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SE-165/SE-165M
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ARTICLE 24,SE-165/SE-165M ASME BPVC.V-2017
Standard Practicefor
LiquidPenetrantExamination forGeneral Industry
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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.
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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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ANNEXES
(MandatoryInformation)
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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
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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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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:
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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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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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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.
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