigh tothenearest0.1g and recordtheweightof
higher. the100-mL beaker.
A2. 7.8.1 .Reproducibility2Resultsby— differentlaborato- A2.8.4.2Remove the sample cruciblefrom thecover as
riesshouldnot be consideredsuspectunlessthey differby sembly supportringusinga cleanforceps,and,usinga wash
more than0.013% or 21 .3% of thevaluedetected,whichever bottle,rinseboththeinsideand theoutsidewithwaterintothe
ishigher. 100-mL beaker.
A2. 7.8.1 .Accuracy3 —The averagerecoveryof themethod A2.8.4.3Empty the bomb shellinto the 100-mL beaker
is86 % to 89 % of theactualamount present. Wash down thesidesof thebomb shellwith water,usinga
wash bottle.
A2.8 Analysis,Method B, CoulometricTitration
A2.8.4.4Remove thecoverassemblyfrom thecoverassem-
A2. 8.1Apparatus: blysupport,and,usingthewash bottle,rinsetheunderside,the
A2. 8.1 .1CoulometricChlorideTitrator. platinumwire,and theterminalsintothesame 100-mL beaker
A2. 8.1 .2Beakers,two,100-mL, or glazedcrucibles(pref- The totalamount of washingsshouldbe 50 6 1 g.
erablywith11⁄2 in.-outsidiameterbottom). A2.8.4.5Add specifiedamounts of gelatinmixture and
A2. 8.1 .3Refrigerator.
aceticacid-nitricacidmixture,orgelatinmix-aceticacid-nit
A2. 8.2Reagents: acidmixture,ifthiswas premixed,intothe100-mL beakertha
A2. 8.2.1AceticAcid,Glacial. containsthe 50 g of washings includingthe decomposed
A2. 8.2.2Dry GelatinMixture. sample.
A2. 8.2.3NitricAcid. A2.8.4.6Titrateusinga coulometrictitrimeter,accordingto
A2. 8.2.4Sodium ChlorideSolution—100 meq C/1 .Dry a operatingmanual procedure.
quantityofNaCl for2 h at130to150°C.Weigh out5.84406
0.0005g ofdriedNaCl ina closedcontainer,dissolveinwater, A2.8.5CalculationsCalculatethechlorideionconcentr—
and diluteto1 L. tioninthesample as follows:

A2.8.3ReagentPreparation: ~P2 B!3M


Chlorine,weight% 5 (A2.3
W
N OTE A2.10—The normal reagentpreparationprocesshasbeen slightly
changed,duetotheinterferencefrom the50 mL ofwaterrequiredtowash where:
thebomb. Thismodified processeliminatesthe interferenceand does not P = counterreadingobtainedwiththesample,
alterthequalityof thetitration.
B = averagecounterreadingobtainedwithaverageof the
A2.8.3.1GelatinSolution—A typicalpreparationis:Add threeblank readings,
approximately1 L of hotdistilledordeionizedwatertothe6.2 g of M = standardizationconstant.This is dependent on the
drygelatinmixturecontainedin one vialsuppliedby the instrumentrangesettinginuseand thereadingobtaine
witha known amount ofthe100 meq ofCl perlitreof
solution,and
W = weightof sample used,g.
A2.8.6Precisionand Accuracy:

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A2.8.6.1Duplicateresultsby the same operatorcan be 0.1 % chlorineand above ±2%

expectedtoexhibithe followingrelativestandarddeviations: 0.001 to 0.01 % chlorine ±9%.

Approximate % Chlorine RSD, % A2.8.6.3Ifbromine ispresent,36.5% of the trueamount


1.0 and above 0.10
willbe reportedIfiodineispresent,20..7% ofthetrueamount
0. 1 2. 5 willbe reportedFluorinewillnot. be detected.
0. 003 5.9

A2.8.6.2The method can be expectedto reportvaluesthat vary


from thetruevalueby thefollowingamounts:

A3. METHOD FOR MEASURING TOTAL FLUORINE CONTENT IN COMBUSTIBLE


LIQUID PENETRANT MATERIALS

A3.1 Scopeand Application A3.4.2.2Weigh 100 g ofthecleanerintothealuminum dish


A3.1 .1Thismethod coversthe determinationof fluorinein A3.4.2.3Placethe aluminum dishon a hotplateina fume hood.
combustibleliquidpenetrantmaterials,liquidor solid,thatdo not
containappreciableamounts of interferingelements,or have any A3.4.2.4Letthe materialevaporateuntilthe dishisnearl dry.
insolubleresidueaftercombustion.Itsrange of applicabilityis1 to
200 000 ppm. A3.4.2.5Placethedishintoa preheatedoven from 194°
[90°C]to 212°F[100°C]for10 minutes.
A3.1 .2The measure of the fluorinecontentemploys the A3.4.2.6Take the dishoutof the oven and allowto cool.
fluorideselectiveionelectrode. A3.4.2.7Reweigh the dishand recordweight.
A3.2 Summary ofMethod N OTE A3.1 — For Cleaners—If theresidueislessthan 50 ppm, repor
theresidueweight.Iftheweightisgreaterthan50 ppm, proceedwith the
A3.2.1 The sample isoxidizedby combustionin a bomb bomb procedure.
containingoxygen underpressure(seeA3.2.1 .1)The. fluorine A3.5 Apparatus
compounds thus liberatedare absorbedin a sodium citrate
solutionand the amount of fluorinepresentis determined A3.5.1Bomb, havinga capacityof notlessthan300 mL, so
potentiometricallythroughthe use of a fluorideselectiveion constructedthat itwillnot leak during the test,and tha
electrode. quantitativerecoveryof the liquidsfrom the bomb may be
A3.2.1 .1Safety—Strictadherenceto allof the provisions readilyachieved.The innersurfaceof thebomb may be made of
prescribedhereinafterensuresagainstexplosiveruptureofthe bomb, stainlessteelor any othermaterialthatwillnotbe affecte by the
or a blow-out,providedthe bomb isof properdesign and combustionprocessor products.Materialsused inthe bomb
constructionand in good mechanicalcondition.It is assembly, such as the head gasket and leadwir
desirable,however,thatthe bomb be enclosedin a shieldof insulation,shallbe resistanttoheat and chemicalaction,and
steelplateat least1⁄2 in.[12.7mm] thick,or equivalent protectionbe shallnot undergo any reactionthatwillaffectthe fluorin contentof
providedagainstunforeseeablecontingencies. the liquidin thebomb.
A3.5.2Sample Cup, nickel,20 mm in outsidediametera
A3.3 Interferences
thebottom,28 mm inoutsidediameteratthe top,and 16 mm in
A3.3.1Silicon,calcium,aluminum, magnesium, and other height;or platinum,24 mm in outsidediameterat the bottom,27
metalsforming precipitateswith fluorideion willinterfereif they are mm inoutsidediameteratthetop,12 mm inheigh and weighing10
presentin sufficientconcentrationto exceed the solubilityof to11 g.
theirrespectivefluorides.Insolubleresidueafter
A3.5.3FiringWire,platinum,approximatelyNo. 26 B & S gage.
combustionwillentrainfluorineeven ifotherwisesoluble.

A3.4 SamplePreparation A3.5.4IgnitionCircuit(Note A3.2),capableof supplyin


A3.4.1 Penetrants,Developers,Emulsifiers,MagneticOils: sufficientcurrentto ignitethe nylon threador cottonwickin
withoutmeltingthe wire.
A3.4.1 .1Weigh 50 g of testmaterialintoa 150-mm petri dish.
N OTE A3.2— Caution:The switchintheignitioncircuitshouldbe of a type
A3.4.1 .2Placethe150-mm petridishintoa 194°F[90°C]to thatremains open, exceptwhen held in closedpositionby the operator.
212°F [100°C]oven for60 minutes.
A3.4.1 .3Allow the testmaterialto coolto room tempera-ture. A3.5.5Nylon SewingThread,or CottonWicking,white.
A3.5.6Funnel,polypropylene(NoteA3.3).
A3.4.2 SolventCleaners: A3.5.7VolumetricFlask,polypropylene,100-mL (Note
A3.4.2.1Take the tareweightof an aluminum dish. A3.3).

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A3.5.8Beaker,polypropylene,1 50-mL (NoteA3.3). N OTE A3.4—Use of sampleweightscontainingover20 mg of chlorin


may causecorrosionof thebomb. To avoidthisitisrecommended thatfo
A3.5.9Pipet,1 00-µL,Eppendorf-type(Note A3.3). samplescontainingover2 % chlorine,thesampleweightbe basedon the
followingtable:
A3.5.1 0MagneticStirrerand TFE-coatedmagneticstirring bar.
Chlorine Sample White Oil
Content,% weight,g weight,g
A3.5.11FluorideSpecificIon Electrodeand suitablerefer-ence
2 to 5 0. 4 0.4
electrode. 5 to 10 0. 2 0.6
10 to 20 0. 1 0.7
A3.5.12MillivoltMeter capableof measuringto 0.1mV. 20 to 50 0. 05 0.7

N OTE A3.3—Glassware should never be used to handle a fluoride Do not use more than1 g totalof sample and white oilor
solutionas itwillremove fluorideionsfrom solutionor on subsequentuse otherfluorine-freecombustiblematerial.
carryfluorideionfrom a concentratedsolutionto one more dilute.
A3.7.2AdditionofOxygen— Placethesample cup in posi
A3.6 Reagents tionand arrangethenylonthread,orwisp ofcottonso thatthe end
dipsintothe sample.Assemble the bomb and tightenth
A3.6.1PurityofReagents—Reagentgrade chemicalsshall be
coversecurelyAdmit. oxygen (seeNote A3.5)slowly(toavoi
used in alltestsUnlessotherwiseindicated,itisintended.
thatallreagentsshallconform to the specificationsof the blowingthesamplefrom thecup)untila pressureisreachedas
Committee on AnalyticalReagentsoftheAmerican Chemical indicatedin TableA3.1 .
9

Society,where suchspecificationsareavailable.Othergrades may N OTE A3.5— Caution: Itisrecommended to notadd oxygen or igni the
be used,provideditisfirstascertainedthatthereagentis of sampleifthebomb has been jarred,dropped,or tilted.
sufficientlyhigh purityto permititsuse withoutlessening the A3.7.3Combustion—Immerse the bomb in a cold-wat
accuracyof the determination. bath.ConnecttheterminalstotheopenelectricalcircuitClos. the
A3.6.2Purityof Water— Unless otherwiseindicated,all circuito ignitethe sample.Remove the bomb from th bath
referencestowatershallbe understoodtomean Type Ireagent afterimmersion foratleast10 min. Releasethe pressu ata
water conformingtoSpecificationD1193. slow,uniformratesuchthattheoperationrequiresnotles than1 min.
Open thebomb and examine thecontentsIftrace. of unburned oil
A3.6.3Fluoride Solution,Stock (2000 ppm)— Dissolve or sooty depositsare found, discardth determination,and
4. 42006 0.0005g of predried(at130 to 150°C for1 h,then thoroughlycleanthe bomb before agai puttingitinuse.
cooledin a desiccator)sodium fluoridein distilledwaterand
diluteto 1 L.
A3.7.4Collectionof FluorineSolution—Remove th sample cup
A3.6.4Oxygen,freeof combustiblematerialand halogen with cleanforcepsand rinsewith wash soluti intoa 100-mL
compounds, availableata pressureof 40 atm [4.05MPa]. volumetricflask.Rinse the wallsof the bomb shellwith a fine
A3.6.5Sodium CitrateSolution—Dissolve27 g of sodium streamof wash solutionfrom a wash bottl and add the
citratedihydratein waterand diluteto 1 L. washingstothe flask.Next,rinsethe bomb cove and terminalsinto
the volumetricflask. Finally,add wash
A3.6.6Sodium HydroxideSolution(5 N)— Dissolve200 g solutiontobringthecontentsof the flask to theline.
ofsodium hydroxide(NaOH) pelletsinwaterand diluteto1 L;
storeina polyethylenecontainer. A3.8 Procedure
A3.6.7Wash Solution(ModifiedTISAB,TotalIonicStrength A3.8.1Ascertaintheslope(millivoltsperten-foldchangei
AdjustmentBuffer)—To 300 mL of distilledwater,add 32 mL of concentration)of the electrodeas describedby the manufac-
glacialaceticacid,6.6g of sodium citratedihydrate,and 32.15g of turer.
sodium chlorideStirtodissolveand. thenadjustthe pH to
A3.8.2Obtaina blanksolutionby performingtheprocedur
5.3using5 N NaOH solutionCool. and diluteto1 L. withouta sample.
A3.6.8White Oil,refined.
A3.8.3Immerse the fluorideand referenceelectrodesi
A3.7 DecompositionProcedure solutionsand obtainthe equilibriumreadingto 0.1mV. (The
conditionof the electrodedeterminesthe lengthof time
A3.7.1PreparationofBomb and Sample— Cut a pieceof firingwire
approximately100 mm in length.Coilthe middle section(about20
mm) and attachthefreeendstotheterminals. Arrange thecoilso
thatitwillbe above and to one sideof the sample cup.Place 10 mL TABLE A3.1 Gauge Pressures
of sodium citratesolutionin the bomb, placethe coveron thebomb, Gauge Pressure atm (MPa]
Capacityof Bomb, mL
and vigorouslyshake for minA max
15 s todistributhesolutionovertheinsideofthebomb. Open the 300 to 350 38 40
bomb, placethe sample-filledsample cup in the terminal 350 to 400 35 37
400 to 450 30 32
holder,and inserta shortlengthof threadbetween the firing wire 450 to 500 27 29
and the sample.The sample weight used should not exceed 1 g. A
The minimum pressuresare specifiedto providesufficientoxygen forcomplete
Ifthe sampleisa solid,add a few dropsof white oilatthistime to combustionand themaximum pressurespresenta safetyrequirement.
ensureignitionof the sample.

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ARTICLE 24,SE-165/SE-165M ASME BPVC.V-2017

necessarytoreachequilibriumThis. may be as littleas5 min or as S = slopeof fluorideelectrodeas determinedinA3.8.1


much as 20 min.) and
A3.8.4 Add 100 µL ofstockfluoridesolutionand obtainthe W = grams of sample.
readingafterthe same lengthof time necessaryfor A3.8.3.
A3.10Precisionand Bias
A3.9Calculation
A3.10.1RepeatabilityThe— resultsof two determinatio by the
A3.9.1 Calculatethe fluorine contentof the sample as follows: same analystshouldnotbe consideredsuspectunles theydifferby
more than1 .1ppm (0.00011%) or8.0% ofthe amount
2 3 1024 23 102 4 detected,whicheverisgreater.
F 10∆ E1/S 2 1 2 10∆ E 2/S2 1 G
A3.10.2ReproducibilityThe— resultsoftwo determinatio by
Fluorine,ppm 5 W 3 106
differentlaboratorieshould not be consideredsuspec unlessthey
(A3.1)
differby 6.7 ppm or 129.0% of the amount
where: detected,whicheverisgreater.
∆E 1 = millivoltchange in sample solutionon additionof A3.10.3Bias— The averagerecoveryofthemethod is62 to
100 µL of stockfluoridesolution,
64 % of the amount actuallypresentalthough83 to 85 %
∆E 2 = millivoltchange in blank solutionon additionof
recoveriescan be expectedwith propertechnique.
100 µL of the stockfluoridesolution,

A4. DETERMINATION OF ANIONS BY ION CHROMATOGRAPHY WITH CONDUCTIVITY MEASUREMENT

A4.1 Scopeand Application A4.2.2 InterferencesAny— substancethathas a retenti time


A4.1 .1 This method iscondensed from ASTM procedures and coincidingwith thatof any anion to be determinedwil
APHA Method 429 and optimizedfor the analysisof interfereFor. example,relativelyhigh concentrationsof low-
detrimentalsubstancesinorganicbasedmaterialsItprovidesa. molecular-weightorganicacidsinterferewith the determina tionof
singleinstrumentaltechniquefor rapid,sequentialmeasure-ment of chlorideand fluoride.A high concentrationofany one ion also
common anionssuch as bromide,chloride,fluoride, interfereswith the resolutionof others.Sample
nitrate,nitrite,phosphate,and sulfate. dilutionovercomes many interferencesTo. resolveuncertai
tiesof identificationor quantitationuse themethod of known
A4.2 Summary ofMethod additionsSpuriouspeaks. may resultfrom contaminantsi reagent
water,glassware,or sample processingapparatu Because small
A4.2.1 The materialmust be putin theform of an aqueous
sample volumes are used,scrupulouslyavoi contamination.
solutionbefore analysiscan be attempted.The sample is
oxidizedby combustionin a bomb containingoxygen under
pressure.The productsliberatedare absorbed in the eluant A4.2.3 Minimum DetectableConcentrationThe— minimum
presentin the bomb at the time of ignitionThis. solutionis washed detectableconcentrationof an anion isa functionof sample
from the bomb, filtered,and dilutedto a known volume. sizeand conductivityscaleused.Generally,minimum detect
ableconcentrationsareintherangeof0.05mg/L forF− and 0. mg/L
A4.2.1 .1A filteredaliquotof sample is injectedinto a stream of for Br− , Cl− , NO 3 − , NO 2− , PO 4 3−, and SO 42− with a
carbonate-bicarbonateeluantand passedthrougha seriesof ion 100-µL sample loop and a 10-µmho full-scalesettingon the
exchangers.The anionsof interestare separated on the basisof conductivitydetectorSimilarvaluesmay. be achievedby usin a
theirrelativeaffinitiesfor a low capacity, higherscalesettingand an electronicintegrator.
stronglybasicanionexchanger(guardand separatorcolumn). The
A4.3 Apparatus
separatedanionsaredirectedontoa stronglyacidiccation
exchanger(suppressorcolumn) where they are convertedto A4.3.1 Bomb, havinga capacityof notlessthan300 mL, so
theirhighly conductive acid form and the carbonate- constructedthat itwill not leak during the test,and tha
bicarbonateluantisconvertedtoweakly conductivecarbonic quantitativerecoveryof the liquidsfrom the bomb may be
acid.The separatedanionsintheiracidform aremeasured by readilyachieved.The innersurfaceof thebomb may be made of
conductivityThey. areidentifiedon thebasisof retentiontime as stainlesteelor any othermaterialthatwillnotbe affecte by the
compared to standardsQuantitationisby. measurement of peak combustionprocessor products.Materialsused inthe bomb
areaor peak heightBlanksare. preparedand analyzedin a assembly, such as the head gasket and leadwir
similarfashion. insulation,shallbe resistantto heatand chemicalaction,and

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shallnot undergo any reactionthatwillaffectthe chlorine contentof A4. 4. 3 Eluant Solution,sodium bicarbonate-sodi
the liquidinthe bomb. carbonate,0.003M NaHCO 3− 0.0024M Na 2 CO 3 : dissolv 1
.008g NaHCO 3 and 1 .0176g Na 2 CO 3 inwaterand diluteto 4
A4.3.2SampleCup,platinum,24 mm inoutsidediameterat the L.
bottom,27 mm inoutsidediameteratthe top,12 mm in
heightoutside,and weighing10 to 11 g; opaque fusedsilica, wide- A4.4.4RegenerantSolution1,H 2SO 4 ,1 N, use thisregen
form with an outsidediameterof 29 mm at the top,a heightof 19 erantwhen suppressorisnota continuouslyregeneratedone.
mm, and a 5-mL capacity(NoteA4.1),or nickel (Kawin A4.4.5RegenerantSolution2,H 2 SO 4, 0.025N, dilute2. mL
capsuleform), top diameterof 28 mm, 15 mm in height,and 5-mL
concH 2 SO 4 to4 L or100 mL regenerantsolution1 to4 L. Use
capacity.
thisregenerantwithcontinuousregenerationfibersuppres
sorsystem.
N OTE A4.1 —Fused silicacruciblesare much more economicaland
longerlastingthanplatinum.Aftereach use,theyshouldbe scrubbedout with
A4.4.6StandardAnionSolutions,1000 mg/L, preparea seriesof
fine,wet emery cloth,heatedto dullred heatovera burner,soaked in hot
waterfor1 h thendriedand storedin a desiccatorbeforereuse. standardanion solutionsby weighingthe indicat amount of
salt,driedto a constantweightat 105°C,to 1000 mL.
A4.3.3FiringWire,platinum,approximatelyNo. 26 B and S Storeinplasticbottlesina refrigerator;thesesolutionsare
gage. stableforatleastone month.
A4.3.4IgnitionCircuit(Note A4.2),capableof supplying Anion Salt Amount,
g/L
sufficientcurrenttoignitethe nylon threador cottonwicking
withoutmeltingthe wire. Cl− NaCl 1 .6485
F− NaF 2.2100
N OTE A4.2—The switchinthe ignitioncircuitshouldbe of a type that Br− NaBr 1 .2876
remainsopen,exceptwhen held in closedpositionby the operator. NO 3− NaNO 3 1 .3707
NO 2− NaNO 2 1 .4998
A4.3.5Nylon SewingThread,or CottonWicking,white. PO 43− KH 2PO 4 1 .4330
SO 42− K2SO 4 1 .8141
A4.3.6Ion Chromatograph,includingan injectionvalve,a sample
A4. 4. 7 Combined Working Standard Solution,High
loop, guard, separator,and suppressorcolumns, a temperature-
Range— Combine 10 mL of the Cl− , F− , NO 3− , NO 2− , and
compensatedsmall-volumeconductivitycell(6 µL or less),and a
PO 43− standardanionsolutions,1 mL of theBr− ,and 100 mL
stripchartrecordercapableof full-scale responseof 2 s or less.An
electronicpeak integratoris optionalThe. ionchromatographshallbe oftheSO 42− standardsolutions,diluteto1000 mL, and storein a
capableofdelivering 2 to5 mL eluant/minata pressureof 1400 to plasticbottleprotectedfrom light;contains10 mg/L each of Cl − ,
6900 kPa. F− , NO 3− , NO 2− , and PO 43−, 1 mg Br− /L,and 100 mg SO
2−
4 /L.Preparefreshdaily.
A4. 3 . 7Anion Separator Column, with styrene divinylbenzene-
A4.4.8CombinedWorkingStandardSolution,Low Range—
basedlow-capacitypellicularanion-exchange
Dilute100 mL combined working standardsolution,high
resincapableof resolvingBr− , Cl− , F − , NO 3− , NO 2− , PO 43−, range,to1000 mL and storein a plasticbottleprotectedfrom
and SO 42− ; 4 × 250 mm. light;contains1 .0mg/L each Cl− ,F− ,NO 3− ,NO 2− ,and PO 43−,
A4.3.8Guard Column,identicaltoseparatorcolumn except 0.1mg Br− /L,and 10 mg SO 42−/L.Preparefreshdaily.
4 × 50 mm, to protectseparatorcolumn from foulingby A4.4.9AlternativeCombinedWorkingStandardSolutions
particulatesor organics. Prepareappropriatecombinationsaccordingtoanion concen
− 3−
A4.3.9SuppressorColumn,high-capacitycation-exchange trationto be determined.IfNO 2 and PO 4 are notinclude the
resincapableofconvertingeluantand separatedanionstotheir combined working standardisstableforone month.
acidforms.
A4.5 Sample Preparation
A4.3.10Syringe,minimum with capacityof 2 mL and equipped
A4.5.1Penetrants,Developers,Emulsifiers,MagneticOils
a male pressurefitting.
A4.5.1 .1Weigh 50 g of testmaterialintoa 150-mm petr dish.
A4.4
Reagents A4.5.1 .2Placethe150-mm petridishintoa 194°F[90°C]to
A4.4.1PurityofReagents—Reagent gradechemicalsshall be used
212°F [100°C]oven for60 minutes.
inalltestsUnless. otherwiseindicated,itisintended
thatallreagentsshallconform to the specificationsof the A4.5.1 .3Allow the testmaterialto cooltoroom tempera ture.
Committee on AnalyticalReagentsof theAmerican Chemical
9
Society,where such specificationsareavailable.Othergrades A4.5.2SolventCleaners:
may be usedprovideditisfirstascertainedthatthereagenthas
A4.5.2.1Take the tareweightof an aluminum dish.
sufficientlyhighpuritytopermititsuse withoutlesseningthe
accuracyof thedetermination. A4.5.2.2Weigh 100g ofthecleanerintothealuminum dish
A4.5.2.3Placethe aluminum dishon a hotplatein a fume
A4.4.2DeionizedorDistilledWater,freefrom interferences hood.
A4.5.2.4Let the materialevaporateuntilthedishisnearl dry.
attheminimum detectionlimitofeach constituentand filtered
througha 0.2-µm membrane filterto avoidpluggingcolumns.

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ARTICLE 24,SE-165/SE-165M ASME BPVC.V-2017

A4.5.2.5Placethe dishintoa preheatedoven from 194°F of unburned oilor sooty depositsare found, discardthe
[90°C]to212°F [100°C]for10 minutes. determination,and thoroughlyclean the bomb beforeagain
A4.5.2.6Take the dishoutof the oven and allowto cool. puttingitin use.
A4.5.2.7Reweigh the dishand recordweight.
A4.6.4Collectionof Solution—Remove the sample cup
N OTE A4.3— For Cleaners—If theresidueislessthan 50 ppm, report
theresidueweight.Iftheweightisgreaterthan50 ppm, proceedwith the bomb withcleanforcepsand rinsewithdeionizedwaterand filterthe
procedure. washings intoa 100-mL volumetricflask.Rinse the wallsof the
bomb shellwith a fine stream of deionizedwaterfrom a wash
A4.6 DecompositionProcedure bottle,and add the washings throughthe filterpaperto
A4.6.1 Preparationof Bomb and Sample— Cut a pieceof theflask.Next,rinsethebomb coverand terminalsand add the
firingwire approximately100 mm inlength.Coilthe middle washings throughthe filterintothe volumetricflask.Finall add
section(about20 mm) and attachthefreeends totheterminals. deionizedwaterto bringthe contentsof the flask to the line.Use
Arrange thecoilso thatitwillbe above and toone sideof the sample aliquotsof thissolutionforthe ion chromatograph (IC)analysis.
cup. Place5 mL of Na 2 CO 3/NaHCO 3 solutionin the bomb,
placethe coveron the bomb, and vigorouslyshake for 15s A4.7 Procedure
todistributhesolutionovertheinsideofthebomb. Open the bomb,
placethe sample-filledsample cup in the terminal holder,and A4.7.1System EquilibrationTurn— on ion chromatograph and
inserta shortlengthof threadbetween the firing wire and the adjusteluantflow rateto approximate the separati achievedin
sample. The sample weight used should not exceed1 Fig.A4.1 (2 to 3 mL/min). Adjust detectorto
g.Ifthesample isa solid,add a few dropsof white oilatthistime desiredsetting(usually10 µmho) and let system come to
toensureignitionof the sample. equilibrium(15 to 20 min). A stablebase line indicat
equilibriumconditions.Adjust detectoroffsetto zero-ou
N OTE A4.4—Use of sample weightscontainingover20 mg of chlorine eluantconductivity;with thefiber suppressoradjustheregen
may causecorrosionofthebomb. To avoidthisitisrecommended thatfor
samplescontainingover 2 % chlorine,thesample weightbe based on the erationflow ratetomaintainstability,usually2.5to3 mL/min.
following: A4.7.1 .1Set up theion chromatographin accordancewith the
Chlorine Sample White Oil manufacturer’sinstructions.
content,% weight, weight,
A4.7.2CalibrationInjectstandardscontaininga— singl anionor a
2 to5 0. 4 0.4 mixtureand determineapproximateretentiontimes Observed
5 to10 0. 2 0.6 timesvary withconditionsbutifstandardeluantand
10 to20 0. 1 0.7
20 to50 0. 05 0.7 anion separatorcolumn are used,retentionalways isin the orderF −
,Cl− , NO 2 − , PO 43− , Br− , NO 3− , and SO 42− . Injectat
CAUTION: Do not use more than1 g totalof sample and whiteoilor
otherfluorine-freecombustiblematerial. leastthree differentconcentrationsfor each anion to be
measured and constructa calibrationcurve by plottingpeak
A4.6.2AdditionofOxygen— Placethe sample cup in posi- heightor area againstconcentrationon lineargraph paper
tionand arrangethe nylonthread,or wisp of cottonso thatthe end Recalibratewhenever the detectorsettingischanged.With a
dipsintothe sample.Assemble the bomb and tightenthe
system requiringsuppressorregeneration,NO 2 − interacti
coversecurelyAdmit. oxygen (seeNote A4.5)slowly(toavoid
blowingthesample from thecup)untila pressureisreachedas withthe suppressormay leadtoerroneousNO 2− results;make
indicatedinTable A4.1 . thisdeterminationonly when the suppressorisat the same
stageof exhaustionas during standardizationor recalibra
N OTE A4.5—It isrecommended tonot add oxygen or ignitethesample frequentlyInthistypeofsystemthewaterdip. (seeNote A4.5) may
ifthe bomb has been jarred,dropped,or tilted. shiftslightlyduringsuppressorexhaustionand witha fas run
A4.6.3Combustion— Immerse the bomb in a cold-water column thismay leadtoslightinterferenceforF − orCl− . To
bath.Connect theterminalstotheopen electricalcircuitClose. the eliminatethisinterference,analyzestandardsthatbracke
circuito ignitethe sample.Remove the bomb from the
bathafterimmersion foratleast10 min. Releasethepressure ata
slow,uniform ratesuch thatthe operationrequiresnotless than1
min.Open thebomb and examine thecontentsIftraces.

TABLE A4.1 Gage Pressures


Gage Pressures,atm
Capacityof Bomb, mL
mm A max
300 to 350 38 40
350 to 400 35 37
400 to 450 30 32
450 to 500 27 29
A
The minimum pressuresare specifiedto providesufficientoxygen forcomplete
combustionand the maximum pressurespresenta safetyrequirement.
FIG.A4.1 TypicalAnion Profile

630
ASME BPVC.V-2017 ARTICLE 24,SE-165/SE-165M

the expectedresultor eliminatethe waterdip by dilutingthe A4.7.4 RegenerationFor— systemswithoutfibersuppresso


sample with eluantor by adding concentratedeluantto the regeneratewith 1 N H 2 SO 4 in accordancewith the manufac-
sample togivethesame HCO 3 − /CO 32− concentrationasinthe turer’sinstructionswhen the conductivitybase lineexceed 300
eluant.Ifsample adjustmentsare made, adjuststandardsand µmho when the suppressorcolumn ison line.
blanksidentically.
A4.8 Calculation
N OTE A4.6—Water dipoccursbecausewaterconductivityinsample is A4.8.1 Calculateconcentrationof each anion,in mg/L, by
lessthaneluantconductivity(eluantisdilutedby water).
referringto the appropriatecalibrationcurve.Alternative when the
A4.7.2.1If linearityis establishedfor a given detector setting,itis responseisshown to be linear,use the followin equation:
acceptableto calibratewith a singlestandard. Record the peak
heightor areaand retentiontime to permit calculationof the C5H3F3D (A4.1)
calibrationfactor,F.
where:
A4.7.3 Sample AnalysisRemove— sample particulates,if C = mg anion/L,
necessary,by filteringthrougha prewashed 0.2-µm-pore-diam H = peak heightor area,
membrane filter.Using a prewashed syringeof 1 to 10 mL F = responsefactor− concentrationof standard/height(o
capacityequipped with a male luerfittinginjectsample or area)of standard,and
standard.Injectenough sample to flush sample loop several D = dilutionfactorfor thosesamplesrequiringdilution.
times:for0.1mL sampleloop injectatleast1 mL. Switchion
chromatograph from load to injectmode and record peak A4.9 Precisionand Bias
heightsand retentiontimeson stripchartrecorder.Afterthe lastpeak A4.9.1 Samples of reagentwaterto which were added the
(SO4 2− )has appearedand theconductivitysignalhas common anions were analyzedin 15 laboratorieswith the
returnedtobase line,anothersample can be injected. resultshown inTable A4.2.

TABLE A4.2 Precisionand Accuracy Observed forAnions atVariousConcentrationLevelsinReagent Water


Single-
Overall Significant
Amount Amount Operator
Anion Precision, Bias 95 %
Added, mg/L Found, mg/L Precision,
mg/L Level
mg/L
F− 0. 48 0. 49 0. 05 0. 03 No
F− 4.84 4. 64 0. 52 0. 46 No
Cl 0. 76 0. 86 0. 38 0. 1 1 No
Cl− 17 17. 2 0. 82 0. 43 No
Cl 455 471 46 13 No
NO 2 0. 45 0. 09 0. 09 0. 04 Yes, neg
NO 2 21.8 19. 4 1.9 1.3 Yes, neg
Br− 0. 25 0. 25 0. 04 0. 02 No
Br− 13.7 12. 9 1.0 0. 6 No
PO 43− 0. 18 0. 10 0. 06 0. 03 Yes, neg
PO 43− 0. 49 0. 34 0. 15 0. 17 Yes, neg
NO 3− 0. 50 0. 33 0. 16 0. 03 No
NO 3− 15. 1 14. 8 1.15 0. 9 No
SO 42− 0. 51 0. 52 0. 07 0. 03 No
SO 42− 43.7 43.5 2.5 2.2 No

631

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