Liquid Penetrant (Lev1el-I-level - II''

7/22/2019 Liquid Penetrant (Lev1el-I-level - II''

http://slidepdf.com/reader/full/liquid-penetrant-lev1el-i-level-ii 1/100

UNIQUE TECHNOCR.ATSSCHOOLOFNON.DESTRUCTIVETESTING& WELDING

LISUID PENETRANT ESTING

LEVEL I/LEVEL-tr

S.H.DESHPANDE

ASNTLE\IEL_M

REGD,OFFICE:

UMQUEIECHNOCRATSNO.47,P.O.BO)CO.9153,MACIADIROADSIINKT{DAKATTEMNGALORE-56009IPILNO. 0t0- 3489140?1td6.59.FAX: 080 34853?4'



_=/a l_ONIOOE

Liquid Penetrant nspection s a non{estructivo method of revealingdiscontinuitieshatareopen o thesurfaces f solidandnon-porous aterials.

Liquid Penetrant nspectiondepends mainly on the penetrantefectivelyWEfnNG thesurface f the test objec{,FLOWINGver he surfaceo formacontinuouslyniform oating,SEEPINGapidlyntocavitieshatareopen o thesurface ndefiicientlyettingBLOTTED UTof thecavityoforman ndication.

A simplistic escriptionf the LiquidPenetrantnsp€ction rocoss an be asfollours:

A tiquid, suallyRed calledPENETMNT)s appliedothe estsurfaceo formauniformayerover he surface.Adequateime s providedor the penetrantoseep ntocavitiespeno thesurface.A suitablemethod fcleaningCLEANER)is used o remove nty heexcess enetrantefton the surface.Then he dyethathasseepedntodiscontinuitiess madeocome ut& forman indicationnacontrastingackground.calledDEVELOPER]he evaluationf th€ ndicationsso obtainedan evealotof usefulnformationbout he estsurface.

Themainadvantage f the test s its simplicity nd its applicabilityo a wide

variety f situations.Themainimitationf the est s itsapplicabilityo only thosedefectsopen hesurface.

EVOLUNON FTHEPROCESS

vv|renKerosene as made o flow on a iest surface, erosene ntered hecrevices pen o the surfaceand the excessKerosene ither lowedout orevaporated. heapplicationf wtritewashprovided contrastingackgroundagainstwhictr re Keroseneromthe oponingsmadevisual ndication. The

sensitivrtyf the procees ouldbe increased, y hitiing he test surfacewith ahammer.Theresultingibrations roughtmorekeroseneutof thecracks ntothewhiteuiash.Thisproc€ss ascalledOil& \Mriting"method. mprovementsof hismethod ausgdhedevelopmentf LiquidPenetrantnspection.

Page of21



PENETRANTESNNGIATERIALS

Followingre hecommonmaterialsequiredorpenetrantesting.1. PENETRANTS/DYE2. EMULSIFIER3. SOLVENTCLEANER/REMOVER4. DEVELOPER

Dependingn hedlaraeteristicsf theabovematerialshoserr, widevariety fpenetrantests anbedefined, trich resuitedor differentetof circumstances.

PENETRANTS

Thereare no basic ypesof penetrants-FLUORESCENTenetrantsVISIBLEenetrants.

A thirdcategory f penetrantalledDUALSENSITIVITY"enetrantsre alsoavailable.hesepenetrantsre suited or use,bothwith visible& fluorescentmethods.

The aboveclassifications basedon howthe oenetrantndicationsre seenduringnspection.

Another lassificationf p€netrantsanbe madebasedon themethod sed orexcess enetrantemoval. heyare

WATERWASHABLEenetrantsPOSTEMULSIFIABLEIPOPHILICenetrantsPOSTEMULSIFIABLEYDROPHILICenetrantsSOLVENT EMOVABLEenetrants

FLUORESCENTsn€tranttilisss enetrantshatareusually reenncolour ndfluoresceshine) rillianfy nderUltravioletight blackight).

Thesensitivityf fluorescentenehantsependsn itsabilityo form ndicationsthat app€aras smell sourcesof light n an othenrvisearkened rea. Thesensitivity f thesepenetrantmethodsare easilyaltered by the natureoffluorescing dditives dded o thepenetrants.

VISIBLEPFNETMNTutilisesa perietmnthat is usualty ed in colourandproducesharply isible ed ndicationsn contrastothe ightbackgroundf he

Page2 ot 21



wlilooE

developernder isibleight.Thesensitivityf thesepenetrantsreeasily ltered

by changinghe dyre oncentration the natureof thedye.

PEN TRANT HARECTERISTICSAll penetrantmat€rialEhould have someciharacteristicso make hemgoodpenetrants.

* Chemicaltability unificrmonsistency" Goodv'iettability* LorrViscosity* Sufficient righhess* Chemicalnertnesso containers testmaterialg

' Sloirrdryingcharacteristics" Easeof removal* lndfensive Odour* LowToxicity" Resistanceo UV ight& / or heat" Low@st' High oleranceopossibleontaminants* High lashpoint

EMULSIFIERS

Emulsifiersre iquidshatmake heexcess enetrant aterN€shablendhenceaid the processof excesspenetrantemoval.Theseproducts re extremelyusefulwhen esting f largeno.of intricate arts.The surface enetrantemovalprocessanuld e madeesscr.rmbersomecomplete.

There re vroypes femulsifiers1. LIPOPH]LIC and 2. HYDROPHILIC

LIPOPHILICmulsifiers re essentially il basedand work by diffusingntoexcess enetrantmakingt washablen water. The emulsificationction s fastand continues s longas it is in contac{with exc6$s enetrant.Therefore,he

rinseoperation houldbe quicklycompleted.The timefor emulsificationsdependentn theparticularmulsifier,ts concentration,mulsificationate, estpiecesurface ondition tc, andhencacannotbe a fixedvalue.

IT IS, ALWAYS PREFERABLE O FIND EMUL$IFICATIONIME BYEXPERIMENTATION,

LIPOPHILICMULSIFIERSre usedas supplied ndgetcontaminatedy water&pefietrart

Page of 21



HYDROPHILICMULSIFIERSreessentiallyater ased ndaresupplied s

concentrates. heeeare dilutedn waterbeforeuse. 530016oncentrationsusedbr dip applications.0$'5% oncentrations used or sprayapplications.Hydrophilicmulsifiersc{by detergent ction.e.,bydisplacementfp€netrant.Hydrophilicmulsifierc re slowactirrg& hence,norfrallyadequate mulsificationtime E available.Normally, re+insing ith coar$ewater s done o reduce'emulsificationtimeandpenehantontamination'.

Penetrant anufacturersormallypecify ominal mulsificationimesor specifictypesof emulsifiersnd heconc€nfationn wttich heyaresupposedobe used,Houpver, t uould be still advisableo determinehe emulsificationime byexperimentations emulsifiercontaminationan alter the emulsificatior,characteristics.

SOLVENT LEANERREMOVERS

Solvent leaners re chemicalghatare used o remove xcess enetrants,urtheyact by Direc* olvent ction.Excess urface enetrants cjissolvedy thesolventdeanerwhen appliedusingslightlymoistenedint free cloth I cottonwaste. Flooding he surfacewith excessive leaner ncreases he risk ofpenetrantrom within the defectsalso gettingdissolved. This will makeindicationsisappear.

Solvents reclassifiednto2 types

FLAM[,IABLENON- FIAMI\,IABLE

- FREEOFHALOGENS- HALOGENONTAINING

Halogenatedolvents ave he advantage f beingnon-flammable,ut are notacceptedncertain pplicationsfisrepresencef halogens ouldbe harmfulothematerials f testobject.

DEVELOPERS

The pwposeof the developers to increase he visiblecontrastof visiblepenetrantndicationsn normalvisiblepenetrantostingand to increase hebrighhess f luoreseentndicationsn luorescsntenetrantesting.Developers a oitical partof the inspec{ion rocess. A gooddevelopersrequir6do havemany haracteristics,uchas,

" it mustbecapable f providing contrast ackgroundin colour ontrast enetrantesting.

Page4 ot 21



- it mustnotpmducets ovwrluorescence

to theoperator.

penetranttom a defect.* it musthavea goodblotting ction.* it mustbeeasy o r€move fler nspedion

Generally, ll ihesecharacteristicsre presents varyingdegrees n variousdevelopers.Hence, t is possibleo get different ensitivity sing differentdevelopers.

There re4 tlrpes f developersgmmerciallyvailable.

1. DryPouder2. WaterSoluble3. Water uspendible4. Non-aqueoussolventsuspendible

1. DRYPOWDER

These remorewidely sed nfluorescentenetrantesting.Theyarenotgenerallys6dwithvisible enetrantesting s theydo notproduce oodcolour ontrast.

Dry developers houtdbe light& tlnffyand non-hygroscopicor goodusage.Theyshould ling o thesurface f the estobject s a thinuniformcoating.They are normally riedby heatingo remove roisture. Thisrestoresheirability o dustuniformlyndavoids lumpingiumping.

Handlingf drypouderss to be donewithcar€as t cancausedryskin&respirationroblems.

Prolonged xposureo drypowder

pplication ayrequire seofglove,espiratorsparticleiltration quipment.

Drypovldersan be applied y dipping, loudinghe.surfacen a dustyatmospherer by fog chambers.

Page5 of 21



4.

WATERSOLUELEDEVELOPER

Thesedevelopers an be used with all types of penetrants xceptwaterwashablepenetrants, Slight excess developerapplicationcan causedefect penetrant o be washed away in the case of water washableponerants.

Water-solubleevelopers re available s drypowder oncentrate,/hichcanbe digsolvedn water. Onapplication,he pov\derecrystallisess aunibrmdeposit s the waterevapqrates.Usually, 12- O.24Kg/L s thebathconcentration,rhich n be convenientlyheckedwith a hydrometer.

Advantagesfri/ater-solubleevelopers re

i) Theydo not require ny bathagitation.ii) Dryng of components rior to developerapplioations not

necessary,nd1ii) Post leanings veryeasyaswaterwashingsadequate.

WATER USPENDIBLEEVELOPERS

Thesedevelopersan be usedwithbothvisible& fluorescentenetrants.Theyare supplied s drypo'ader oncentrate.Usualbathconcentrations

are 0.O4 0.fZ lQlL. Particle oncentrationan be checkedwith ahydrometer.Watersuspendibleevelopersan be applied efore ryingcompsnents. Mrq of thecomponentfterdeveloperpplicationanalsohelp aidpenetrant leedouts romdefects/crevices.

Normatly,onoslonnhibitors, ispersing gentsand weitingagentsareaddedn developerso improveheirperformance.

NON AQUEOUSOLVENT,SUSPENDIBLEEVELOPERS

Thesedevelgperc,heR sedwith luorescentenetrantsrovidehe bestsensitivig. Thesedevelo'persre commonly sed for both visible&fluorescantenehant rooess. Theycontainparticles uspendedn amixlure f volatile olvents ith suitable ispersantso keep he particlesfromsettling.Theyproducehe highest ensitivity,s the volatileiquidstend to enterthe crevices, ilutethe penetrant& help bleedout ofpenetranty ncreasingtsvolume.

Page6 of 21



--:/a l-(|HTOOE

SELECETK'NFPENETRANT ETHODS:

Having ndorstoodhevarious enetrant aterials,t is now mportanto be ableto selectanappropriate€netrantestingmethodora givenapplication.

1. Thesize, hape,weight vork pieces, o.ofpiecesobe eeted,equiredsensitivity,vailableacilities, urface onditionf the estpiecas tc.,areall adorcwtlicfi nffuenceheseledion f a proper enetrant ethod.

2, Cost,sensitMty $ired, naturoof d€fects eingsoughtandoiticalityoftestingalso nfiuenceshe seleciion f apenetrantmethod.

The fotlowing fiartgivesus variougoptionsavailableor penotrantmethods,

basedon various nput ngredients.

Various combinationsof ponetant materialsyields various penetrant estmethods,nd,dependingn thecombinationhosen, ensitivity chievable ayvary. Because f the difficultiesn quantiffing ensitivitynd the possibility fdifferentsensitiviti$ within a partio.rlar ombination,t has been he practice ospeclfya test methodcomblnafon and insist on a written procodure orperforming h6 tcat

yvhilet is notnece$ary o individuallyescfibehevarious ombinations,t iraybspertinento eam eurspecificdvantages limitationsf differentmethods.

1. Mshle pene$antsre utilised rimarily r localisednspection hereasfluorescer*enefantsend hemselvesasllyo mechanisedlargescaleinspeciion.

Z. Highest ensitivities re achievablen post - emulsifiableluorescentpenetrantrcpoction withhydrophilic mulsifiers).

PENETRANT EMULSIFIER CLEANER DEVELOPERVISIBLE L "flLtc WATER DRYPOWDERFLOURESCENT HYDROPHILICHALOGENATED

SOLVENTWATERSOLUBLE

WATERWASHABLE HALOGEN-FREESOLVENT

WATERSUSPENDIBLE

POST-EMULSIFIABLE NON.AQEOUSSCLVENTSUSPENDIBLE

SOLVENTREMOVABLE

PageTof21



3, Solvent removablefluorescentpenetrant method is ideal for spotinep€ctionrwhereu/ater snnot econvenientlysed.Whenadequatecare ia taken, his method s as s€nsitive s the post - emulsified

f uqf€scentpenetrantmethod.

4. Waterwashable luorescentpenetrantmethodsare the fastest. Overueshingsthemost requentause f ossofsensitivitynthismethod.

5. Solvent emovable isiblepenetrantmethodsare most versatileandportable. This methodcangive goodsensitivitywhenadequate are istaken npenebentemoval.

6. Wateru/aEhableisiblepenetrant

methods re fastest,butprovide

eastsengitivity.They are very usefulwfien shallow& wide defectsare notsignificant.

7. Fluorescent enetrantmethodsoffer higher sensiiivitieshan visiblep€n€trantmethods.

PENETRANTESTING QUIPMENT

Theequipmentsed n Penetrantnspectionariesromsprays, erosol ans ooomplex utomated,ornputer ontrolledystemg.Houover,even he automated

linesarebasicallymaterial andling ysternsor coneclhandling f componentsproviding ccuratoimesof penetrant pplication, uell time,penetrant rainout,excegspenotrant emoval,washing,drying,developerapplication, rying.lnspedionetc.

PC}RTABLEQUIPMENT

Most requently, enetranlnspections caniedout n thefield n betvrreenariousprocessingtages o identify efec.tsevelopedue o theprocessing.This helpsin etiminatiqrof these defsctsb€fore urthsr processing/sortingut defectivecomponeqtsrom urtherprocassing.

Portabilig s a very importrant riterion n field inspection. Variouspenetrantchemicalsreavailablen spraycansor aerosol ans or easyportability.E','enUltravioletamps black ampsare designed o bepacked nto compact ortablekits.

Page8 of21



_:/a l_olttQoE

'

Pre-cleaner, enetrant, enetrant emoverand developer, ll in spray canswith

adequateint ree doih / paper o\ryelsor?n standardpeneirant it. Black ight san additional ool for fluorescentpenetrant esting.

STATIONARY ENETRANTNSPECTION

The type of equipmentmost frequentlyused in fixed installation onsistsof aseries of modular anks designedspecificallyor a particularpurpose. Thevarious tations re

1. Gleaning tation2. Penetrantstation

3. Drain dwellstation4. Emulsifiertation5. Pre& postwashstation6. Dryingtation7. Developertation8. Inspection tiaiion

Usually,a drain / dvuell tation s positionednext to each dip tank to provideflexibility f time.

CLEANINGSTATION

Pre-cleaningof uork pieces prior to penetrant nspection s very imporiantbecause onlaminantsi) mayprevent he penetrant romentering he laqii) mayalter hephysical roperties f a penetrant, r,iii) may nterferewithproperexcessperEtrant leaning.

Precleaning s nonnally chieved hemically,mechanically r by usingsolvents.

Chemical leaning ncludesalkalineor acid deaning,pickling,chemicaletching,

moltensalt bathcleaning tc.

Mechanical leaning ncludes umbling,wet blasting,wire brushing, ighpressuresteamcleaning, ighpressurewatercleaning tc.

Solventcleaningmethods ncludes vapor degreasing,Ultrasoniccleaning nsolvents, olvent praying wipingetc.

Page oI 22



Onemajor actor o be consideredn selection f the cJeaning ethods that he

method hould llcndefectso remain pen o thesurface ithouteavingresidues, trichnterbrewith srbsequent rocessing.n order o achieve heaboveobjective,more hanone of theabovemethodsmay be requiredo beusedorpre-cleaning.

Sincepre-cleaning ethods hangevery widely,design of the pre-cleaningstationmayalsovaryverywidely.

PENETRANTTANON

The principalequirementf a penetrant tiations to providea coatingof

penetrantnd have acilityo cover hepenetrantl hennot required]o avoidevaporation contaminationnd o collectheexcess enetrantrainout. Drainplugsare normally rovidedo help drain he contentsor periodic leaning.Coating f the perntrantmay be accomplishedy dipping, praying singairgunsor using electrostaticprayguns. An 'expendable"techniques alsofrequently mployedwhereno effort s made o collect he drain out wheneconomiesf operationermil.

Normallypenetrant ontainers re made using galvanized teel, but maysomelimese made sing tainlessteel, specially henwaterbasepenetrantsarestored.

EUULSIFIERTATION

Emulsifieranks are used for dippingpenetrant-coated,omponentso helpremove xcess urface gnetrcmtas n he caseof lipophilicmulsifiers)rspraystationswith coarse spray to removeexcesspenetrant as in hydrophilicemulsifiers). mulsiticationimesare normally stablishedy experimentationoreachnatureof components.

PRE& POSTRINSINGTATIONS

Pre- insing ormally recedesydrophilicmulsificationnd s accomplishedycoarsewatersprayusinghandheldsprayguns. Thewater& penetrant,incetheydo not mix,canbe allotr,r€do separate ut n settlinganks, eclaiminghepenetr€nt.

Post rinsingnormally ucceeds mulsifier pplicationnd is accomplishedyscrubbing ith coarsewatersprayusinghandhelpsprayguns. Wash roughshould e suitableo turn he componento cleanall surfaces.Normally,plash

Page 0of 22



shieldspreventhe conlaminationf neighboringenetrant, mulsifier developer

tanks. Rinsestations re alsoeguippedWthoneset of Ultravioletightso that heprogressof removalof fluorescentpenetrantcan be assessed.Since ot of lvaterwill be in contactwith the tank material,stainless teel s theprefened ank material, romconosion resistancepointof view.

DRYINGSTATION

Re-cifculating ot air dryers are the most popular or drying of components.Electricelements, teamand hotgas are the variousheatsources. Eitherbatchtypeor conveyorype dryerscouldbe designed o suit he componento bedried.

DEVELOPERSTANON

Develqperstation s locatedafter lhe drier stationwtren dry developersare useo.\t1/|en dipping is used, the excoss po,rder is shakon off before ailowingdevelopment. A/trenarge est articlesare to be locallydeveloped,a scoop sused for throwing he pouder over the surfaces. Dry developers an also beapplied n fog chambers r usingelectrostaticplayguns. Suitabledust control&ventilation nangements ave to be madeto see that no respiratjondifficultiesariss.

When wet developersare used, the developer station should be locatedimmediatelyefore he drier. Therewill be a provisiono store he componentsafter dipping n developer o allow drainbacJ<f developer.

In case of water suspendible evelopers,t is n€cessary o stir the developereitirerusingpaddlesor pumps o keep the developerparticlesrom setfling. Incageof water-solubleevelopers, osuchseparate rangement s required.

INSPECTION TATION

It isa rcrk tablewlrere estpiecescanbe thoroughlynspected nderaF,propriate

lightirg after developing. In case of visiblepenetrantnspection,t has to beilluminatedwith white light of adequate ntensig, and in case of fluorescentpenetrantest, t has o be illuminated ithblack ight andprovidedwith a hood oblockwhite ight tom nspecdionrea. Goodair-circulation as to be providednthisarea o lirnitdiscomfttureue to heat.

The abovedesoiptiondescribeshe variouszuFunits of a mechanised vstemand he specific ystemwillconsistof various ombination f the above o suit thepafticular rocess equirements.

Page 1of21



-VAEZ-oNtooE

PROCESSINGARIABLES ORTESTING

Having iscussedhe various enetrantariables,ossible ombinations theeguipmentequiredo cany out the test, t is irnportanto learnsomeof theimpoilant roc€ssingariables, frich ffed est& test esults.

SOLVENT EMOVABLEIETHOD

1. A typical equencefprocessingsgivenbelow

Penstrantan be appliedby brushing, ouring,Bwabbing,ipping r bysprayingAllmethods re acceptable.

It is goodpradice o allortrhepenetranto drainafter he entiresurface scoveredwithpenetrantather hankeep t dipped.

Heatirg omponentsrior o penetrantestings notrecommendedue opossibleolatiliaation.

Ihrell imedepends ntheviecosity& surfaceension f thepenetrantits contad anglewith the inspe<iionsurftace. The longestdvr,ell imeacceptables the time it takes for the penetrant o dry on the surface.lf thepenetrant ,ere o dry,p€retrarilshouldbe ra.applied ofore urtherprocessing. Optimumdlvell times have to bo establishedor eachpenetrant. ormostp.rposes, 0mins.To 30 mins.wouldbe optimum.

Page12 oI 21



6. Solvent hould everbeused n excess s t willdissolvehepenetrantn

the defeclsmakingndications isappear. t is necessaryo apply hesolvent sing clean, int teematerialmoistenedith he solvent.

7. Dry porarderevelopers re not recommended ith visiblepenetrant

soivenlemovableombinationue o reasons f lowEensitivity"

WATERWASHABLEtIETHOD

1. Atypical equencefprocessingsgivenbelow

Wder washablemethodwithvisiblepenelrantss a very low censitivity

method. Water washablemethodwith fluorescentpenetrant s quitepopular.

considerationsn determinationfpenetranttlEll imeare hesame s or

solventemovalmethod.3.

Page13of21



-va l-(|1{to(IE

'

4. Overwashings the majorprobl€mn waterwashablemethod.Optimum

rinsing onditions re bestestablishedy observinghe specimen nderblack ightuntil he luorescent ackgrounds removed atisfactorily.

5. Rinsings normally onearound 0 psi pressure f waterwhich s @ 10-40" C. Whenair s mixedwithwater or spraying, ir pressurehould otexceed 5psi.

6. l/Vhen queous evelopers re used,drying s required fter developerapplication. Mren dry povrder nonagueousdevelopers employed,dryingetrculd epior to devetoper pplication.

7. Nominalinsingimesmaybe 1f2min. o2 min.

POST EMULSIFIABLElETHOD

1. A typical equence f processings irdicatedbelow or both ipophilichydrophilicmulsifirapplication.

Page14 ot 21



woNlooE

2. Considerationsn determinationfpenetsant\ Ell timeare hesameas or

solvent emovablemethod.

3. Pre-rinsingo partly emove xcess enetranto minimise ontaminationf'emulsifiers @mmonn emulsifierpplication.

4. $irnultaneous pplication f emulsifiero afl surfaceso be inspectedsvery important. hile spraying& dippingare acceptable, rushingofemulsifiers banned. his svery mportantspeciallyhenusingipophilicemulsifier.

5. Emulsificationimeshould e determinedyexperimentation.

6. Considerations xplained or \^rater vrashablemethod' regarding'developerapplication' 'dryrngcyde'apply o post-emulsifiableethodalso.

7. Developingimeof 10 mins. s normallydequate, utshould e strictly sspecifiedn specifications,f any.

INSPECTION

1. First step in the inspection f penetrantests is to ensure hat theprocessingonditions pecifiedntheprocedure readequatelyolloived&theresufts fprocessingre satisfactory.

2. Availabilityf proper ightings a very mportantactor n the inspectionstage.

a) Sufficientwhite light shouldbe pres€ntfor visible penetrantinspedion.Lightntensitys many imesspecifiedn specifications.Typical alue500LUX 50 Footcandles.

b) Sufficient arknesa black ight ntensity houldbe availableorFLOURESCENTENETMNTNSPECNON.

Typicalalues: 1@0-1500Dw/cm2 tack ight intensity tinspection nface.20 LUX 2foot candles)max. or darkness.

Page15 of21



EVALUATIONVWtat,8 seewhenwE nsped hesurface nderproperconditions re ndications(except or badqground) ln penetrant esting, the penstrantseen on theinsp€ciionurfaces the ndication.NDICATIONSan henb€ ermed sFALSENDICATIONS

Examples1 Excessiveackgroundltrorescen@n luorescentenetrantest.

Possibleause: nsuffcient leaningdevelopercontaminationithPenetrant.

2.Fingermarks

Possibleause:Penetrantnoperatofs ands.t is veryimportantoavoidpenetrantn nspectiontable, eveloperontaminationadequatepenetrant eaning o avoid FALSE]NDICATIONS.

IRRELEVENTNDICATIONS

Theyare ndicationsaused y some eature f designof thecomponentnownto oxist.

Examples Press-fit arts,bolted rivetedoints,scaleon rolledplatesurface.Roughsurface n a casting forging.

TRUE RELEVENTNDICATIONS

lndications trichare not FHSE / NON-RELEVANTre TRUE NDICATIONS.TRUENDICATIONSbove pre-specifiedizeareRELEVANTndications.

RELEVANTNDICATIONSanb€of tvrro)/p€s.ROUNDEDNDICATIONSLINEARNDICATIONS

Theseare normallydefined n speciftcations.Also, the accepiance riteria orrelevantrdicationsregivennSPECIFICATIONS.

Page16of 21



w ii-m-oEE

It is mportantonote hatacceptancereiections basedon |NOICATIONIZE&

noi on Ff-qW SEE. Thereforb,Une on'trol f processing yclereguired o getconec;tnterpr€tationannotbeover-emphasized'

POST€LEANINGAfter Ins9ec-tion, ost-cleaningmay be r€quired o ascertain hat penetrant

;;&;b-d" #t int"rf"r" wiih su6sequentprocessing. Most specifications

requirethatpostctewrirrgequiramontsrEgiven n NDTprocedures'

QUAUTYASSURANGEFPENETRANT ATERIALSFu-tpo""of.OU"lityAssttance s to ensurehatthe regultsof the test aretrueto

th"'pot*ti"t of

-trsteet method and have not deteriorateddr-re o faul$

irpfirent"tion of proceduresrdeteriorationf penetrantawmaterials.

lmplementationf proceduress controlledby rigorous raining,qualification&

""hin*tionof peisonnel employed,establishirg lwitten proceduresstating

various afiablei o Oeusedandperiodice+rtification of personnel'

Deteriorationf Penetrantawmaterialsare ctreckedby comparison f.cunent

p.tro*"n"" against awptable performance y a referencestandard n the

iesting fa REFERENCELOCK

Various est blocksand m€thods f comparisonf samplesare specifledn

standardsspecifications,he mostpopularof wttich s theCRACKED LUMINIUI ELOCKMATL. 2024T€ ALUMIN]MUMIZE2"WDEX1TLONGX WATHK

SKETCH

Tl-

+fI ,'1u'

ll_l*- i -.{ lr---+te'

Page17 t21



:v-(|NIQOE

Sucha block,Wlenheatedo approx'650:Fi19 queno\odn waterprcduces

uncontrolledracr pattems;Ifiil" width& depirr' This ig useful or high

seneitivity roceduree.Rt--had;;o-d0 r proaucewidercracks'whichare

usefulor loivsensitivity rocedures'

Theperformancef any vo testmethods anytuloponetranta\Mmaterials an

be assessed YGompanson'

PHYSICALROPERTYEFUFICATION,OI'IPARISON

$ome knom physicalproperty^ofhe penetrartctremicals verifiedby a

standardisgdrocedure, c[n-trilquality& penetrantmaterials. uchtestsare

WATERCONTENTTESTMENISCUSTESTCERAII,IICLOCKTESTvrsoclwrEsrSPECIFIC RAVITYTESTir-uonescencEADEEsrWATERWASMBILITY EST

Thesetestsaredescr ibedinstandards&tectrn ica|pubt icat ions.ThesanJnJJri d io||"rto utren rese testsarerequiredo becaried out

RECORDINGFRESULTS

Thisest oesoteavenv ermanentqcgoJu9.ffo';,ilT,1t;"1,:ffi""tjJ;iir*rL-r" lo haveperman-entecordof indicati

requirements"v n r"fiyu drd or, i" t"iturenveitigationsin - service

inspection tc.

,1. PHOTOGRAPHY

BI-ASK&WHITE coLouR Photographyancreatea permanent€cord'Polaroid notograPis n provioeritantineous records fobservation'

2. PLASTIC ILITI EVELOPERS

Specia|@velopershavingp|asticconstitrerrtareavai|ab|e'wtricttfixthepenstrflt inOications'-Gse developers anbe peeledoff & storedwith

ProPerdentification.

Page 8of21



-S/4E4.(|lilo(|E

3. STRIPPABLEACQUERS

Three o six ayers f lacquer anbe sprayed n the developedurfaceswhoseecords desiredobekept.Afterdrying,hese anbe ifted irecflyor usingransparentellophaneapeso orma permanentecord.

TYPESOFDISCONTINUITIES

In ordero be able o evaluatendications,t is necessaryo havean ideaof thevariousstagesof processinghat a materialundergoes nd the natureofdiscontinuitieshatare relevanto thosematerials nd theproc€ssingnvolved.An nspectorerforminghe estshould e able o makea judgementf the ypeof ndicationsoexpec{ henooking t thecomponent.

DISCONTINUTIESanbedividednto hreebasic ategories.

INHERENTPROCESSINGSERVICE

INHERENT iscontinuitiesre those discontinuitiesresent n the originalproduc{ionf metal alloydue o henature fproduction.

Processingiscontinuitiesre thusediscontinuitieshatare formeddue to thenatureof procsssingmatefalsundergo casting,uelding, orging, ormingoperationsikebending,olling&extrusion, achining,eat reatment,[latingetc.

servicing iscontinuitiesrediscontinuitieshatare ormedwhenmaterialsre nservica cDnosion,atigue, rosion tc.

DISCONTINUITIESRENOTALWAYS EFECTS, HEYBECOME EFECTSONLY /V}IENTHEYARE IDENTIFIEDS RELEVANT AREKNOWNTO BELARGERN SIZETHANWHAT S CONSIDEREDCCEPTABLEORGIVEN

APPLICATION.

Page 9of21



-=/A l-OHIOOE

TRANING& CERTIHCANON

ln order o help the industryn anivingat a uniform evelof knoWedge&understandingf the test method American ociety or Nondestrucliveestinghasbrought uta docum€ntitledSNT-TC-1Afiich sa recommendedraclicefor Training Certificstion.

The ebovedo@ment s to bo us€d as a GUIDELINE Y EMPLOYERSnestablishingVi/RITTENROCEDUREORTRAINING CERTIFICATIONFN.D.T. ERSONNEL.

ASNThas dentified levels fqualifications

GENERAL,PECIFIC; RACTI'CALSGENERAL,PECIFiC, RACTICALSBASIC, ETFIOD,PECIFIC

LEVEL ILEVEL IILEVEL_II .

LEVEL | is the o'n€stevelof qualification is meantor personnelo performtestsandevaluateestsasperwritten rccedures.GENERALLY,ODETAILEDKNOWLEDGEFCODES, TANDARDSSPECIFICATIONREEXPECTED.It is expecfedhat fie person s trainedenough o workwith a pre-approvedprocodure rovidedohim.

LEVEL ll is the evelofqualification,here n additiono LEVEL I , knowledgeto set up & calibrate quipment, nterpret& evalu€te est rosults n accordancewithcodes,standards specifications, reparew'ittenprocedures report estresultssnecsssary.

LEVEL lll ie the highestevelof qualificationn eachmethod ndrequires nability o estrbtish eclrnique, eleclappropriate .D,T,method,and train &qualifyNDT Level I & Level ll personnel.n additiono Level | / Level llknotflledge& tmdions, he should also have broad based back ground inEngirnering,ecfrnologymaterial rocessingo beable o assist n establishing

acceptanceriteriawhersnoneexistl.

AS.N.T. presently onduds he BASIC& METHODEXAMINATIONSn 12DIFFERENT DT methoG & leaves he $PECIFICH(AMII{ATIONo theemployer.LEVEL I & LEVEL ll training, t€mination& certificationre efttobe contludedby LEVEL lll as detailed n theurittenprocedure f theemployer.

Students rca&ieed o study ho SNT-TC-1A odmentpublished yASNT.

Page20 of 21



LIQUIDPENETRANT TANDARDSS PERASMESEC.V

GENEMLREQUIREMENTSLIQUID ENETRANTXAMINATIONSTANDARD EST METHODFOR LIQUIDPENETRANTEXAMINATIONSTANDARDEST METHOD OR LIQUIDPENETMNTEXAT\4INATIONSTANDARD TEST METHOD FOR FLUORESCENTPENETRANT EMMINATION USING THE WATERWASHABLEROCESS.

STANDARD TEST METHOD FOR FLUORESCENTPENETRANTEXAMINATIONUSING THE SOLVENTREMOVABLEROCESS.STANDARD ESTMETHODFORVISIBLEPENETMNTEXAMINATIONUSING THE SOLVENTREMOVABLEPROCESS.STANDARDTEST METHOD FOR SULPHUR INPETROLEUMRODUCTSSTANDARD EST METHODFOR SULPHATEON INWATER.STANDARDESTMETHOD ORCHLORINEN NEW&

USEDPETROLEUMRODUCTS.STANDARD TEST METHOD FOR SULPHUR INPETROLEUM PRODUCTS (HIGH TEMPERATUREMETHOD).

ARTICLE -ARTICLE -ART]CLE4

sE-165

sE-1209

sE 1219

sE 1220

sE 129

sD 516

sD- e08

$D 1s52

Students re advisedo understardhe abovestandards o that they could eferthes€ tandardsffciently uringheircare€B.

Studyof similar tandards y otheragencies illenhanceheirunderstandingfthesubjedand srecommended.

Page21 of 21



sFc oN6. NIn,Fc l l ( )N nWs ) l .1 /D1.1M:2002

Table6.1

Visual nspectionAcceptanceCri ter ia see6.9)

'l'ubular

Connections

Discontinuiry AII Loads)

(l) Crackcrack hallbe ofsizc or local ion.

(2) $tld/Brsc-l\tctrl l'usi0n

Thoroughirsion hallexist ctween djaccntaycrs f$ eldnletal ndbctwccD cld nctal

andbasemctal.

(3) CraterCrossSection

All cratenshatlbe illed o providc hespecifiedveld izc,exccpt or thccndsof

intcrmittentilletweldroutsidc f theireffectivccngth.

(4) Wrlr l I ' ro l i lo$

Wcldprol i lcs hal lbc n conlbrnrnncc it l 5.24.

(5) Tlmeof nspectionVisualnspcctionf wcldsn allstccls ray cgir nrrncdiatcllf tcr hsconrl lctcd clds

havc oolcdo ambicntcmpcrnturc-cccptanccritcriiror AS M A 514,A 5 7,attd

A ?09Cradc 00 nd 00 W stccls hall cbascd nvisualnltpcctioncrli)nlrudot css

thrn48hours fter ofthe eld.

((r) Undcrsizcd flt ls-l

hcsizc fa fi l lctwcld n any onlinuouscld niy bc csshrrnlc spccil icdxrntirtal

size L) withoutcorrection y thc otlowing mountsU):

L, U.

spccif icdomiualrvcldizc.n. mm] allowableccrclscromL. n Inrtnl

< 3/r6s]_ l/4 [6 ]

> 5/16 8]

< l / 6 ? ]< /32 2.s]s l /8 3l

In a l l cascs.hc undcrsizc ortion f thc t cld shal lod cxcccd 0')i 'of thc $'cLl cugth.On wcb-to-flangewclds on girdcrs,undcrmnshall bc prohibitcdat thc cnds for a lcngth

cqual to twicc thc width of rhc

(7) Undcrcut(A) l.'ormntcrialcss han in. 25mm] hick. ndcrcuthall otcxcccd/32 n. l mm],

with tlrc i,lk'winll cxccnrion: UsfggllEl]-lllgscd l/l{r in. 2 mrnl itr q1

accumulatcdcngth p 2 n. 50mm] nony 2 in.1300 ml. ior natcri:rlqurl oor

grcatcr han I in. thick, undc.cut shall not excced / I6 in. [2 mml for any lcngth of wcld.

(B) tn primtry membcrs, ndcrcul hal lbc no morc han0.01 n. [0.25mml dccpwhcn

thc wcld s t ransvcrsco tcnsi lc t rcss n<Jcrny dcsign rading ondit ion tJndcrcul hal l

bc no rrrorc ltrtr /12 in. l r rrrn l { ) r n l l o lbcr c:rsus.

(8) I'orosity(A) CJPgroovc elds n buttjoints ransverseo thedircction f computedensile lrcss

shallhavenovisiblepipingporosity, orall othcrgroovewcldsand or fillet *clds, the

sumofthe visiblepipingporosity /32 n, I I mmJor greatern diamctcr hallnotcxcccd

3/8 in . [ l0mml inany l inear inchofweldandshal lnotexcecd3/4 in . [20mm] inany l2 in .

[300mfn] ofweld.

(B) The frequencyofpiping porosity n fillct welds shall not cxcecdonc in cach4 irr

L l00 mff l of weld ength nd he maximumdiamctcr hallnot exceed /32 n. [2 5 tnrtt] .

Exceptiofl: or filler wclds connectingstiffeners o wcb, thc sum of thc diamctersof

pipingporosity hal lnot exceed /8 n. [10 mm] in any incar nchof weldandshal lno i

cxcccd /4 n. [20mml i$ any 2 n. [3o0mml lengthof wcld-

(C) CJI' groovcwcl(ls n butt () ints ransvcrsc] thc d;rcct io l l ,l c( t t lp l l lud cl ls i lc t tc\s

shal lhavcno pipingporosity. ;ora l l othcrgroovcwclds, hc frcqucncy f pip ingporosi ly

shal lnot exceed nc n 4 in. 100 mml of lcngthand he nlaximumdiamctcr hal lno (

cxcccd3/32 n. [2.5mm].

Stat ical ly

Loaded

Nontubular

Connections

CyclicallyLoadcd

NontubularConnections

Ccncrr l Nolc:An

' 'X" indicatesppl icrbi l i ty or thc connccr ior ylc l a shidcdarca Ddic.tcs on'nPpl icrbi l i ty.

2 1 8



'.rA/14 ONIOOETECHHOCRfiTS3Z

No.47,o.Boxo.rss, asadioad,:,,j:111-i:"Jlili1il";llt^lll

(|Nto(|E : 3486659 Fax 091 B0 3485374E-mail [email protected]

^Errfi.4cls noM ASME nc.vrtr Drv.l

E.3 EVALUATION OTINDICATIONS -L indication s the evidence fa mechanicalmperfection.Only ndicationswith

majordimensions rater han l/16 in' shallbeconsideredelevant

".i lin.u, indi.ution is onehavinga lengthgrater han hree imes hewidth.

t.erounceaindicationisoneofcircularorellipticalshapewithlengthequaltoorless han },reeimes hewidth'

c.Anyquestionableordoubtfulindicationsshallbereexaminedtodeterminewhetheror nottheYare elevant.

t.4 ACCDPTANCESTAI{DARDSTh"**".pt-""standardsshallapp|yunlessothermorerestrictivestandafdsarespecifiedor specificmaterialsor applicationswithin thisDivision'

All srfaces to be examined hallbe freeofRelevantinear ndicationRetevantoundedndicationsgreatertnn 3/16 n

fou. or *o.e t"tevartt ounderl=ndicationsn aline separatedy 1/16 n' or

lesdedgeo edge)An indication lan imperfection aybe arger han he mperfectionhat

causest; however,lte sizeofthe indication s thebasisor acceptance

evaluation

'XTEICTAS FNOM ASME SEC.IX

QW - 195LIQUID PENETARNT EXAMINATIONdW-fSS.f Thi liquidpenetrant xaminationn QW-214or corrosion-resistanceeld

metaloverlayshallmeet he requirements f sestionV Article 6 Theacceptance

standardsf QW-195.2 hallbemet.

QW-f95.2Liquid PenetrantAcceptance riteria

QW- 195.2.1 elPinolorya. Relevantndications indioations ith majordimensionsreatefhan 1/16

in.(l.6mm)b. Linear ndications an ndicationhavinga lengthgreater han hree imeswidth

c. RoundedndicaUons an ndicationof circutaror elliptical shapewith the ength

equalo or less han hLreeimes hewidthQW - f95,2.2Acceptance tandards.

n-rocedo"atrO erfo-t unce estsexamined y liquid penetrantechniqueshaltbe udged

unacceptablehen heexaminationxhibits ny ndicarionn excess fthe limits

specified elowd. Relevantinearndications

e. Relevantoundedndicationsreaterhan3/16 n.(4'8mm)

f. Fouror more clevant oundedndicationsn a ine separatedy l/16 in-(l.6mm)

or less edgeo edge)

a.b.c.

d.



'

Equipln€lt.

ARTICLE 1T- l 0

T-120

T- 130

T - 1 4 0 '

T-150

T-16 0

T-17 0

T- 18 0

T-190

MandatoryAppendixAppendix

I - 1 l 0

I- 12 0

I - | ]0

. ' i : . .

S c o p e . . . . . . . . . . , .

C e n e r a | , . . . . , , . . . . . , ,l 2t 2l ?l 2l 3

1 3t 4I 4

t 5t 5I 5l 5

R€quirements

Procedure

Calibration

Eraminationsand lnsDectionsEvaluation.

RecordsDocumenlation

Glossary f Terms or Nondestrucriver(aminationS c o p e . . . , . . . . , . . . . .

GeneralRequirements

Requirenrents

l l



Afiicle of SubsectionA or as specified in orher CodeSections.2

T-130 EQUIPMENT

It is the responsibilityof thc.Manut'flcturer,abricator,or installer o ensure hat the exxnrinrtioncquipmcnt

being used conforms to the requirenrentsof this CodeSectioD.

T-140 RBQUIREMENTS

(rr) Nondestructive xanrinationPcrsourtel hall bcqualified in accordancewith tbe requirenrenrscf thereferencingCode Section.

(b/ For those Code Sections rhar direcrly refercncelhis Article for the qualificationof NDE. persontel, thequalification shall be ir accordancewifi one of rhefolldwing docunrents:

(1) SNT-TC-1A,3 ersonnel ualif icarion nd Cer-tification in NondestructiveTesting; or

(2) ANSVASNT Cp-189,3 ASNT Standard or

Qualificationand Cedficatiofl of Nondes(nictiveTestingPersounel;or

(3) ACCP,3 ASNT Central Cenification program.

(c) When the referencing Code Section does norspecify qualifications or does nor reference dircctlyArticle I of this Section, quali i ication may sirrrplyinvolvedenronstratjonn routinc manulacturing pera-tions to show that the personnclperforning the nonde-

rFor example, T-213 r€quircs tha( Inrigc Qurliry l dicntors bcmanufaclured nd identificd in :tccoftl:rncewith the rcquirerncrls orihematives al lo\ |ed i r SE-7.17 r 5E- 025, rnd Aoi)elrdiccs. s.pnropri l l tc or the srylcof IQt ro bc used. hesc . 'r" i r i c onty r,r , rrsof ei thcr SE-747or SE-1025 hnr arc nr irndrrolJ n Anicle 2.rSNT-TC'lA (1996 Edir io 'r . wirh t99S i\ddcnitunr). I 'crsonncl

QurlificJlion and Ccriificnlion irr Nondtsrr*rire ,c],Jifl :" ANSI/ASNT CP-189 (1995 Fdir ion,.

ASNTsL: i t r l . , ,Lttr r)J.r t i r r : ,u ion

and Ccrlificriion of NordcslrrKlivc Tcstin- Pcfsonnctr" irnd ,\CClll l levis io| l 3 (Nolcrulrr 199])1,

ASN'l 'Ccr)r | t r lCc i l jcr t i ( )n l , r t )-

8r:rDa publ ishcd ) thc An|cr ic:rrSocicty or N(nrdlr l rLrcr ivccsl i ru.lTt l Ar l ingr(( ln 'rr . t ' .O. I l . ' \ , l r i j l r i . a. '1, , , , ,1 ' , , .r t ' ; , , t r : :s.r t i t i .

l 2

ARTICLE 1

GENERAL REQUIREMENTS

T-110 SCOPE

(c,l Unless otherwise specified by the refurencingCode Section or other referencingdocuments,his Sec-tion of the Code contains requirementsand methodsfor nondestructive xaminationwhich areCodereouire-nlcnts to thc exlen they are specificallyreferenceiandrequired by other Code Sections.Thesenondesrructiyeexilmination methods are intendcd to detect surfaceand intemal discontinuities in materials, welds, a-ndfabricateri pans and components.They include radio-eraphicexamination,ultrasonicexamination, iquid pen-ctrant examination,magneticparticleexamination,€ddycurrent examination, visual exanrinaticn, leak testing,.urd acousticenrission xamination.

(D) For general termssuch as Inspectiou,FIaw, Dis-coDIi uitl, Evaluation, etc., refer to MandatoryAppen-dix L

't'-120 GENERAL

(d) SubsectionA desqibes the methods of nonde-structiveexaminationto be used f referencedby otherCode Sections.

(bj SubsectionB lists Standards overingnondestruc-tive examination methods which have been acceptedas standards, besestandards re ntended o be nfonna-tive only and are nonmandatory unless specificallyrefcrenced n whole or in part in Subsection or asirldiciited in other Code Sections,

{c,}Refcrcnce o a paragraph'of

any Anicle in Subsec,l ion A of this Scction or in tlrc referencinirCode

Scction includcs rll of the applicabte ules in rheparagraph.' In every case, referenceto a paragraphincludesall the subparagraphsnd subdir.isionsndertl)rt paragraplr.

(ri) Rcference o a Standardcontaincd n Subsection13 is nrandatoryonly to the extent lpecified in an

Il'or er;rnrptc, refcrcncc td T-270 includcs ull rh. nrlus (onri|i|lcd

iD 1' ' :7t t l r rougl iT,27?.3.



T-140 ARTTCI-E _ CENERAL REQUIMMENTS ' 'r-170

Code, it shall be the responsibilityof the Maoufacturer,fabricator,or installer o estdblishnondestructivcexami-nationprocedurcsandpersonnelceni{icationproceduresconfomring to the referencingCode requirements.

(cJ When required by the referencingCode.Section,all nondestructiveexamilations perfonned under rhisCode Seciiofl shall be done to a written procedure.

This procedureshall be demonstraterlo the satisfactionof the Inspeclor.The procedureor methodshall complywith the applicable requirementsof this Secrion forthe panicular examinationmethod.Where so required,written procedures hall be madeavailable o tbe Inspec-tor on request, At least onc copy of each proccdurcshall be readily available o the Manufacturer,sNonde-sauctive Exantnation Personnel for their referenceand use,

T-160 CALIBRATION

(a) The Manufacturer, fabricator, or insraller shallassure hat all equipment ctlibrations requiredby Sub-section A and/or SubsectionB are pcrfrrrnred.

(D) When sperial proceduresare developed fsee T-150(a)1, he Manufacturer, abricator, or installcr sltallspecify what calibration s necessary, vhen calibrationis required.

.T.170 EXAMINATIONS ANDINSPECTIONS

{a) The Inspector concernedwith the fabrication ofthe vessel of pressure part shcll, h,J,ve the duiy ofverifying to his satisfactionthat all exrminations re-quired by the referencingCode Sectionhave beenmadeto the requirementsof this Section and the referencingCode Section.He shall have the righr ro wirnessany oftheseexaminationso the extent stated n the referencingCode Section. Throughout this Sccrior of the Code,the word Inspetlor means the Au pri:ed Inspectorwho has been qualified as required in Lh€ various

referencingCode Sections.{0.)The specialdistincdon established n the various

Code Sections between inspectiou tod e.ranination anrJthe personnelperforming them is also adopted n thisCode Section. In other words, (lle term rirr?drttorrapplies to the functions perfonned by the Autlnrizedlnspector, b.ut the term exanination applies to thosequality control functions performed bv personnelcnt-ployed by the Manufacturer. One areir o[ occasionilldcyii l t ion ronl thesedistinctions xisrs. n thc ASTMSla,ldilrdMethodsand Recornrtren<ledracticesncomo-

oaooooaoaI

oa

oooooo

oooaoo

oao

ooo

oat

ao

t3

structive xaminttions recompetento do so n accord-ance witlr the Manufacturer' establishedprocedures.

fr?lThc cenificare holder shall ensure hat NDEpersonnelare qualilied and cenified ii accordancewiththi$ Arriclc. The certificate holder's euality program

sh{ll stipulate how this is to be accomplished.(aJ Qualincations in accordancewith a prior edition

of SNT-TC-IA, CP-189, or.ACCP are valid unti lrecinification. Recertificationor new cerdncationshrllbe ir accordancewith the edition of SNT-TC-IA. Cp-189, or ACCP specified in footnote 3.

(l) Linited certification of nondestructiveexamina-tiol pcrsonnelwho do not perform all of the operationsof \ no|destmctive method that consistsof more thnnonc operation,or who perform nondestructive xamina-tions of limited scope,may be basedon fewer hoursof training and experience han recommendedn SNT-'IC-lA.

CP-189,or ACCP. Any limitationsor reshic-tions placed upon a penon's certificadon shall bedescribed n the wntten practiceand on thecertification.

(g) Tlrc SNT-TC-IA document s a guide to esrablishpracticesfor taining, qualification,and certificationofNl)E. personnel as required by the referencingCodeSecrion,

'I"I5OPROCEDURE

f4, Tbe nondestructive xaminationmethods ncludedin LhisSectionare applicable o mostgeometricconngu-

rations and materials encounteredn fabricationundernonnal conditions.However,specialconfigurations ndmaterials may requiremodified nrcthodsand techniques,in which case the l,{anufactuer shall develop specialprocedures which are equivalent or superior to then]ethodsand tecbniquesdescribed n this CodeSection,and which are capableof producing nterpretable xami-nation results under the specia.l onditions-Suchspecialprocedures nray be modifications or combinadonsofnrethodsdescribed or referenced n this Code Section.and shlll be proved by demonstration o be capableof detecting discontinuitiesunder the specialcondirions,

and such demonstratedcapabilitiesshall be equivalentto thc capabilities of the methods described n thisCode Seclion when usedunderrnore generalconditions,Depending on the quality assurance r quality controlsystem requirementsof the referencingCode Section,thcse spccial proccdures shall be submitted to rheInspcck)r for acceptancewhere required,and shall beadopted as part of the Manufacturer'squality cortrol

Pro-qrilm.(/r.JWhcn ln cxanrinationo the requiremcntsf this

Scclionol the Codc s requircd y otherSections f the



T- 170

rated in &is Section of the Code by referenceor byreproduction n SubsectionB, the words inspectionorInspector,which frequentlyoccur iq the text or drlesofthe referencedASTM documents,may actuallydescribe

what the Code calls exatnination or exauiner. Thissituation exists becauseASTM has no occasionto beconcemedwith the distinctionswhich the Code makesbetween aspecliol arrdexaminatiott, inceASTM activ_ities and documents do not involve the AuthoizedIt$pector descibed in the Code Secdons. However. noxttempl has been made to edit the ASTM documentsto conform with Code usagei this should cause nodifficulty if the usersof this Sectionr€cogdze that theterms inspection, testing, artd examination in the ASTMdocuments eferenced n SubsecticnB do not describedulies of the Authorized Code Inspector but rather

T.190

describethe things to be done by the Manufacturer,sexamina on personnel,

T-180 EVALUATION

The acceptance hndards for thesemethodsshall beas stated iR the referencing Code Section.

T-190 RECORDS/DOCUMENTATION

Records/Documentation hlli bc in accordancewiththe referencingCode Scction and rhe applicable equire-mentsof SubsectionA and/or B of this Code Section:The Manufacturer, fabricator, or installer shall be re-sponsible for all required Rcco.ds/Documentation.

2001sEcTIoN V

t 4



APPENDIX I_GLOSSARYOFTERMS FOR NONDF,STRUCTIVE

EXAMINATION

t-r 0 scoPEThis MandatoryAppendixs used or the purpose

of establishing tandardems and definitionof terrnsconmonto all methods sedn Noldestructiye xami_nation,

I-120 GENERAL REQUIREMENTS

(c) The StandardTerminologyor NondestructiveExarninarionsASTM E 1316)has beenadopted ytheCommiftees SE-1316.

(rl SE-1316SectionA provideshe definit ion fternls isred n I-130(a).

(c) Paragraph.130(b)provides list of termsanddelinitions,which are n addition o SE-1316 nd areCodc specific.

I-130 REQUIREMENTS

(al The following SE-1316 ermsareused n conjunc-tion with this Article: defect,disco thruiry*, valu.ttion,

fel"^e indication, faw, law characterization, impetfec-I or1,ut erprctution, nonrekvant indication, relevant in-

(D/ The foJlowingCode ermsare used n conjunctionwith this Anicle:

erea of intcrcst - the specific po(ion of the objectthal is to be evaluated as denned by the referencing(lode Section

indication- the response r evidence rorrra nonde-structiveexamination hat requires nterpretation1() de-tenniDerclevance

inspeition - the observation of any operation per-

formed on materials and/or componentsto determineits acceptability in accordancewith given criteria

li,tlitedcertificatiotr an accreditationof an ndividu-al's qualification to perform sonle but not all of theoperationswithin a given nondesFuctive xaminationmcthod or (echniquc hat consists- f ooc or m,)rc thanone operation, or to perforn no:ldestructiveexamina_tions within a limitcd scopc of responsibility

metlnd - thc following is a list of nondesfrnctileexaminationmethods nd espective bbreviationsse dwithin the scope of Section V:

RT - Radiography

UT-

Ultrasonics'MT - Magnetic Particle

PT - Liquid PenetrantsVT - Visual

LT - kak TestingET - Electromagnetic Eddy Cunenr)AE - Acoustic Emission

no,tdestructiveemminarion (NDE) - the develop-ment and application of tech[ical nlethods to extminematerialsand/or componellts n ways rhardo not inrpairfuture usefulnessand serviceability in order to detect,Iocate,measure, nterpret,and evaluate flaws

operation aspecificphaseof a nerhod or technique

ptocedure- an ordedy sequence f actionsdgs-crib-ing how a specific terhnique shall be applicd

sexsir ivit l a measureof (hc lcvel of responsefronr a discontinuity by a nondestrucliveexilnlilirtion

tecluique - z techniquc s a specilic rvayof utiliz_inga Fonicularnondestructivexamiuation NDE) method

aI

acO

oaoaaaa

oaoaoo

tooot

a

aaoaoa

oooao

i : )

MANDATORY APPENDIXARTICLE 1



T-600

T-610't-620

T42l

T-630

T-631

T-640

T-641^t_642

T-643

T-650T_651

T-652

T-653

T-654

T,610

l - o / l

T-6"12

T,6',73

T-6'74

T-6?5

T-676

T-680

T-690

-igure

T-653.2

Trble

T 61 2

I{rndatory Appendix

ARTICLE 6

GeieralRequirements. . . . . . . . . . . . - , _

r22

t2 2

122

t2 ?

t22

122

t23

t23

123

124

t24

t ut24

t25

125

r25

125

125

126

t26

t26

r2'7) 2 7

121

I ?5

MinimumDwellTimes . . . . . . . - . . . 127

Appendix

I -6 t0

t-620

I,630

'128

128

I28

1 2 8

I 2 l



, l

t1

l

ARTICLE 6

LIQTJID PENETRANT EXAMINATION

T-600 SCOPE

The liquid penetant examinationmethod s an effec-tive meansor detecting iscontinuitieshich areopento the surfaceof nonporousmetalsandother materials.Typical discontinuitiesdet€crableby this methodarecracks,seams,aps, cold shuts, aminations, nd pc-rosity.

In principle,a liquid penetrants applied o thesurfaceto beexamined ndallowed o enterdiscontinuities.ltexcess penetrant s then removed,the part is dried,and a developers applied.The developer unctionsboth as a blotter to absorb penetnnt that has beentrapped n discontinuities,nd as a contasting back-groundo enhancehevisibilityof penetrantndications-Thedyes n penehantsreeithercolorcontrastvisibleunderwhite ight)or fluorescentvisibleunderultravio-let light).

T.6T0 R-EF'ERENCINGDOCUMENTS

T-610.1 Wben specified by the referencing CodeSection, the liquid peneEantexamination techniquesdescribed n this Article shall be ujed. The followingSE Standardprovides details that may be consideredin the specificproceduressed:

(a) SE-165StandardTest Method for Liquid Pene-lrant Examination

T{10.2 The liquid penehantmerhoddescribed n

tlis Anicle shall be used togetherwirh Article l,CeneralRequirements.

T-610.3 Definitions of termsused n this Article arein Mandatory Appendix I of rhis Article.

T-620 GENERAL

T-621 ProcedureRequirements

f-621.1 Liquid penetrant xamiration hallbe per-formed n accordance ith a written procedure. ach

procedurehall ncludeat least he following nforma-tion, as applicable:

(aJ the materials,shapes,or sizes to be examined,and he €xtentof the examination:

(b) lype (numberor letter designationf available)

of eachpenetralt, penetmnt remover, emulsifier, enddeveloper;

(cJprocessing etails or pre-examinationleaningand drying, including the cleaning materialsusedandminimum ime allowed or drying;

(d) processingetails or applying hepenctrant:belenglh of time that the penetnnt will remain on thesurfacedwell ime),and he tempemtqref thesurfaceand peretrantduring the examinationf ourside50'F(10'C) to 125'F (52'C) range;

(€) processingetails or removingexcess enetrantfrom the surface, and for drying the surface before

applyirg the developer;(/) processing etails or applyingthe developer,andlengthof developingime before nterpretation;

(8) processingdekils for post-examination leanitg.

T-621.2 Procedure Revision. A revised proceduremay be required:

(a) wbenevera changeor substitution s made n thetype or family group of penetrantmaterials(insludingdevelolnrs,emulsifiers,etc.) or in the processing ech-niques;

(b) whenevera changeor substitutions made nthe typeof precleaningmaterials r processes;

(c) fq anychangen part processinghat can closesurfmeopenings f discontinuities r leave nterferingdeposits, uchas tlte use of grit blastcleaningor acidtreatrnents.

T.630 EQUIPMENT

T-6f PenetrantMaterials

Tlne ermpenetrantmateials,as used n thisAnicle,is ntendedo include ll penetrarts,mulsiflers, olveotsor claning agents,evelopers,tc,,usedn the examina-

t22



_._a

'r'-63t

tion process. he descriptions f &e liquid penetrantclassificationsnd material ypesarc provided n SE-165.

T.640 REQUIREMENNS. _ - : . t : t . :

T-641 Control of Contamitrants

The userof this Afticle shallobtaincertification fcontaminant ontent or all liquid penetrantmaterialsusedon nickel basealloys, au$eniticstairless teels,aod titanium. Thesecertifications hall include thepenetrantmanufaciuiirs'batcbnumb6rs nd the testresultsobtained n acbordance ith (a) and O) below.Theserecordsshall be maintainedas requiredby the

refcrencingCodeSection.(o) Whenexaminingnickel basealloys, all materialsshall be analyzed individually for sulfur content asfollows.

(./) An individual ample f thepenetmnt aterialsrvithexception f cleanershallbepreparedor analysisby herting50 g of thematerialn a 150 mm nominaldiarueter lassPefti dishat a temperaturef 194"F o2l?oli (90oC o 100'C) or 60 riqin.

PI{ECAUTIOh$: Provide adequatevcnrilation ro dissipate he enril-

{?) Analysis of the residueshalt be as follows: If

the residue is less than 0.0025 g, the material isaccepteblc without funher analysis. If the residue is0.0025 g or more, the procedureshown in (a)(l) aboveshilll bc rcpeatedand the rcsidueanalyzed n accordancen'itlr SD-129 or SD-1552.Alrernalely, he materialmaybe decomposedn accordrncewith SD-lZ9 and alalyzedrn accordancewith SF5l6 Method B. The iulphurcontent sllall not exceed l% of tIrc residueby weight.

(-l) An individuat sampleof cleaner/removermate-rirl shall be prepared for analysis by hea(ing t00 gof the naterial in a 150 mm nomilal diameter glassPerri dish at a Gmperatureof I94.F to 2t2.F (90'C

to 100'C) for 60 min.

PIII'CAUTION:tovidc adequateenrilariono dissiparehef f l r i l teJ \ r |or .

(4J Analysis of the residueshall be as follows: Ifrhc rcsidue s less han0.005g, thematerial s acceptablervitbout lurthcr analysis. If the residue is 0.005 g orrDore, the procedure shown in (a)(3) above shall berei)eatedsnd the residueanalyzcd in accordancewithSD- 2a or SD-I552. Atternarely ire marerialmay bedecomposcd n accordancewith SD-129 and analyzedin accordancewith SD-516 Method B. The sulphurcorrLcnLhrl l not exceed % of the residue y weight.

ARTTCLE _ LIQUID PENETRANT XAMINATION "t-642

(b) Whenexamining ustenitictainless teelor tita-nium,all materials hall be analyzedndividually orchlorineand fluorinecontentas follows.

(.1,An individuat ampte f thepenetrant alerialswith the exception f cleaners hall be preparedor

, analysisby heating50 g of rhe material in a 150 mmnominaldiameter lassPetridish at a temperaturef194"F o 212'F (90"C to 100.C) or 60 min.

PRECAUnONT horide adequare enritaiion to dissipate he emir_reo vaPor.

(2) If the csidues0.0025 or more, bcprocedureshown n (b)(l) above shallbe repeated. he residuemay be analyz€d n accordancewith SD-80g and thetotal shall not exceed % by weight.Or, attemately,the residue hall be analyzedn accordancc ith SE-

165,Annex 2 for chlorlneand SE-165,Annex3 forfluorine, and the total chlorine plus fluorine contentshall not exce€d1% by weight.

(3) An individualsampleof the cleaner/removermaterial ballbe preparedor analysis y heating100g of the materialn a 150mm norninaldiametcr lassPetri dish at a temperaruref t94"F ro zlZ"F (90"Cto 100'c) for 60 min.

PRECAUTION: rcvideadequatc enrjlarjono dissipatehe emit-ted vapor.

(4) If the residue s 0.005 g or more, rhe procedureshown in (b)(3) above shall be repeated. The residue

may be analyzed n accordancewith SD-808 and the'total shall not exceed l% by weight Or, alternateiy,the residue shall ba analyzed in accordancewith SE-165, Annex 2 for chlorine and SE-165, Annex 3 forfluorine, and the total. chlodne plus fluorine contentshall not exceed I% by weight.

(c) As an altemative to (a) and (b) above, SE-165,Anaex .{4 may be used for dslelrninalion of anionsby ion chromatography,which provides a single instru-mental technique or rapid sequentialmeastrrement fconmofl anions such as chloride, fluoride, and s[lfate.

T-642, Surface Preparation

(a) In general, satisfactoryresults may be obtainedwhen the surface of the pan is in rhe as-welded,as-rolled, as-cast,or as-forgedcondition. SurfaceDreplra-tion by grinding, machining,or otlrcr mcthods rnaybe necessarywhere surface inegularities could rnaskindications of unacceptablediscontinuities.

(0, Prior to each liquid penetrantexamination, rhesurface to be examined and all adjacent areas rvithinat least I in. (25 mm) shall bc dry and free of aljditt, grease,irt, scale,welding fiux, weld spatter,paint,oil, and other extraneous mrtler that could obscure

oaoooO

eaoo

oaoooo

aaoI

aa

aaaoaa

oat

oa

123



2001SECTION T-653.3

surfaceopeningsor otherwise nterferewith theexami-nation.

Ic) Lyptcat leaningagentswhichmay beusedaredetergents,organic solvents,descalingsolutions, and

paint removers.Degreasing nd ultrasoniccleaningmethodsmay also be used.

(dl Cleaningsolventsshall meetthe req[iremeiltsofT-641.-The cleaningmethodemployed s an importantpart of the examinationprocess,

NOTEI Condidodng of surfaccsgrior lo cxami[ation rnay affecrtle resule Scr SgteS. eraex.l,i.

T-643 DrylngAft€r

preparation

Afrcr cleaning,drying of the surlaccso be examinedshall bc accomplishedby nornal evaporadonor wilhforcedhot or cold ah. A minimumperiodof time shallbe establishedo ensured|at the cleaningsolution hasevaporatedprior o applicationof the penehant.

T.650 PROCEDURE/TECIINIQUE

T-651 Technique

Ejthera color contlasr visible)p€ne&ant r a fluores-centpenetrantshall be usedwith one of the followingthreepenetrantPmcesses:

(a.)water wasbable(b) post+mulsifying(c) solvent removableThe visible andfluorescent eletrantsused n combi-

".u,i:."yjth these tfuee penetant processesesulr in

slx lrqurdpenetrant chniques,

T-652 Techniques ior StandarrtTemperafures

As a standard techniquq the remperatureof thefen-etrantand the surfaceof the palt to be processedshallnorbe below50"F 10"C)noi above 25;F (52.C)(hroughour heexamination eriod. rcal heatingoicooling is permitted provided he pah temper=tu.eremainsn rherangeof S0"F o 125.F 10.C ; 52"C.)during the examination.Where t is not practical ;complywith theseemperatureimitations, ther emper-arures nd imesmay be used, mvided heproceduresare qualifiedaslspecitiedn T_653.

. " \

l'.. i."'

\ \ J

T-653 Techniques for NonstandardTemperatures

T-653.1Ceneral.Wher it is notpracticalo conducta liquid penebant xamination ithin the temperaturerange f50'F to t25.F (10.Cto 5Z"C), heexaminarionprocedureat the proposedower or higher temperaturerangerequiresqualification.This shall requirehe useof a quenchcrackedaluminumblock,wiicfi in this

r Article is designated s a liquid penekantcomparatorblock.

T{53.? Liquid penetrantComparator.The tiouidpenetrantomparatorlocks hallbemade f aluminum.ASTM B 2@, Type 2024,3/ziD.(10 mm) thick,anjshould have approximate ace dimensions

of 2 i'I.. x3 in. (52 mm x 76 mm). At'$e centerof each ace.an areaapproximalely in. (25 mm) in diameter halibe markedwith a 950"F(510"C) temperature,inCicatingcrayon or paint. The markedareashall be heatedwirha blowtorch,a Bunsen urner,or sirnitardevice o atemperatureerween50"F 510.C)and975.F 524"C).The specimenshall then be immediatelyquenchedncold water,whichproduces networkof fine crackson each face.

The block shall henbe driedby heatingo approxi-ma@ly300'F (149.C).Afrer cooling, he blockshaltbe cut in half. One-halfof the specimen hall be

designated lock'A'

and the orher block ..B" foridentificarionn subsequentrocessing.igureT-653.2rllusEa€s he comparator.blocks,A"

and .,8.,,As araltemate o 6u[ing the blcck in half to make blocks"A" and "B," separateblocks 2 in. x 3 in. (52 mm

176 mm) canbe madeusing heheatingand quenching

te;hnique as describedabove.Two comparatorblocks'with closely matched rack pattemsmay be used-Thebloclcs hall be marked A"

and .,8."

T.6533 ComparatorApptication(a)_If.it is desired o qualify a liquid penetrant

eXaminadonprOOeduret a aemperalure f less than50"F (10"C),rheproposed rocedure ha.llbe apptiedto block "B" after the block and all materialstavebeen cooled and held at the proposedexaminationtempen[ure ntil thecomparisbns completed. stan_dardprocedure hichhaspreviously ec; dembnstratedas suitable or use shall be applied o block.,A', inthe 50'F ro 125"F 10.C ro 52.C) temperatureange.The indicationsof cracksshalt be comparedbetwe-enblocks A" and*8.'

If the indications btained nderthe proposed onditions n block .,8"

are essentiallvthesameasobtained n block-A,'

duringexaminational50'F ro 125'F 10'C to52.C), heproposedrocedure

shall be consideredualified or use-

t24



T-653.3

T---F-

: - - I?

e r

, -- 3

Y I

FIG. -653.2 LIQUID ENETRANTOMPARATOR(N0TE:Dirnensionsiven re or guidancenlyandar e

notcritical.)

(1r) f the proposedemperatureor thc examination

is above125"F 52"C), lock.B',shallbe heldar rhistenrperatufehroughoutheexamination.he ndicationsof cracksshallbe compared s describedn T-653.3(a)while block "B" is at the proposedemperatute ndblock "A" is at rhe 50.F to 125.F 10"Cro 52"C)temPcraturcange.

(c')A procedurequalifiedat a temperatureowerthan50'F (10'C)shallbequalifiedromrhat emperarureto 50'F {10"c).

(d) To qtalify a procedure or temperatures bove125'F (52'C), the upperand ower tempemtureimitsshallbe establishednd heprocedureualified t thesc

tcnlperatures,(e) As an alternateo the equirementsf T-653.3(a)and T-653-3(b)when usingcolor conhastpenetrants,it is permissibleo use a singlecomparatot lock forthcslandard ndnonstandardmperaturesnd o makethc comparison y-photography.

/,1)Whenrhesinglecomparatorlock andphoto-graphictechniques used, he processing etails asapplicable)described n T-653.3(a)and T-653.3(b)apply.The blockshatlbe thomughly leaned etweenthe two processing teps.Photographshall be takenattcr processing t the nonstandarderirperaturend

then after processingat the standard empi,rature.Theindicationof cracksshall be comparedbetween hetwo photog:aphs.tre samecriteria or qualificarionsT-653.3(a)

hatl apply.(2) The identicalphotographicechniqueshallLe

jused o Take the comparisonphotographs.

T-654 Technique Restrictions

Fluorescent efletrant xarninationhall iot followa colorcontrastpenetrant xamiflation.ntermixingofpenetrantmatedals rom different families or differentmanufacturerss rlot pemitted. A retestwith waterwahable peDeuants ay causeossof marginal ndica_tionsdue to contamination.

T.670 EKAMINATION

T-671 PenetrantApptication

Tl|epenetrantmaybe appliedby anysuitablemeans,suchasdipping,brushing, r spraying.f the penetrantis applicd y spraying singcompressed-air-rypcppara_tus, filters shall be placedot the upshear.nide neartheair inlet to preclude oRtaminationf the penetrantby oil, water,did, or sedinlelt hat mayhavecollectedin the ines.

' ' l-672 PenctrationTime

Penetrationime s critical.Themininrum enerr:rtiontime sballbe asrequiredn TableT-672or as qualilieriby demonstrationor specificapplications.

T473 ExcessPenctrantRemoyal

After thespecified enetrationime haselapsed, nypenetmntemainingon the surfaceshdl be removed,taking care to minimize removalof penetrant ronldiscontinuities.

T-673.1Water-Washable enctrants. xcesswarer-washable enetrantshall be removedwith a waterspray.The water pressure hall not exceed50 Dsi(3a5kPa),and hc wrtcr tcmp€raturchallnotcxccc,lr 0'F (43"C).

T-673.2Poslemulsification r:nctrants(a) Upophilic Enulsifcation. Aftet the equiredpene-

trantdwell tirne, he excess urface en;truntshall bcemulsified y immcrsingor flooding he paft wirl) thcemulsifi . Emulsilication imc is depeodent n thctype of emulsifierand surfacecondition.The ac(ui\l

ooaaooaoaaoe

oI

oaoa

aaoaaa

aoI

oae

aoooo

ARTICLE 6 _ LIQUID PENETRANTEXAMINATION

t25



T-613.2 2001SECTIONV

emulsificationime shallbe determined xperimentally.After ernulsification, hemixtureshallbe removedbyimmdning- n or.rinsing with water.The temperature

and pressure f the water shall be as recommendedby the manufacturer,(b) Hydrophilic Emulsifcation. After the required

penetrant well time and prior to emulsification,heparts shall be prerinsedwith water spray using thesame rocess s or water-washableenetrants.rerins-ing time shallnot exceed mir. After prcrinsing,heexcessurface enetranthallbe emulsified y immers-ing in or sprayingwith hydrophilicemulsifier.Bathconcentrationhallbeasrecommendedy the.rrra[ufa:-turer.Afteremolsification,he mixture hallbe removedby immersingn or rinsingwith water.The emperatureand pressure f the wa6ershall be as recommendedby the manufacturer.

NOTS:Additional nformarionnay be obrainedrom SE-165.

'f.673.3SotventRemovable enetrants. xcess ol-

vcnt removable enetrantshallbe removed y wipingwith a clothor absorbentaper,epeatinghe operationuntil nrost races f penetrant avebeen emoved. herenaining tmcesshall be removedby lightty wipingthe surfacewith cloth or absorbent apermoistenedwith solverlt-To minimize emovalof penetrantromdiscontinuities,areshallbe taken o avoid }|e useofexcesssolvent. Flushing the surface with solvent,follorving he applicationof th€ penetrantand priorto developing is prohibited.

T-674 Drying After Excess PenetrantRemoval

(a) For ahewaterwashable r post-emulsifyingech-nique, he surfacesmay be driedby blottingwith cleanmaterialsor by using circulatingair, provided thetemperaturef the surfaces not raisedabove 125"F(s2"c).

(b)For thesolventemovableechnique,hesurfacesmay be driedby normalevaporation,lotting,wiping,

or forcedair.

T-675 - Developing

The developer hall be appliedas soonas possibleafter penetrant emoval; he time interval shall notexcced hat estrblishedn the procedire. nsufficientcoating hicknessmay not draw the penetrant ut ofdiscontinuities;onversely, xcessive oating hicknessnay nrask ndications.

T-676.2

With colorcontrast enetrants,nly a wet developershall be used,With fluorescent enetrants, wet ordry developermay be used.

T-675.1Dry DevelopcrApplication.Dry developershaU be appliedonly to a dry surface by a softbrush, andpowderbulb,powdergun,or othermeans,provided he powder s dustedevenlyover the entiresurfacebeingexamined.

T-675.2 Wct Developer Application. Prior roapplying uspensionypewet developero the surface,the developermust be thoroughlyagitated o ensureadequate ispersion f suspendedarticles.

(a) AqueousDeveloper pplication Aqueous evel-oper may be applied o eithera wet or dry surface.

It shall be appliedby dippidg, brushing spraying, rother means, rovideda thin coating s obtained yerthe entire surfacebeingexamined.Drying time rnaybe decreasedy usingwarm air, provided he surfacetemperature f the part is nof raisedabove 125'F.Blotting is not permitted.

(b) Nonaqueous evelopeApplicatiol. Nonaqueousdeveloper hall be appliedonly to a dry surface. tshaUbe appliedby spraying,except 1,here afetyorrestrictedaccesspreclude t. Under such condirions,developermay be appliedby brushirg. Dryirg shallbe by normalevaporation.

T-675.3Developingime for final interpretatione-girs mmediately fter heapplication f a dry develogeror as soon as a wet developer oating s dry. Theminimumdevelopingimeshallbe as equired y TableT-6'12.

T-676 Interpretation

T.676.1 Final Interpretation. Final interprecationshallbe madewithin ? to 60 min after he requirementsof T-675.3aresatisfied.f bleed-out oesnot alter he

examinationesults, onger periodsare permined. fthesurfaceo be examineds largeenough o precludecompleteexamination ithin the prescribed r estab-lished time, the examination hall be perfomred nincrements.

T-676.2Characterizing ndic.ation(s). he type ofdiscontinuitiesre difficult to evaluatef the penetrantdiffuses xcessivelynto he developer.f rhisconditionoccurs.closeobservation f the fonlation of indica-lion(s) during application f thc developermay assistin characterizing nd determining he ex(enrof rheindication(s).

126



T-676.3 ARTICLE 6 _ LIQUID PENETRANT EXAMTNATION T-690.1

TABLE {72 MINIMUM WELL IMES

Dwell imestNote l)l (minutes)

Material Type t Discontioutty Penetrant DeveloperAluminum,magnesium,teel,brass

andbronie, itaniumand high_temperaturelloys

Carbide-tippedools

Castings nd r€lds

' : ' :- , . . :

" - i

Wroughtmaterials extrusions,{orgingr,plate

All formsAll formsAll forms

Coldshuts, orosity,ackof f 5ion,

. cracys (all forl,6)

Laps,cracks (all forrns)

Lackof fusion porosity, racksCracksCracksCracks, oroslty

'Plasl ic

G ass

Ceramic

7

7

7

7

7

t 0

55

5

oooaoI

o' o

oooo

oaoooa

aaooI

a

aaoI

aa

oacaI

NOTE:(1) Fo/ temperatureange rom sooF o 125"F 6O.C to 5z.C).

T-676.3 Color Contrast penetrants. With a colorcol"trast penetrant,. the

-developer forms a reasonatrlyurulorn white coating. Surfacediscontinuitiesare indi-_calcd by blecd-outof the penetrantwhich is nomallyri dcel) rcd coJor thrt stains &e developer. ndicationswith a light pink.color may indicateexcessive leaning-lnadcquatecleaningmay leavean excessive ackgrourirnrking interyretationdifficult. A minimum lighiinten_

:ll :t:Ofc (500 Lx) is r"4uired o ensure;equjtc

$cnslt ivityduring the examinationand evaluation findica(ions_

T-676.4 Fluorescer.t penetranls. With fluorescenrpenetrants, the process is essentially the same as inT-676.3, with the exception that the examination ispcriomrcd.using an u_ltravioletighr, called black light.lr)e exanrinationshall be performed as follows;

(a) It shall be performed in a darkened area(DJThe examiner shall be in the darkenedarea br

at lelsr I rnin prior to performing the examination oenrDjc r,s eyes o adapt o d3rk viewing. If tlte examinerwcarsglassesor ienses, hey shallnot be photosensitive,

(cj The btack light shall be allowed to warm up fora minimunl

of 5 min prior to use or measurementfrne rntensiryof the ulrraviolet ight emitted.

.(dJThe black light intensity shall be measuredwirh

a orack rghl meter.A minimum of 1000pWlcmr onthe surfaceof the partbeing exanrined hall be required.

The black light intensity shall be measuredat leastonce every 8 hr, and whencver the work station ischanged.

T-677 post.examination Cleaning

When post-examina[ioncleirning is required by thepmcedure, t should be conductedas soon as practicalusrnga process hat does nor adverselyaffect ihc part.

, T.680 EVALUATION

(a) All indicationsshall bc evaluated n terms of theacceptance hndards of the rcferencingCode Section.

(bJ Discontinuities at the surface will bc indi.Jatedby bleed-outof penetranqhowever, Iocaljzed surfaceirregularitiesdue to machining marks or other surfaceconcitrons may produce faise indications,

(cJ Broad areas of fluorescence or plgmentalionwhich could mask indications of discontiiuities areunacceptable,and such arcas shall be clcaned andreexamined.

T-690 DOCUMENTA'i'ION/RECOITDS

T-690.1 Documentation/recordsshall be in accord_ance with the referencingCode Section,

121



ARTICLE 6MANDATORY APPENDIX

APPENDIXI_GLOSSARYOF

TERMS FOR LIQUID PENETRANTEXAMINATION

I-610 SCOPE

This Manda[ory Appendix is used for the purposeof establishingstandard erms and definition of termswhich appear in Article 6, Liquid penetrantExami_nation.

1.620 GENERAL REQUIREMENTS

(a) The StandardTerminology or NondestructiveExaminationsASTM E 1316) has beer adopred vthe Cornmi(ee s SE-1316.

fb) SE-1316SectionG provides he definitionsof

terms isted n I-630(a).(c) For general cerms, such as Ind.ication, Flaw.

Discontinuiry,valuarion, tc., efer o Anicle I, Man-datoryAppendix1.

(d) Pangraph -630ft) providesa list of termsanddefinitions,which are n add.itiono SE-1316 nd areCodesnecific-

I-630 RIQUIREMENTS

(4] The following SE-1316 ermsareused n coniunc-tion with this Article: black light; bleedour; bloiting;clean; cofitaminant; contrasfi developer; dcveloper,aqueous;develoi)cr,dry; devclopcr,nonaqueousi evel_

oping time; drying time; dwell time; emulsifler;family;fluoresce[ce; overemulsification:penetmnt; penehantcomparator; peoetra;t fluoresceor; pene$anl, waterwashable;post-cleaning;post emulsification; preclean-ing; rinse; solvent ren]over.

(b) Thc following Cr:de cnns are used n conjuncrionwith this Article:

black light intensit - a quantirativeexpressionofultmviolet inadiance

color contrastpenerralt - a bighly pcnerratingiquidincorporating a nonfluorescentdye, which producesindicationsof such ntensitythlt rhcy ar. readily visibleduring examination

under white lightpost emulsif.cationpenetant - a type of peneirantcontainingno emulsiner, but which requiresa separateemutsifying step to facilitate waler rinse removal ofthe surfacepenetrant

solvent removablepenetrant - a typc of penerrantused where the excesspenefiant is removed from thesurfaceof the part by wiping using a nonaqueousiquid

I 2 8



0 1 ARTICLE 24LIQUID PENETRANT STANDARDS

SD-129 StaldardTestMethod or Sulfur n petroleum roducts Cenerat( A S T M 1 2 9 - 9 5 ) B o m b e $ o d ) _ . . . . . . . . . . . . . . _ . . . . . . . 4 4 s

SD-516 StandardesrMerhod or Sulfateon in Warcr . . . . . . . . . . ....._ 44t)(ASTM D

516-90)

SD-608 Srandard esrMethod or Chlorine n New and Usedperrolcum(ASTM D 808.95) productsBombMethod).. . . . . . . . .. ..... 453

SD-1552 Standard esrMethod br Sulfur in pctroleum roducrsHigh_(ASTMD 1552,95) Temperatureerhod). . . . . . . . . . . . . ... .. 457

SE- I6J Srandr rdestMef tod or L iqu id ener ran|Examirar ion.. . . . . _ . . . . . . . . . . . , . . . . 464(ASTM

E 165-95)

.':,..,'

444



. J

sD_129

(Identical ith ASTM D 129_95)(fhis specifications availablen SI Unitsonly.) 4ffII,

I. Scope

1.1 This test method covers the determination ofsulfur in petroleum prnducts, ncluding lubricating oilscontainingadditives,additiveconcentrates, nd lubricat_ing greases hat cannotbe bumed completely in a wickIamp. The test method is applicable to any petroleum

product sufficieotly low in volalility that it can be .weighed accurately n an open sample boat and con_talnjng at Ieast0.170sulfur.

NOTE - Thjs esr erhods norapplicableo samplesontaiDingelcmenG lhar givc residues,otlEr lhBn barium sulfite, which ariinsoluble in dilute hydrochloaic acid and would inrerfcre in rbeprecipjtalioDstep, Thesc inteifaringclements ncludc iron, aluminum,calcrum, siiicon, and lead c,hich arc sometimes presenr n greases,Iube oil addirives, or addirive oitr. Other acid insotubte m;lcristslhat inrcrfere are silic4 molybdcnum disulfide, asbestos,mic4 elc.Thc rest rnethod s not applicrblc to uscd oils conraining wcar mcrals,l'nd leid or silicares from contamiaation.Samplcs thni are cxcluijedcilrl bc anfrlyz-€d y Tesr M.thod D 1552.

1.2 This snndqrd does not purport to address all(l the :;efelf cotcerni if any, as.rociatedi r its use.II is the responsibility oJ the user of this standard toestablish appropriate satetyand health practices anddelennine the applicahility of regulatory limitationspior to use.See3.2 for specificprecautionarydircctionsincorporated'n the test method.

2. Referenced Documents

2.7 ASTM Statdards:

D | 193Specification fi Reagert WaterD 1552Test Method-forSulfur n petroleumproducrs

(lli gh-TemperatureMerhod)

E 144 Practicc or SafeUse of OxygenCombustionBombs

3, Summary ot Tcst N.{ethod

3.1 Tlle samples oxidizedby cornbustionn a bombcontaining xygenunderpressure.he sull'ur, s sulfatein the bomb rvashings,s deterntineil rlvimetricirlJyas bariunl sulf i l tc.

3.2 lYarning * Sticr adl.tererce to all. oJ theprovisions prescribed herealer etrttres againstexplo_sive rupture of the botnb, or a blor.out, providetl thebornb s of propcr designand con.rtruction tntl in goorl,rechanicql co dition. It is desirable,h,.ty,e,ter,httt theboob be enclosed n a shield of stecl l) .le dt leosll3 nn thi&, or uJ iwtlent hrotct:tio,t hc providcl

t . t i t ts lu J i t rsat ( t . )n | i g , . t i , . \ .

rl. Apparatus tnd Nlateriats

4.1 Bonh, hitving cilpacilyof not lcss rhan 30 0nrl-, so conslruc(ed hat it wilt not leak during the testand that quantit tive recoveryof the liquids frorn lhebomb miry be achieved readily. Thc inncr surlace ofthe bomb may be tnlde of stai,r icss teelor aty orhernaterial thal wil l not be affectedby the combustiorrproceris r products,Materials scd n thc bornbassem_bly, such as thc headgasketand lcld,wire insuhtion,shallbe resistanto helt ind chenicll action,andshallnoi unclcrgo [ry rcilction hir wil l alfccr the sulfdrcontentof thc liquid in rhc ixrnrh.

STANDARD TEST METHOD FOR SULFURIN PETROLEUM PRODUCTS(GENERAL BOMB METHOD)

445



SD- 29 2OOISECTION

aaoaoaaooooa

oI

a

4.2 kutltlc Crrp,platinunr,24 nrnr n outsidediametcrat the bottom,2? rnrn in oubidc diameterat the tbp,12 rrnr in heiglrt ourside, nd weighing l0 to ll g.

4.3 Firitg lyi?, pla(inum,No. 26 B & S gage,0.41nnr (16 thou), 27 SWC, or equivatent,

NOTE2r Caution Theswirchn rhe Sniriooircuit hall eofa rypc which rernxins opcn, exc.pt whcn hcld in closcd posirion by

4.4 lgnitiort Cirrir, capable i supplyingsufficientcurrenr o jgnite the cottonwicking or nylon threadwithout oleltingthc wire. The curent shall be drawnfronra stcp-downransformerr from a suitable attery.

4.5 CoftonWickitlgor NyLn SewingThread,white.

5, Rcagcn(sund Mctcrials

-i.l Prrrrr_r,J Reagents Reagentgrade chemicalsshil l j bc used n ali tests.Unlessotherwise ndicated,it is intended lt i l t { l l reagents hrll conform to thespccil ic1lr ior lsf the Conrmittec n AnalyticalReagentsof the ,A.ntericanltcmicalSociety,wheresuchspecif i-ciltior)s re available.Other gradcsmay be used,pro-vidcd it is l lrst r.jccnaincd hiLt thc rc gent is ofsull icienrlyhigh purity ro pcrnrir rs use without ess_enl - t jLhcuccuf i rcy f l l te dctcr i l l t ion .

5.2 Purity uf lvdet - Unlcss otherwise ndicated,refereltces tr: rvaier shall meao wtter as defined byTypc I l or I I I o1 ' Spcc i f ica t ion 1193.

5.3 Buriunr Chloride Soltuiott(85 g/litre) - Dissotve100 g of barium chloridedihydrare BaCl2 2H2O) ndisti l led rvatcrand dilute to I I i trc-

5.1 Ilrontirv Weter (satur(jted).

5,5 Jlsrlnx:ltloric;1crr/sp gr t.l9) - Concentratcdhydrochloric cid (ttCl).

5.6 O-n'qca,rec of combustiblcmllcr ial and sulfurcoDrpolrn{Js.vi l j lablc lt tr prcssurcol 4l kgf/cmz

{40 r l r r r ) .

5.7 Sodint CarLtctrtQrcolution (50 g/litre) _ Dis_solve 135g of sodiumcarbonate ecflhTdrateNa2CO1

l0 l l -O) or i rq equiva lcnr c ighL n d is t i l ledwaterand diiure ro I iitre.

5.8 ll4rire Oif, USP, or Liquitl par<ffir, Bp, or

6. Proccdure

6.1 Preparationof Bornb and Sanple - Cut a pieceof firing wire I00 mm in lcngth. Coil rhe middlesection(about 20 mm) and attach the free ends to theterminals. Arrange the coil so that it will be aboveand to one side of the samplecup, Insert between woloops of the coil a wisp of cotton or nylon thread ofsuch length that one erd will extend into the samplccup. Placeabout5 mL of Na2CO3 olution in the bonrb(Note 3) and rotate the bomb in such a manner thatthe interior surface s moistened y the solution. Intro-duce into the samplecup the quantitiesof sample andwhite oil (Notes 5 and 6) specified in the followingtable,weighing the sample o the nearest0.2 mg (whenwhite oil is used, stt the mixture with a short lensthof qutrtz rod and allow the rod to remain n the sam-plecup during the combustion).

NOTE3- After epeatedscof ihebombor sulfordelerminadons-a nlm may b€ noticed n lhe inn.asurface. his dullncss an beremov€dy periodic olishing f drc bornb.A satisfactorve(hodfor doing his s to rolaretc bombn a larhe t abour 00 Pmrndpohshfic oside urface irhenerypotishingapcrs rirN-o.2,,or cquivalentape.,oated irh lighrmachineil to pre\.cnrcutt;ng. rnd rhcn wilh a pasteof grjr-frEechfomic oxide and watcr.'fhis.pr.cdure

\rill rehove all bur very deep pirs and pul a hi:hpolrih on the surlace. Bcfore rie bomb is used ir jhall be washcdwilh soap and warer ro remove oil or patte l€fr from the pol;shingoperniion-

NOTE 4: Caution - Do not use more ihan 1.0 g rotal of samplcand white oil or olhea ow sulfur combusriblemate.ial or more ltar.0.8 e if the lP 12 bonb is used.

WeigbtofSample,I

0.6 o 0.8

0-3 o 0.4

WeighrofWhireOil ,g

0. 0

0.3ro 0.,1

Sulfur Content, %

5 or undcr

tj9TF 5 - Use of sampteweiehlsconraining ver 20 mg ofchlorinemay causecorrosion f the bomb.To avoid this. t jsrecoormendedhat for samples ootaining ver 2% chlorine, hesamplewcightbe basedon lhe chtorinccontentas given in rhefollo*inp rabie:

ooa

aooaoa

OaI

o

ChlorineConlenl,%

2 t o 5

Over5 to l0

Ovcr 0 lo 20Over20 o 50

Wcighr fSample,I

0.4

0.20. 10.05

wciShrofWhiteOil ,g

0.40.6

0.70. 7

NOTE 6 - tf rhe samples nor readitymiscjblewi$ whitc oil,someo$er low sulfur combustible ituent may be substituted.However,he combinedwejghtof sampleand nonvolatile jluenlshallnot€xcecd .0g or mor. rhan .8g if the p 12bomb s used,

6.2 .Addition of Oxygen - place the sample cuD inposition and arrange the cotton wisp or nyion threadso that the end dips into the sample. Assemble thebomb and righten the cover securely. (Caution _ See

ot

aoaoa

', :r-.1gl

446



Capaciti ofBomb.d'

. ' ARTICLE 24 _ LIQUID PENETRANT STANDARDS

300 o 350350 o 400400 to 450450 o 500

Note 7.) Admit oxygenslowly (to avoidblowing theoil from thecup) until a pressue s reachedas ndicatedin the following table: .;S:1, ;

sD,129

6.5 Detennination of Suvur - Evaporate he com-bined washings to 200 mL on a hot plate or. othersouce of heat. Adjus( the heat to maintain siow boilingof the solution and add l0 rol- of rhe BaCl2 solution,eittrer in a fine steam or dropwise. Stir the solutionduring the addition and for ? min thcreafter. Coverthe beaker wilh a nuted watch glass and continueboiling slowly until the solution has evaporated o avolume approximately75 mL as indicatedby a markon the beaker. Remove rhe beaker from the hot plare(or other sourcc of hcat) and allow it to cool for Ihr before filtering. Filter the supcrnatantiguid through

ari ashless,quantitati{e filter paper (No(e 9). Wash theprecipihte with water, first by dccantationand then onthe.nlter, rrntil free from chloridc. Transfcr the paper

and precipitate to a wcighed crucible and dry (Note

l0) at a low heat unril the moisturchas evaporaied.Char the paper conrpletelywithour ignir ing it, andfinally ignite at a bright rcd hcar unril (hc residue swhite in color. After ignition is complere, llow th ecrucible to cool at roont temperarure,and wcigh.

NOTE 9 * A wciglrcd porcelain lihcr cnrciblc (Sclxs type) ol 51o 9-pm porosily miy bc used in plrce of rhc lllrer paper. In rhiscase ths pr€cipit:rte is w:rslled frec of chloridc xnd rhen (lricd toconst&|ltweight at 500 r ?5'C.

NOTE l0 - A sa(isfirctorymeilns of drying, ch ring, tDd igniiinglhe piper and precipititc is to pLace he crucible coahinir,g the $erliher papcr in a cold elcckic mufflc furrace and ro tum on rhecurrel|t. Drying, chaning. and ignition usulll] will (xcur al rhedesircd rate.

6.6 Blank * Make a blank determinltionwhenever

newreagents, hiteoil, or other ow-sulfur ombustiblematerialarc used.When runnilg a blank on white oil,use 0.3 to 0.4 g and follow the normal procedure.

7. Calculation

7.1 Calculatc lle sulfur conten'iof the sample asfollows:

Sulfur, weight percent = (P - B)13.'l3lW

where:

P= grams .rfBaSOa btained rom sample,B = gramsof BaSOaobrrincd fron) blank, ardl,Y: granrs f santplcUscd,

E, Report

8.t Report the resulls of rhe test to tfre n€iirest0 .0 lVo.

MiniqutoGaBqPressurei gf/cml attn)

39(38)36(35) ,

. 3l (30)28(27)

,: MaximumGagePrcssuic,^ gfl.in'z (atin)

4l (40)

38 (37)

33 3?)30(29). .

'1Thc minimurn prcssuresarc speaifredo ptovide sufncieDtorygenfor complete combustiohand thc natimM prcssuhcscpletent a

:afetj- requircnent.

IOTE ?i Caulion - Do nor edd oxygetr t ignile lhe samplefthe bomb has been arred, dloppe4 o rilied,

6.3 Combastion - Immerse the bomb in a cold

distilled-water bath. Connect the terminals to the open

clectrical circuit. Close the circuit to ignite the sample.(Caution - See Note 8.) Remove the bomb from the

bath after immersion for at least l0 min. Release hepressureat a slow, uliform rate such that tbe operationrequires not less than I min. Open the bomb andexamine the contents. If traces of unbum€d oil or

sooty depositsare found, discard he determinationardthoroughly clean the bomb before again putting it in

use (Nore 3).

NOTE8: Caution Do not o nea ie bomb ntilar e3st 0 salier firing.

6.4 CollectionoJSufur Solution Rjnse he nteriorof the bomb, the oil cup, and the inner surfaceof thebomb coverwith a fine et of water,andcollect hewashingsn a 600-mLbeaker avinga mark o indicate75 nrl-. Removeany precipitaten thebombby meansof a rubberpoliceman.Wash he base f the terminals

until the washings re neutral o the indicatormethylred. Add l0 mL of saturatedbromine water to theu,ashingsn the beaker. [he volumeof the washingsis normally n excess f 300 mL.) Place he samplecup n a 50-mL beaker. dd 5 mL of saturatedrominewater,2 mL of HCl, and enoughwater ust to coverthe cup. Heat he contents tthe beakero just belowits boilingpoint for 3 or 4 min andadd o lhe beakercontaining he bombwashings.Wash he sample upand thc 50-mL beaker horoughlywith water.Removcany prccipitate n the cup by meansof a rubberpoliceman.Add the washings rom ahecup and the-50-nrl- eaker, nd he precipitate,f any, o the bombwashings n the 600-mLbeaker.Do not nlter any ofthe washings, ince iltering would removeany sulfurt)rescnts insoluble aterial.

44 7



sD-129

9, Precision nd llias

2OOISECTIONV

oaooaoaat

aoa

oeaooo

aoooI

a

aaot

t

a

oaooc

0.25o.2:1

Ll Tl)c precisionof this (est s not known to havcbeeo obtained in accordancewith currently acceptedguidelines (for exanrple in Comrnittee D-2 ResearchReport, "Manual on Determining precision Data for

ASTM Methods on Petroleum products and Lubri-cants").

9.7.1 Repeatability The differencebetween wotcst results, oblai ed by thc same o;:crator with thesalnc apparatusunder constantoperatingconditionsonidentical tesr material, would in the long run, in thenomral and coftcct opeEtion of the test method,exceedthe follorving values only in one case n twenty.

9.1.2 lleprotlucibility - Tl.)e difference betweentwo singleand ndcpendcntesults btained y differentoperators workiog in different laboratorieson identicaltestntaterial vould, n

the long run, n the normalardcorrcct operationoI the tcst mcthod. exceed lre l-ollow-urg valuesonly in one case n twenly:

1.5 o 2-0 0.t22,0 o5.0 0,18

NOTE I I - Thc pr.rision sho*r in the abovc able do€snot applyto samples ontainingover 2% clrlorinebecause n added eslricrionon the amoDntof samplewhich can be ignired is imposed.

NOTE 12-

This teslmethodh.s beencoop€rntivclycsrcdonlyin fte rnnge f 0.1 to 5.0%sulfur.

NOTE 13 - The followioS rfofiarion on rhe precision f thismethodhasbeen developed y thc lnstitule of Petroleum London):

(a) Resulls f duplicatcestsshouldnot differ by nrorc han rhefollowinSamount :

Rcp€atability

0.016 + 0,06

Reproducibilily

0.03? + 0.13

SLrfur,

wci hr %

0.1 lo o--5

0 . 5 o 1 . 0

1 . 0 o 1 . 5

Jicpeatability

0.040.06

0.08

Reproducib;lhy

0.05

0.09

0 .15

wherer is tha meao of dupli4ate est resulls.

fr, Theseprecision alocswere obtaincd n 1960 Jy statislicrlexaminstion f interlaboratoryes,t esults-No limirs have beenesbblishEd or additivc conceftrates.

9.? Bias-

Results btainedn one laboratory yTcstMethodD 129on NIST Srandard eference are-rial Nos. 1620A,1621C, nd 16628were ound ro be0.05mass ohigher han he acceptedeference alues.

10. Keywords

10.1bomb;sulfur

448



qffI|)

1. Scope

1.1This urbidimetricestmethod overshedetermi-nationof sulfate n water n the range rom I to 40rnC/Lof sulfate on (SO+--).

1.2 This test methodwas used successfullywithdrinking,ground,and surfacewaters. t is the user'sresponsibilityo ensurehe validity of this testmethodfor waters of untestedmatric€s,

1.3 Formergravimetricand volume.tric est methodshave been discontinued. efer to AppendixXl forhistorical nformation.

1.4 This standard does not purport to address hesaJetyconcems, if any, associatedwith its use. h isthe responsibililyof theuserofthis standard o establishappropriate safety and healthpractices and determinetlrc applicability of regulatgA limitafibns prior to use.

2. Rcferenced Dosrmenls

2.1 ASTMStdndards:D 1066Practiceor Sampling teamD 1129TerminologyRelatingo WaterD I 192Specificationor Equipmentor SamplingWater

ilndSteamn ClosedConduitsD 1193Spdcificationor ReagentWaterD ?'1"17 ractice ot Determination f PrecisionandB as

of ApplicableMethods f Cbmmittee -19 on WaterD 3370Practicesor SamplingWater romClo$edCon-

duitsE 60 Practice or Photometricand Speclrophotometric

Metbods or the Chemical nalysis f Metals

E 275 Practice or Describingand MeasuringPerform-ance f Ultraviolet, isible, ndNear nfrared pcctro-photometers

STANDARD TEST METHOD FOR

SULFATE ION IN WATER

sD-516

(IdenticalwithASTM D 516-90)

3. Terminology

3.1 Defnitiotts - For defiritions of tcrms used in

this test mcthod, cfc r to TenninologyD 1129.

4. Summery of Tcst Mcthod

4.1 Sulfate ion is conv erted o a brr ium sulfate

suspensionndercontrolled ondit ions. solution on-

tainingglyccrin and sodium chloride s added o stabilizethesuspension nd minimize nterferences. he resulting

turbidity is determinedby a nephelonreter, pecbopho-

tometer, or photoelectriccolorinreterand compared to

a curve prcparedfrom standardsulfate solulions.

5. Significance and Use

5,1 The determinationof suliate s important because

it has becn reportcd that when tbis ion is prescot in

excessof about 250 mg/L in drinking water, it causes

a cathaflicaction(especially n children) n the presence

of sodium and nragnesium,and gives a bxd taste tothe water.

6, Intcrfcrcnccs

6.1 Insoluble suspcndcdmatter in thc sample musl

be removed. Dark colors that can bc compcnsated or

in the procedure intcrfere with the neasurenent of

suspended xriuin sulf ir te BrSOa).

6.2 Polyphosphatcss low as I mg/l- will inh ibit

barium sulfateprecipitationcausinga negative nterfer-

ence.Phosphcnatcs rescnt n low concentrations,de-pendingon tlre type of phosphonrte, ill also causc

a negative ntcrfcrencc. ilica in excess f 500 mg/L



oo

sD-516 2001sEcTIoNv ooooooaooa

ooo

may prccipitate along with the barium sulfatg causing

a positive interfcrence. Chloride in excess of 5000

ngn- \+)11 aus€ a negative interference,Aluminum,

polyrners,and large quantitiesof organic materialpres-

cot in the test sample may cause the barium sulfate

to precipitatenonuniformly, In the presenceof organicmatter cefiain bacteria may reduce sulfate to sulfide.

To minjmize thc action of sulfate reducing bacteria,

samples houldbe refrigented at 4"C when thepresence

of such bacteria is suspected.

6.3 Alihough other ions normally found in water donot appear to interfere, the formation of the barium

sullate suspension s very criticat. Determinations hat

arc in doubt mry be checked y a gravimetricmethod

in some clses, or by the procedu.esuggestedn Note 2,

7. Appalatus

7,1 Pluno leter * One of the following, which are

given in order of preference.

7.1.1 Nephelorneter r t urbidimererl

7.1,2 Spcctrophoto,netercrr usc at 420 nm n'ith

l i i l r r l ) r th ( ' t '4 to 5 cn) l

7.1.3 Filter photometerwi$ a v iolet lilter having

a nraxinrum ear420 nm and a l ight pathof 4 to 5 cm.

7.2 Stopv, cl\ if the magneticstjrrcr is not equipped

witl'r arl ac curattsimer.

7.1 Measuring Spool,capicity 0.2 to 0.3 mL.

7.4 Iriltcr photornctcrs nd photonrctric ructiccs rc-

scribccl n {his test nrethodshrll conform o Practice

E 601 spcctr{)photon'rcterracticcssltnll conform toPracticcE 275.

li. lleagcnts

8,1 Pttitr oJ-Retgetts Reagenr radechemicals

shli l l l)c uscd in i l l l tcsts.Unlcssothcfwisc trdicatcd,rl is rIrtcIl(1.(lltirt il l l reagcnl$ l)lll co|llbrnl to th cspecil ic ionsol the CoDlmittee n AnalyricnlReagentsol (he Amcrican ChcmicalSociety.Otlrergradesna yirc used,y>roviclcdt is first {sccdaincd hat he reaBentis ol suli icicnrlyhigh purity to pcrn)ir rs use withoutlJsjJr)iu :lc uccuracyof the delcrutlinxtio,l.

8.2 l 'ut ir . t , , I lvatcr - Unlcis otlrr:rrviscndicated,referenccso u,ater hallbe undcrsloodo tnean eirgentwlltcr conibnrl inlt to SpccijictriorlD 1193,Type III-

8,3 Barium Chloritle- Crystals of barium chloride(BaCl2 2H20)screenedo 20 to 30 mesh.To prepare

.in the laboratory, spread crystals over a large watchglass, esiccateor 24 h, screeno removeany crystalsthatarenot 20 to 30 mesh, ndstore n a clean,dry ar.

8.4Conditioning eagent Place 0 mL of concen-tnted hydrochloric cid (HCl, sp gr Ll9),300 mLreagentwater,100ml- 957oethanol r isopropanolnd?5 g sodiumchloride NaCl) in a container.Add 50mL glyceroiand mix.

8.5 SulfateSolution,Sandard (l mL = 0.100mgSOr--) - Dissolve0.1479g of anhydrous odiumsulfate Na2SOa)n water, and dilute with water toI L in a volumetric lask

9. Sampling

9.1 Collect he sample n accordance ith PracticeD 1066,Specification 1192,andPractices 3370,rs applicable.

10. Calibration

10.1Follow heprocedureiven o Section l, usingappropriate mountsof the standard ulfate solutior,preparedn accordanceith8.5andprepare calibrationcurve showingsulfate on content n milligramsper

litre plottedagainsthe correspondinghotometeread-ings Note ). Prepare tandardsy dilutingwirh water0.0,2.0,5.0, 10.0,15.0, 0.0,30.0,and40.0 nrl- ofstand d sulfate olutiono 100-mL olumesn volul])er-ric flasks. hese olutionsvill havesulfate on concen-trationsof 0.0, 2.0, 5.0, 10.0, 15.0, 20.0, 30.0, and40.0m/L (ppm), espectively.

NOTE I - A scparatc ,.ialibration curve must tle prepared for eachpholoDrclcr and a ,)rw curye murt be prcprred jf il , neccsstry n)changc hc ccll, lamp, or frl tcr, or if any orlrcrakeftrtionsofi||strunrcntor reagenlsare made-Check rhe curve wirh each serics of tests byrunning two or morc solutions of known sulfate concenfadons,

11. Procedure

1l.I Filter the srn)ple f ir is turbid, and adjusr lretenrperalure o betwcen 15 and 30"C-

11.2 Pipet into a 250-mL beaker 100 mL or less ofthe cle . samplecontaining between0.5 and 4 mg ofsulfate ion (Note 2). Dilute to 100 mL with water ifrequired, and add 5.0 mL of conditioning reagcnt(Nore l).

oaa

aooaoa

aooaoo

ool

oo

45 0



l r i

ARTICLE 24 - I,IQIJID PENETRANT STANDARDS sD.s16

NOTE 2 - The sotubiliry of BaSO. i6 such that difficulry may be

experienced n thc deteaohatio[ of sulfatc conccntrationsbclovabout 5 mg/L (ppm), Thb can be overcomcby colccntratint lhe

sample or by adding 5 dtr of dtrlrdard $tlfatc-solutiol O mL =

0.100 mg SOr--) to thc taEplc bcforE dilutiDg to 100 mI- This

will add O-5mg SO,t o thc ssmpL. which mu$ bc subFrctcd rom

TABLE

OVERALL5/) ANDSINGLE.OPERATORSO)STANDARDEVIATIONSGAINST EAN

CONCENTRATIONORNTERLABORATORYRECOVERYFSULFATEFROMREAGENTWATER'4

the frnal result.

11.3 Mix in the stining aPParatus.

11.4 while the solution s being stirred,add a

measured poonfulof BaCl2 crystals(0.3 g) and begin

timing immediatelY.

11.5 Stir exactly1.0 min at constant peed.

NOT 3 - The sii.ring shouldhc at a consbnt rale n all delcrmin _

r;ons-The use of a magnctic atfulcrhi.s becnfound satisfactoryorthis purposc.

11.6 mmediately fr€r hestirringperiodhasended,

pour soludon nto the cell and measureh€' urbidity

at 30-s intervals or 4 min. Recordthe maximum

readingobtainedn the 4-min Period

1I.7 If the samplecontains olor or turbidity, un

a sanrplc lankusing heprocedurel.2 throughl. 6

without thc additionof the bariumchloridc.

11.,3f interferencesresusPectcd,ilute he sample

\r'ith an equal volumeof water, and determinehe

sullatcconcentrationgain. f the valueso determinedis one half that in the undiluted ample,nterferences

lu)aybe assumedo be absent.

12. Calculation

l2.l Convert he pholometereadings btainedvith

thc sample o milligramsper litre sulfate on (SOl--)

by uscof the calibration urvedescribedn Section 0.

13. Precisionand Bias

13.1 Theprecisionandbiasdatapresentedn this test

method meet the requirements f Practice D 2777-86.

13.2Theoverallandsingle-oPeratorrecision f the

test method;within its designated ange, varies with

the quantity being tested actording to Table I for

reagent water and Table 2 for drinking, ground, and

surfacewaters.

13.2.1Sevenabontories articipatedn theround

robin at three evels n triplicate,makinga totalof 2l

lrleanConcentratlonX),

mg/L

StandardDeviation,mg/L

1-0

2. 5

r The estmethods inearo 40 mg/L Tesling t the63.9 evel as

accomplishedhro gh i lut ion sdescribedn 11.2.

TABLEOVERALLSI)ANDSINGLE.OPERATOR50)

STANDARDEVIAIIONSGAINST-MAN

CONCENTRATIONORNTERLAEORATORYRECOVERY FSULFATEFROMDRINI(ING,GROUND,

A[D SU FACWATERN

Standnrd evilt ion, ) /L

SsI

20.4

0 .1

0 .4

s"MeanConcentration') ,

mq/L

6. 9

24.2

h3 .3I

The estmethod s l inearto 40 nlgl l , Tesl ing t lhe 69.9 lel 'e l$ '45

accomplishedhrouqhdi lut ionas descr ibedn I1.2.

observationsat each lcvcl for relgent water and for

matrix wrter (drinking, ground, and suriaca water).

13.3 Recovcriesof known amountsof sulfate from

reagentwater ancldrinking, ground, and surfacewatcrs

are as shown in Table 3.

13,3.1A tabte ot estimating he bias of the test

mcthod throuilh its ltpplic:tblc concentrationrange canbe found in Trlrlc 4.

13.3,2Thesecollaborative est data were obtaincd

on reagentgrtdc water and nilturalwaters.For other

matrices, thcse dala may not aPPIY

14. Keyrvords

14.1 drinking watet; ground wateri sulflrt elsurfuce

water; turbidimctric

0 . 7

2 .24 .5

0 . 5

1 . 8

1 .6

4 5 1



sD-5r6

aoaaaooaoooo

oaaooa

oaot

ao

aaI

oaO

ocaI

a

;5

fr

2OOISECTIONV

TABLEDETERMINATIONOFBIAS4 TABLE

*,',"1Tir1ijtii#..,i,iif,y"ilffl il.'.,^^,. _?r-v^r.s.r.0ll. 0wNoRNrERLABonaroi

. -mountAdded,mglL

AmountFound,mg/L

Statistica

Significantat 5% Level

lBias :%8i"s (ar : 0.05)

Reageniwater 20 .863.947 ,0

Drinking,ground

and str face

waler 20.8

6.gn

7, o

20.4 -0,4 _1.9v"63.7A -a.2 -0.2"/"

6.6 -a.4 _5.30/6

24.2 -0.6 _1.7V"

63.34 -0.6 -0.i./"

6 ,9 -0 .1 _1 .8%

NoNO

No

FJ^r"TlyLrlL R̂.qc-oveniesu _rnrERoREAGENTWATERANDDRINKiNG-, ROUND,NDSURFACEATER,

MeanSurface ecovery,11,ng/L

Reagent ater Sr) MatrixWater .ta)

SufateAdde4 g/L

7.O20.a63.9

l{ol o

No

6.6 (0.5)

20.4 1.0)

63.7 (2.5)

6.9 (0.7)

20.2 2.2)

63.3Q.5)

-lil,ll:Ji,I"..'"''.ll"'.too'y1--al,;lllffil]fiffi ;"*:::::J:'l-"-1r:IT:'toqo'?uT"f,igu-iiiiril;Ecconrptishedt rorsh itutions d s;r,;;;:;,ri:;l accomplishedhroushit"tio"u. aiririO"O'ii'rijl

API'ENDIX

(Nonmandatory Information)

t1.It r.lgIArE .oRDrscoNt,rNuArroN0Ir l\.lttT[toDS

X7.l (iruvine t c:

_" I ,t . , Th is . lc r t re t l )oJ as l iscor r r i r rucdn I9gg.r , lc r ( . \ f n tc tnodnr i ly bc four ]d t nc lgg i A t tnuu l

BrtoLol A,ll 'I4 Stqnrktrrls, ol ll.t)1.. l . l tc

Icsrntctho.l*,irs or.j-qin li-yssucij l J93lJ.

. ) t , , . . ,T l r is rcs tn) r , r i r , )L lo \ .c : " i , . ( jJ tc ln inr r ion

( ' r . fu / t , r tcn qr ter andwi ts lcw l lcJ . r t r , rp losonta in in"lrur)r ft) to 100 rlg/L sulfatc rnli I,c iuj l lyzed.

. .* , . , , . : S l r r r rc . I r ' cc i I r r r , , . , rr l ) . rwcr , , l l l cd r \

r ) ; l I l ' ln lu l i , , , l l r c r r . r , f l l o r i l i , r r r , lo t l rc rnso lub lcD t i l I l c l .

,

X1.1.4 l'histc.sr rcrhodwas (trs(ontinucd

becauseIlrcrcu('t-c r)suflicicllLabornt()ricslt( :rcstedn pafl ici_l)ating iD lDothcr coll boraljvc srul]t) ,o obtajn th e

11":lt:yyprccision and bias rs rcquirectby pracrice

D 1111.

Xl.2 Volunetric:

_.Xl. l . l This estmethodwrs discontinucdn l9tig.Thc. test method

nray be found tn the lggg AnttualBook of ASTM Standarcls,Vcl l l_01. fll* t"rt rlr"rflJiwas onginally issued n 1959as a non-refereemetho(

lj:,j l ' :1.1"hc prirnrry nrcrhod n rhc t9S0 ijsrr. L) ll 'csl

Mcthod D 5i6

..X-1.2.2 his tesrmethodcovers he dcterrnir:r{iorr

of sulfate n industrial water. San)plescontai.ning ;o;;5 to 1000 mg/L of sulfate m0y be anatyzed.

.X1.2.3 Sulfalc $ titratcd n an alcoholicsollttiorr

ur:oer ontrolled cidcondit ionswith a stan<iardariu|lrchloridesolutionusing horin as fie indicator.

. X7,2.4 This testmethod was discontinucdbccausctherewcre insuflicient laboraroriesnterestedh p*i"l-pating in another collaborative study to oUtuln tf.,"necessaryprecision and bias as required by practicci 111'1

452



ffi fill,l. Scope

1.1 This test method covers he determination f

chlorine n lubricatingoils andgreases,ncludingnew

and used ubricatingoils andgreasesontaining ddi-tives,and n additive oncentrates.ts range f applica-

bility is 0.1 to 507ochlorine.The procedure ssumes

that compoundsontaining alogens ther hanchlorine

will not be present.

1.2 The preferred nits arc masspercentand SI.

1.3 This standud does not purport to address all

c.,f he safetyconcems, f any, associatedwith its use-It is tlrc responsibility of the user of this standard to

establishappropriate sdfety and healthpractices andrlerennine the applicability of regulatory limitations

PrQr to u|e.

2, Refcrenced Docurnents2.1 ASTM Standards:

D 1193 Specification or ReagentWater

D 4057 Practice or Manual Samplingof Petroleumand

IrcrrolcumProducts

3. Summary of Test Mefliod

3.1 The sample s oxidized by combustion n a bomb

conraining oxygen under pressurc (Caution - See

Note l). The chlorine compounds hus liberatedare

rbsorbed n a sodium carbonate olutionand he amountof chlorine present-s determined gravimetrically by

DreciDitationas silver chloride.

STANDARD .TESTMETHOD FOR

CHLORINE IN NEW AND USED PETROLEUM

PRODU.CTS BOMB METHOD)

. sD-808

(Identicat ith ASTM D 808-95)

NOT€ l: (Ceution - Safct - Slrict adherence o all of lhc

provisions prescribedherciniftcr ensurcs ngrinst erPlosive ruptDre

of thc bomb, or a hlow-out, provided lhc lornb is of propcr dcsiSn

and cons(rlction ad in good Jncchanicnlcondilion, It is d€sirable,

however, tbat the bomb bc €ncloscd in a shield of st€el plate at

l€asi l3 mm (% in.) thick. or equivirlenl protcction he provided

agsinst unforseeablcconlingeDcics.

4. Significancc and Usc

4.1 This test method nray be used to measure thc

level of chlorine-contai ring ompounds n petroleum

products.This knowledgecan bc used to Predictper-

formance or handling chlracteris(icsof the product in

questioIl.

5. Apparatus

5.1 Bonb, having a crrprcityof not lcss thrn 300

n]L, so constructedhat;t will rot lerk during the test,

and that quantita tive ecovcryof the liquids from thebomb m y be readily chicvcd.

' l ' l reinner surfaceof

the bo nrb may be nradcof stainlcss lcol or any otber

material lrxt will nol bc offcc tcd by thc cornbustion

proccss r products.Mrt(:riirls sccln thc bontb assctn-

bly, such s thc hcrd grsket:tnd lerd-wire nsulation,

shallbe resistanto heatandc)rcmicalct ion, and shall

not undergoany reaction hlt wil l affcct the chlorine

Jontentof the liquid in the bomr.r.

5.2 SanpleCap,platinum, 4 nrnr n outsidc ian'rctcr

at thc bottom,2? mm in outsidcdianretcr t the top,

l2 mm in he ightouts idc, nd wcigh ing10 to l l g .

5.3 Firing l Vlre,phtinunr,No- 26 B & S gage0.41

(16 thou) ,27 SWG or cqr r iv r lcn t .

453



sD.80lJ

aatoI

I

aaI

I

oI

eI

t

:OO;SECTION

5-4 gnitiott Clrrair, caprLblq f supplyingsufficicntcuffent to ignite the nyJon hreador cotton wickingwrthout nlelliDg he wirc-

5.4.1I'he

switch in thc ignition circuit shall beol a typc hat rcntains pen,exceprwhen

hcld n closedposit ionby tl)e operator.

5.5 Nylon Sewing Threotl, or Co ,on Ilticking, white.

,5.6 Filter Crricr&Ic, fritted-glass, 30-mL capacity,nediurn porosity,

6, Rexgentsand l\.Iatcrials

6.1 Puritl, of Reagent:; Reagentgrade chemicalsshall bc used n ail tests,Unlessotherwise ndicated,rt rs rntended hat all rcagenCshall conform to thespecif ications

f the Comlnittec n AnalyticalReageltsof the American ChernicalSocicty, *treie suctrsplln_catio s are available. Otlrer gradesmay be used',pro-vrdcd it is lirst asccrtained that the reagent is ofsuff icienrlyhigh purity to permit ts use without ess_ening the accuracvof tbe detcmination.

6.2 PuriD. of Water - Unless otherwise ndicated,rcferences o tvafcr shali be understood o mean reagentwaler as dcfined by Type II or III of SpecificationD I 1 9 3 .

6.3 Nlrric Acil ( l + I) - Mix equal volumesofconccnrratcd itr ic acid (JjNO1.sp gr 1.42)and water.

6.4 Otlgru. i lcc olcornLru,rible arcrial nd halogencompoulcls, vaihblc at a pressure f 4t tgf/cm, i4 0atnros). Wxr-ning - Scc Norc 2.)

NO'rE 2: l\,arning - Orygen vigorously accelcratcs ombuslion.

6.3 Silter Nitrete So/utiot (50 g AgNO3/L) _ Dis_solve 50 g of si lver nitrare (AgNO3) in water an ddi lu lc to I L .

6.6 Sodiun C( rbonarcSolution (50 g Na2CO3/L)Dissolve 50g of anhydrous arCO3. g.5g of NarbO,

H1O, or 135 g oi NaICO-I i0 H2O i,r *ot"i au i

dilurc ro I l-.

6.'1 llhirc Jil refined.

7 . Sur r rp l in

7.1 l 'akcsln'tplcsn lccodllnce with the ostlgctions

in PlacticcD .1057.

.7.?T|ke carc hirt hc srlDplc sthoroughly cprcsenta_

trvc of the nti l tcr inl o bD rcstcdand lhat the poftion

TABLEQUANTITIESFSAMPLENDWHITE IL

Chlorin€Content, -.

% Weighr. f Sample, Weighrof WhireOit,q

0 .00. 40- 6o .7

0. 7

of the sampleused or the test s thoroughly representa-tive of the whole sample.

8. Procedure

,8,1Preparationof Bomb and Sample_ Cut a piece

of firing wire approximately t00 mm in lensth. Coilrhe middle section(abour 20 mm) and attach the freeends to the terminals.Arange the coil so that it willbe above and to one side of the sampte cup. Insertinto the coil a nylon thread,or wisp ofiotton, of suchlength that one end will extend into the sample cup.Place about 5 nrl- of Na2CO3solution in ttre toniband by meansof a rubber policeman, wet the interiorsurface.of he bomb, including the head,as. horoughlyas possible. ntroduce nto the samplecup tl,e quantitlesof sample and white oil (Notes 3

and 4) specif,ed nTable I (Caution - Note 5), weighing he sample othe nearest0.2 mg. (When white oil is used. stir tlremixturewith a shon length of quaftz rod and allow therod to remain n the samplecup during the combustion.)

8.1.1 After repeateduse of the bomb for chlorinedetermination,a film may be noticed on the innersurface. This dullness can be removed by periodicpolishingof the bomb. A satisfactorymethod for doingthis is to rotare he bomb in a lathe at about 300 rpmand polish the inside with Grit No. 2/0 or equivallntpeper oatcdwith a i ight machine il to prevcnicuuing,and then with a paste

ofgrit_free

chromic oxide andwater. This procedurewill remove all but yery deeopitsand put a highpolishon the surface.Aeforeusinithe bomb wash it with soap and warer to remove oilor paste eft from the polishing operation.Bombs withporousor pitted surfacesshould never be usedbecauscof the tendency o retain chtorine fronr sample tosample.

8.1.2 When the sample is not readily misciblewith white oil, some other nonvolatile, chlorine-frcecombustiblediluent may be employed n place of white

2 and underAbove to 5, inclAbove5 to lO, inclAbove10 to 20, inclAbove 0 to 50, ncl

0. B0. 4o, 20.r0.05

aoo

aott

I

I

te,

aI

o

tooao



TABLEGAGE RESSURE

MilimumGagePtesure,, gf/cmz

Capacityf Bomb,mL (atn)

MaxinumGagePresure,' gflcrn2

- . (ah)

4r (40)

38 (37)

33 132)30 129'

" Theminimumpressurcsre speclfiedQprovide ufficient rygenfor completecombustion,and the maximumpressures cpresentasafetyrequiretuent.

oil. However, the combinedweight of sampleandnonvolatilediluentshall not exceed g. Somesolidadditives re elativelynsoluble, ut maybesatisfacto-rily bumedwhencoveredwith a layerof white oil.

NOTE 3 - The practice of running altedarely high ard low samptesin chlorine content shall bc aroidcd whenever possibla, It is difficulrto .inse lhe last traces of chlodne from thc walls of the bomb andLhe tendency for residual chlorinc to carry over from sample tosampie has been observed io a number of laboratories.When asample high in chlorine has precedcdone low in chlorine contcnt,lhe (est on the low-chlorinc sample shnlJ be repeatedand one orboth of the low values thus obtnincd caq be consideredsuspec( f

lhcy do not agrce wjthin thc limits of repeatabiliryof this method-'

F"OTE 4: Ctutioll - Do Dot usc mo(e than I g to(al of sarnplelnd whi(e oil or other chlorine-ftec comburtible matcrbl.

8.2 Addition of Oxygen Place he samplecup inposition ndarrangehenylon hread, r wispof cotton,so that the end dips into the sample.Assemblehebonlb and tighten he cover secudy. Admit oxygen(Caution - SeeNote 8) slowly (to avoid blowingthe oil from the cup) until a prcssures reached sindicatedn Table2.

NOTE 5: Caulion - Do not add oxyge[ o ignilc rhe sample flhe bomb ha9 been aficn,

dropped,or tiltcd.8.3 Combustion- Immersethe bomb in a cold

waterbath. Connect heterminals o the openelectricalcircuit.Close he circuit to ig[ite the sample.Removethe bomb from the bath after immersionfor at leastl0 min. Release he pressureat a slow, uniform ratesuch that the operationrequiresnot less than 1 min.Open he bomb and examinehe contents.f tracesofunbumedoil or sooty depositsare found, discard thedetermination,nd thoroughly lean he bomb beforeagain utting t in use 8.i.1).

8.4 Collection oJ Chlorine Solution - Rinse the

interiorof the bofnb, he sample up, and the irnersurfacedf the bomb coverwith a fine et of water,and collect the washingsn a 60GmL beaker.Scrub

300 0 35 0

350 o 40 0

400 o 450450 o 500

39 (38l

36 (35)

3I /.JO'

2a (21)

'ARTICLE 24 _ LIQUID PENETRANTSTANDARDS sD-808

the interior of the bomb and the inner surfaceof thebomb cover with a rubber policeman. Wash the baseof the terminals until the wastringsare neuaal to theindicator methyl red. (The yolume of the washings isnomally ir excess of 300 mL.) Take special care ootto lose any wash water.

8.5 Detenninationof Chlorine- Acidify the solutionby adding HNO3 (1 + l) drop by drop unril acid tomethyl red. Add an cxccss of 2 mL of the HNO3solution.Filter through a qualitative paper [if tbe solu-t ion is cloudy, thc prescncc f lead chtoride PbCJ2)is indicatedand the.solurionshould be brousht to a

boil before filteringl rnd collecr in a second00-ml-beaker.Heat the solution to about 60'C (140.F) and.while protecting the solution from strong light, addgradually,while stining. 5 nrL of AgNO3 solution.Heat to incipient boiiing and retain ar this temperatureuntil the supernatant iquid bilcomcsclear. Tcst toensure omplc(eprccipilalionby xdding a few dropsof the AgNO3 solution. If nrore precipitation takesplace, repeat dre above steps which have inyolvedheating, stirring. and adCirion of AgNO3, as often asnecessary, ntil thc additionrl d.aps of AgNO3 produceno turbidity n the clcrr, sulernatrnt iquid. Allow rhe

beaker and contents to stand in a dark Dlace for atlcast an hour. Filter the prccipitrrte y slcr ion on aweighed ritt'ed-glassilter cmciblc. Washthe precipitatewith watercontaining2 nL of HNO3 (l + 1)lL, Drythe crucible and precipitateat ll0'C for I h- Cool ina desiccator,and weigh.

E.6 Blank - Make a blank detennination with 0.7to 0.8 g of white oil by following the normal procedurebut omitting the sample (Notes 6 and 9). Repeat thisblank wheoever new batchesof reitgentsor white oilafe used. The blank rnust not exceed 0,03% chlorinebasedupon the weight of the white oil.

NOTE 6 - llis procedure measureschlorine in lhe while oil andio th€ rcrgents used, as well as thar inkoduced from conramination.

9. Calculation

9.1 Calculatc he chlorinecontentof thc sampleasfollows:

Chlorine,massS" = l(P - B) x Z4.74lttl

where:

P= gramsof AgCl obttrincd rom the sample,8= gramsof AgCl obtained rom the blank, :rndW= gramsof sampleused-



2001 EcTroN

ooaoooooaaoaO

t

oooo

aacI

oo

aaoO

oo

ooaoa

10. Precision and-l l ias

10.1The precision f this testmethod s not hiownto hilvc been obtailed in accordancewitfi cunendvrcceprcdguidclincs for crample, n CommitrceD_ iResearchReporr RR:D2-100?,Manual on Dererminins

PrecisionDltl lbr ASTM Methods n petroleum rod_ucts and Lubricants).

10.2 The precision of this test method ts obtained.by statisticalexanination of interlaboratory est resultsis as follows:

10.2,1 Repeatability - The difference betweensuccessrye est results obtainedby the same operatorwith rhcsamcafnar tusunder onstant pcrating ondi_tions on identictl test mate al would, in the long run,in the normal and conect operationof the test niethjcxceed he following r,alues nly in onc case n twenty:

twosingleand ndependeDtesults btained y differenroperatoru orking n differcnt aboratoriesn identicaltestmaterialwould, in the long rua, in tbe normal anrlcorrect perationf the estmethod xceedhe oltowingvalues nly n onecase n lwenty:

Chlorine, %

0.1 o 1.92,0 o 5.0Above5.0

lO.3 Bias:

1I. Keywor&

11.1bomb; chlorine

103.1 Coope&tivedata ndicate batdeviationsoftestrcsults rom the true chlorineconfent_are.ofhesameorder of magnitudeas the reproducibility.

10.3.2 t is not practicableo specify he bi4softhis test method or measuring hlorinebecauseheresponsible ubcommittee,fter diligent search,wasunable o attractvolunteersor an interlaboratorystudv.

Reproducibility

0 .100.x0

5%of smouitpresent

Chloripe,./c. 0 - i ro .9

2.0 o 5. 0Abovc .0

Repea(ability

0.0.10 , t 5

3%of amovDlpresent

10.2.2 Raproducibili4,- The difterencebetween

456



.L Scope

1.1 This test methodcoven three proceduresor thedetermination f total sulfur- n peffoleumproductsincluding ubricatlngoils containing dditives, nd inadditiveconcentrates.his estmethods applicableosamples oiling above 7?'C (350.F)and containingnot less than 0.06 mass% sulfur. Two of the threeprocedures se iodatedetectio.n:ne employinganinduction fumace for pyro$sis, the other a resistancefumace.

Thethird procedue

use$R detection ollowingpyrolysis n a resistanceumace.

1.2 Petroleumcokecodtainingup to 8 mass% sulfurcan be analyzed.

1.3 This standardmay involve hazardous nnterials,operations, and equipment.This standard does notlrurpon n address all of thz safety concems, f any,associated with its use. It is the responsibilityof theuser of tltis standard to estoblish appropiate safetyawl health practices and determine he applicabilityof regulatory limitatioru

pior to use.

2. Referenced Documents'

2.1 ASiM Standards:D I 193Specificationor ReagentWaterD 1266Test Method for SuIfur in PetroleumProducts

(LampMethod)D 4057Practice or ManualSamplingof Petroleumand

Petroleum roducts

3. Summary of Test Method

3.1 lodate Detectiort lyste,'r The sample s burnedin a sream of oxygen at a sufliciently high ternpcrrtureto co nven about 97% of the sulfur to sulfur dioxide.A standardiz-a(ionactor is employed to obtain accuritteresults.Thc combustionproducts rc passcd nto anabsorber ontaining nacidsolution f potassiumodideand starch ndicator, A faint blue color is developedin the absorber solution by the ,ddilion of starrdard

potassium iodate solution. As combustion proceeds,bleaching the blue colo( more iodate is added. TheaDount of standardodateconsumedduring thecombus-tion is a measureof the sulfur content of the santple,

3.2 IR Detectiort System Tbe sanrple s weighedinto a special ceramic boat which is then placed intoa combustion urnacear l37l'C (2500'F) in an oxygenatmospherc,Most sulfur preseot s combustedto SO2which is then mealured with an infrared detectoraftermois(ureanddus( areremovedby traps. A microproces-sor calculatesdle mass percentsulfur fron the sampleweight, the integrar€ddetector signal, and a predeter-

mined catibration factor. Both thc sxrlrplc den(ifica(ionnumber and mass pe.cenl sulfur ate. then printed out.The calibration actor is detenrrincdusing standlrdsapproximating the marerial to be lnalyzed.

4. Significancc and Use

4.1 This testmethodprovides meansof monitoringthe sulfur level of various petroleum products andadditives. This knowledge can be used to predict pcr-formaoce, handling, o. processingpropenies. In some

cases he prcscnceof sulfur cornpounds s bcncficial

SULFTIR IN PETROLEUM PRODUCTS

STANDARDTEST METHOD FOR

sD-1552

(IdeBticalwith ASTM D 1552-95)

(HIGH.TEMPERATUREMETHOD)

(ilt,

45'7



sD-15s2 2OOISECTIONV

I

t

I

0

oI

taaooO

aat

ooo

taoaoI

aat

aIt

o

It

ooa

to rhe productand monitoring he depletion f sulfurcan provide uselul inforntltion. In orher cases h:presencc f sulfur cornpounds s detrimental o the

Drn(c)5inS r use of the l)rodrrcl.

5. Interlercnccs

5.1 For the odate ystents,hlorine n concenta tionsless thair I mass 96 does not interfcre.The IR systencan lolcriLte onrervhat ighcr concentrations.itrogenwhen present in excessof 0.1 ruass7o may interferewith thc jodatesysrems; hc extent of such nterferencemay bc dependent n the type of nitrogcncompoundas wcll as trte combustion onditions.Nitrogendoesnol inrerferewidr the IR system.The alkati and alkalineeanh netals, as rvell as zinc, phosphorus,and Iead,do not intcrrerewith ejthersystenl.

6. Apparatus

6.1 Cotnbtrstiottand lodate L)durio srstetn

6-1.1 Funtttces- Trvo ntljor rypesare available,(he p.intarydiffercncebeing he rnrnner n which th enecessury iglt ternperuturesle ohtoined. hese wotypes arc as follows:

\6.1.1.1 nductionT)pc, which dcpencispon he

high-frcqucncy lectrical nductionmethodof heatilg.

This asseltbly shallbc capable f a aininga temperatureof at least l4g2"C (2'100"F) D tho sample combustionzone,undcr he conditions ct /br(h n Section 0 andshall lrr: crlL:ippctlwirh rrrr rrili: ionirl nductioncoillocatcd al' ]ovcLl)ecorrbustionzonc, substanti i t l ly sshown u F ig . I .

6.1.1.2 Thc furnace vork coil should have amrriDun) outprt of 500 W; (he ntinimum nput ratingof thc I'urnlcc nlust bc 1000 W. With thc conectanronnt i iran chips,weighcd o: 0.05g, thc nraximumpla{ecurrc)nt ,il l bc between 50 and 450 mA.

NOTE l :l \ ' r r rni | lg

-- f t r isrypc ot nrnrrcc s crpableof inf l icr inghi-qh rcqu.ncy Lrums Jrd high-\'ottrge shocks. Ilt addirion ro otbei

piccnutions. mrinr;rin all gurrds properly. prccxution - Disconnectlhc fum?cc fro the fower line whenevcr clectrical repa;s or'ndiustmcnt irrc nrrdc.

6.1.1,3Resistattct.. tpc, apabJe f naintaininga ternpcr:rtrrrci ar lcmL 1371"C 2 500"F).

6-1.2 Absorher, as dcscribed n Test MethodD 1266.

FIG. COMBUSTIONUBE

NOTE: - Also suirablc or use*irh ei{her ypeof furnaer s i. rautomalic irraror,specificallydesignedor iodometry,This combjnesthe unclions f absorptioland iration o a predeterminedodpoint.

6.1.3 Buret, st.lndard 25-mL or automatic typesavailablc rom thc manufacturcrs f the sf,ccificcort)l s-tio$ units, are suitable (Note 2).

6.2 Combustionand lR Detection.syrreri, comprisedof auiomatic balance, oxygen 0ow contols, dryingtubes,combustion umace, infrareddetectorand micro-processor.The fumace shall be capableof maintaininga nominal operating temperatureof I350.C (2460.F).

6.3 MiscellaneousApparalas - Specific combustionassemblies equire additional equipmentsuch as cruci-bles, combustion boats, crucible lids, boat pushers,separatordisks, combustion tubes, sample insetters,oxygen flow indicator, and oxygen drying trains. Theadditionalequipmentrequired s dependenton the typeof fumace usedand is available rom the mnnuf4q1x...of dre specinc combustion unit. To attain the lowersulfur concentrationgiven in Section l, the ceramicsused with the induction fumace rssembly shall be

Secondaryheatet

Vycor tube

ltl

I

.tt'4.

'&rt



i:i:{-1i::: l

:j:i';:jar:i':,i

ARTICLE 24 _ LIQUID PENETRANTSTANDARDS sD-1552

7.7t Potassitonodare,StandardSolution 0.01248M, I mL = 0.2 mg S) - Measure xacrly200 mLof KIO3 solution 0.06238M, 1 mL = I mg S) inroa l-L volumetriclaskanddilute o volumewith water.Thoroughlymix the solotion.

7.12 Ascaite, 8 to 20 mesh.

7.13SpecialMatcrials for lruIuction"TypeFurrlc"s,

7.13.1Tin (20 to 30-mesh).

7.13.2 ron-ChipAccelcrotorhavinga sulfurcon-tentof not more then0.005mass7o.

7.14Standard antplc Porassiumlunl AlK(SOa)2. t2Hzol

7.15 Starch-IoelideSolution - Make a paste byadding 9 g of soluble starch ro 15 nrl. of water. Addthis mixture, with stirring, to 500 mL of boiling watcr.Cool the mixlure,add 15 g of potassiumodide (Kt),

and dilute to I L with watcr.

7.16Sul/uricAcit l (rcl l t ivc dcnsity J.84) Concen-trated sulfuric acid (l I?SOa).

NOTE6: Wsrning Pois.ir.Corrosive.{roDgxidizer.

7.17 Vqnadiunt Pentoxide, anhydrous, powderedVzo:.

.8. Sampling

8.1 Take samples n accordancewith the instructionsin PracticeD 4057.

9. Preparation of Apparatus

9.1 Induction-TypeFurnace - Assemble he appara-tus according c the instructions urnishedby the manu-facturcr. Purify the oxygen by passing t rhrough (.1)H2SOa relativedensity 1.84), (2J Ascarite, and./J)magnesium perchlorate [MS(ClOq):] or phosphoruspentoxide (P2O5) Precaution - sce Note 3). Connecta rotameterbctween he purifying train and the fumace.Inserta small glass-wool lug in thc upperend of theglass ubing connec(ing hc urnaccwjlh the absorberto catch oxides of tin. Connect rhe exit end of the

combustion ube to the absorbcrwith glass tubing,usingguni nrbbcr ubing to nrlkc connections, osit ion

the absorber o xs to ntake his dclivcry ine as shortas

ignitedn a muffle umaceat l37l.C (2500"F)or atl e a s t 4 h b e f o r e u s e .

6.4 Sieve,60-mesh250-mm).

7. Reagentsand Materials

Z.t,ipur;ty of Reagenti-- Reagentgradechemicalsshall be used n all tests.Unlessotberwisendicated,it is intendedthat all reagentsshall conform to thespecifications f the Committeeon Analyical Reagentsof the AmericanChemicalSociety,where uchspecifi-cationsarc available.Other gradesmay be used, pro-vided it is first ascertained hat the reagent is ofsufficientlyhigh purity to permit ts use without ess-ening the accuracy f the determination.

7.2 Purity of Water - Unless otherwise ndicated,referenceso watershallbe understoodo mean eagentwater as definedby Type II or III of SpecificationD I 1 9 3 .

7.3 Ahtndnn (4120) or MagnesiunOride (Com-Aid).

7.4 Anhydrone(MagnesiumPerchlorate).

NOTE 3i Prccaulion - ln additiotr to olhe prccaurioos,handlemngnesiumpercltoratc with carE.Avoid contacringt with acid and

'

organic materials.Rcactio$ rdth fucl may bc violenl

7.5 Hydrochloic Acid (3 + 197) - Dilute 30 mLof concentratedydrochloric cid HCl,relative ensityl. l9) to 2 L with waler.

NOTE4: Wsrning Poison. on6ivc.May be atal f swallowed.t-iquidand vaporcausc cvarc ult|s.

7.6 Oxygen(Extra Dry) - The oxygen shall be atleast 99.5ol pure and show no detectablesulfur byblxnk determination.

NOTE5: Warnlng OxygFn igoaouslycccleratesombustion.

7.7 Phosphorus Pentoxide (P2Q).

7.8 Potassium Alum (Alwninum Pomssiun Sulfate).

7.9 Potassiun lodate, Standard Solution fi.06238

M I mL ='l mg S) - Dissolve2.225g of porassiumiodate (KIO3) that has been alried at about 180"C toconstantweight, in water and dilute to I L. Thoroughlymix the solution.

'1.10Potassium lodate, Standard Solution (A.fi6238

M, I mL = 0.1 mg S) - Measure exactty 100 mL

of KIO3 solution (0.06238M, I mL = I mg S) intor l-L volunretric lask,anddilute to volume with water.Tlroroughly mix the solution.

459



sD-1552

FIG.2 SCHEMATICLLUSTRATIONFINDUCTION.TYPEURNACE

TAB E1

SAlv'IPLEWEIGHTFOR NDUCTION URNACE

Absorbet

FIG. SCHEMATICLLUSTRATIONFRESISTANCE.TYPEURNAC

I A 6 L c . Z

SAIIPLE EI 'HTFOR ESISTANCEURNACE

2001 EcTroN v

I

att

]

t

t

oaI

I

t

oct

t

toIO

t

t

oo

aI

I

ot

t

ooooI

Normalityof Sl,andard

K[03Solut ionorTitration

0.006238

0_01248

0.06238(No te )

Weight f SampteSulfurContent/ o to Be Taken,mg

100 o 200100 o 200100 o 200(Note )

0 t o 22 l o 5

5 t o l 0

over 0

Veiqht f SampleS]llflr Content,/o to Be Taken,mg

Nornrality l StandarCKI03Solut ionor

Titration

0 t o 2

2 I a 4

4 1 o 1 0

over 10

90r50 o 90

50 0 901 2 . 1 . 1

0 ,005280.006238

0.01248(No te )

possible. igure2 illustrareschelr l i l t icallyheassembledlpprralus. Adjusr.he oxygcn iow to I r 0.05 Umin.Add 65 nrl- oi HCI (3 + 197) and 2 mL of srarch-iodidcsolution o thc absorbcr. dd a sufocient mounlot the npproprirle srandardKIO3 solurion (Table l) toproducea frint blue color. This color wil l serve asthe cnd poilt{ bf the titration.Adj[st the buret o zero.Turn on thc lurnace llamentswitch andallow at leastI min wrrnr-upbelbrc unning amplcsPrecaution

scc No(e 3).

9.2 Resistouce-'Ite Il.rt.tcc - Asselnblc he appara-tus rccordingo the nstructionsurnished y themanu-

tlc(ufcr. Purily thc oxygenby p;rssingr througb ^l)l l25Oa (rclarive dcnsiry 1.84). 2) Ascarite,and (J)Mg(CIO{): or P?Os Precaution- seeNote3). Connecra rotan]ctcr bctweeI the puriiying train and the fumace.Figure3 illustrates chernaticallyhe assembledppara-tus. Turn on thc cuoent itnd ildjust he furnacecontrolto nrlintirin it constlLntcntperature,i l3l6 + t4"C(2400 l 25"F). Adjust rhe oxygen llow rate to Z a0.1 L/min. AJd 65 ml- ol- FlCl (3 t I97) .rnd 2 nrlol sturch-iodicleolution to thc rbsorbct.Add a few

dropsof the appropdatestandarclKIO3 solution (Table2) to producea faint blue color. Adjust tbe buret to zero.

" ,.3 Resistance-Ttpe umace-IR Detectioa Assem-ble and adjust apparatusaccording to manufacturer'sins[ructions.nitialize microprocessor, heck power sup-plies, set oxygen pressureand flows and set furnacctemperature o l37l'C (2500"F).

9.3.I Condition a fresh anhydrone scrubber withfour coal samples.

93,2 Calibrate the automaticbalanceaccordingtomanufacturer'snstructions.

10. Standardization

10.1 For lodate Methods:

10.7.1Determination of Al.un Factor:

10,1.1.1 Because hese rapid combustionmcth-ods involve the reversible eaction2SO2 + 02 = lger,it is not possibleto evolve all the sulfur as SO?. Thcequilibrium of the reaction is temperaturedepcntlentand, in an oxygen atmosphere bove l3i6"C, about9'7o/o f the sulfur is prescn[ as SO2, To assurethatthe furnace s in properadjustnlentand that its operation

460



.i :':, ... : AR?ICI-E 24 _ LIQUID PENETRANT STANDARDS

prod_ucescceptablyhigh temperaturc, otassiumalumis eriiployed or standardizinghe

apparatus.Dependingon thd typeof combustiorr.equipmentsed,proceed sdescfibedn Sections0 tb 13 to determinehe alumfactor. Use tS mg weighird o *0.1 mg of potassiumalum or this determination se he samematerialsnthedeterminationf tbealumandsundardiz:atioractorsrs for the unknownsamples. or example,V2O5hasa definiteeffect and shouldbe included f used orunknowns s recommendedn the procedure ith thercsisrxnce-typeumace Note l0).

10.1.1.2C^lculate he alum factor as follows:

Alum ictor /F) = (glxWal[tm(V"- V) (t)x ctl

where:

S^= mass ercent ulfur n potassiumlum used,IV,e milligrams f potassiumlum used,y.,= millilitresof srandarrdlO3 solutionuscd n

determininghealum actor,y, = millilitresof standard IO3solution sedn the

blankdetermination,rdCr= sulfurequivalentf theshndardKIO3solution

used n determininghe alum factor, mg/ml.

10.1.1.3 he alum actorshouldbe in theransefrom 1.02 o 1.08. f values maller han 1.02aieobsewed, onfirm ndependentlyhe sulfur contentofthealum and the sulfur equivalentof the KIO3 solutionbefore epeatinghealum actordetermination.f valueslarger than 1.08 are observd make adjustmentsnthe equipment n accordancewith the manufacturer'srecommendationld repeat he alum factordetermi-nation.

10.1.2Determinationof StandardizationFactor:

10.1.2.1 ecauseffects uch ssample olatility

can also affect the daaive rccovcry as SO2 of thesulfur originally present n the samplq it is necessaryto determin€a standardizationactor. koceed as de-scdbed n Sections 0 to 13, usingan oil sampleofsimilar pe to the unkrownsample nd of accuratelyknownsulfurcgntent.

10.1.2,2For IR detection, etermine nd loadthe microprocessorwith the calibrationfaclor for theparticular )Te of sample o b€ analyzed ubricatingoil, petroleum oke, esidualuel)as recommendedytbe maflufacturer.

10.1.2.3Calirilate the standardizationactor aslbiiows:

sD-1552

Strandardizationactor F,) = (S, * W")I[OO L p)

- V ) x C t

wnetp:' 'S,= mass percent sulfur in standddization sample

used,

I/, = milligrams of standardization ample used,Vr= millilitres of. standardKIO3 solutionused n the

blank determination.

%= millil itres of standardKIO3 sclutionused ndeterminingthe standardizationactor,and

C= sulfur equivalentof the standardKIO3 solutionused n determining he standardizationactor,mg/mL.

10.13 Quality Control - Piuna suitableanalyticalquality control sample several times daily. When tbeobserved value lies bctween acceptable limits on aquality control chart, proceed r,vithsample dctermina-hons.

ll. Preparation of Coke

11.1 It is assumedbat a representativeamplcha sbeen received for analysis.

U.2 Crind and sieve the sample receivcd so as topass a 60-mesh (250-mm) sieve,

113 Dry the sieved material to constant weirht ar105 to I lO'C.

12. Procedure With Inducrion-Type Furnace

,l2.l Sanple Preparation - Add a 3.2 ro 4.8-mm(7r to Zr-in.) layer of alundumor magnesium xideto a sample crucible. Make a depression n the bedwith the end of a stiring rod. Weigh the crucible tq0.1 mg. Weigh into the depression

he pnoperamourtof sampleaccording o Table I (l2.l.l) (Note 7). Coverthe sample with a separatordisk (Note 8. place onth€ separator disk the predeterm;nedamount of ironchips necessary to obtain the required temperature(6.1.1.2).This is usually between1.2 and 2.0 g, bu tshould be held constant with 10.05 g. Sprinkle about0.1 g of tin on the iron. Cover the crucible with a li<tand place on the fumaca pedestal

12.1.1Under no conditionsshall an organic sanrplelarger than 100 mg be bumed in'an induction-typefumace,

NOTE - More onceoliled IO]solulions,uch s he0.06233nr' soludon, may be found .norc .o vedenr t6r ssmrtcs c.,nr.]iflifls

461



ta

sD-t552 at

2001SECTIONV

r ,'rc.rfixn .10%

$ullur. llle samplc sitr in,l KtOl concentrarionsr,c,utd c chojcn so rhnr not more thrn 25 mL of tilr3nl is oceded.

NOTE 8 - Thc lJs€of lhe sepaFror disk j oprional.

72.2 Cotnbustiortand Tiffatiotr _ Tum on the platecunent switch. After about.l min for warm_up,aise

the-pedestaland lc,ck into position. The plate cunentwill fluctuate for a few secondsand should graduallynse to a nlaximum value.Add the approprif,te tandardKIO3 solurion (Table l) to the absorber o maintainrl)c blue color. Should thc absorbersolution becomeconlpletely olorlcss, iscard he delermination. ak eKlOq 1al6li1i611*s the m(e of evolutionof SO3dinrin_ishes such thar, when combusrion is compleied, thejntensiryol.rhe blue color is thc sameas the initialintcnsily.Combus(ion s completcwhen this color re -nrains or at least I min and the plate current ha sdropped cor)siderably, ecord the volume of KIO3solution required to titrate

the SO2 evolved.12.3 jltuk De ernirrnlion _ Make a blankdetemtina_

tion lvlrcnevcr new supplyof crucibles,materials, rrelLgcn(ss uscd, .bllow tl.leprecedinElroccdure, ut0fitt the siluplc.

I3. Proccdur.eWith lksistltncc-.fypeFurnace

13.1Srlrryr/c'reltert i()tt ,Wcigh intoa colnbustionboal lhc pfopcr a|tou|t ol-slinple uccording o Tab]e2. Add 100 t -5 mg of vanrdiunrpentoxide nd com_p)ctclv covcr lhe rnixturc vir l tAlunclurn.

13.2 Coutbustionand Titntrion __ place thc boat inthe co()l lr(Jfti() ) l ' the conlhustion ube, ncar thecntrancc. b pnrcccclwith thq conlbLrstion,ush th cLroittorlLirinilurhe slLnrplerogrcssivelynto tle honerz-oncol lltc con)bustion ubc using thc equiplnentprovitlcd by t lrc nranuiacrurcrs..he bort should beadvarceci s ftrjridlyas possjble onsistcnt ith the ateol.evolulionol SO2.Add rhe ppropriatc tandard IO3solulion 'f i l l) lc2) to thc rlrsorl)cr o nraintlin ltc bluecok[. Shouirl ltc absortrcr ol tiot)bccorr]c onlplctclycotorlcss, i icrrd the dctcnnination.Mrke KIO] addi-t ioxs as rhc r,lle ol cvolLrt ion

l SO3rlinrinishe^suchtlrlt, wh(:,t cor1lbrrslions conrplctcrl,llc irrlcnsityoftht bluc' color is t l tc snn:c lrs thc inititl i ltcnsity.Conrbustions conlplctewhen this colol rcmains orat lcrst I min. Record he vclume oI KIO3 solutionrcquired o rirriite hc S02 evolvcd.

13.3 llanii [)ctcnnirratroa Make a blankdetermina-l ion whenever a new supply of colrbustion boats,rtlatcrials. r rcrsents s uscd. ro]low lreabovepro(:e_dnre, but ontit thc sanlple_

14. Procedure With ResistanceFurnace-IR Detection

14,1Allow the system o warm up and the furnaceto reachoperating emperature.

-14.2After homogeneity f the sampte s assured,select he sample izeas follows:for liquid samples,takeup to-0.13g for analysis nd for solia samples,ta.ke pto 0.4 g for analysis.n eachcase,masspeicenrsulfur times weight of samplemust be less than orequal o four in the caseof the SC32 nstrumen andtwo in, the caseof the SCl32 instrument. or otherrnstruments,,.onsult he manufacturer'snstructions.

14.3Determine nd store he systemblankvalue.

f4.4 Weighthe samplesnto combustion oatsandrecord he net weights. t. is possible o weish and

store seveftl weights in the microprocessoreforebeginning seriesof bums.

f4.4,1Filt thecombustion oat o one-third apac_ity with evenlyspreadMgO powder.

..14.4.2Form a slight trench n the MgO powder

with a scoop.

14.4.3Place he combustion oaton rhe balanceand weigh an appropriate mountof the saolplc ntothe trench n the MgO powder.Enter he wcfuht.

14.4.4 Remove he combustionboat from rhe

balanceand add MgO powder until the co bustionboat s filled to two-thirds apacity.

NOTII9.- lf nrcccpri lb lccpeitrbi l iLys cncounrcrL.Jnr pi ln ie lj.xr sjutu'rcs, onbusrron pronroter such as V?Or or lhu LtiCO prorlu.tLoDt-Aut can ba subsriruted or the MgO.

NOTE l0 - CautioD - \/.2O5 nn causedererjorlrion of rhc iurflr. (cerarnlcssO use rl uith c e_

14.5 Initiate oxygen florv and load boat into fumacc.

-I4.6_Wlrcn lhc anulysis s cotDplclc. ci ld th(, rcsull

rrom the microprocessor.

14.7 Remove the expended combustion bo:il frool(lrc firrnace.

l4.E Make repeaceduns until two results difl.er byless dtan the repeatabilityof the method.

15. Calculation

15.7 Calcukttiontor lodate Detuction - Calculatcthe sulfur content of the sample as follows:

at

oaaoaI

oO

oof

o

aO

oI

I

a

oat

aI

a

aooO

o

462



$

:,H.

.#. , :

i l '..

''Sulfur,mass% = llf0 (V - V) x F" x Qll|l (3)

ARTICI-E 24 _ LIQUID PENSTRANT Sf,ANDARDS

operators working in diffcrent loboratoricson identicaltest material would, in the long run, in the nomal and

V= standard KIO3 solution, ml. used in theanalysis, -: i: ,

Vr= standardKIO: solution,mL, used n theblankdeterminatiorL I

4= standardizationactor see10.1.2),C= sulfurequivalentf thestandard IO3solution

used r the analysis,mgn . ndI4: milligramsof sarnple sed n the analysis.

15.2 Calculationor IR Detection:

15.2.1Reportall rcsultsusing the rnicroprocessor.

15.2.2 Report the averageof two results.

16. Rcpod

16.1 n the rangehom 0.05 to 5.00 mass% sulfur,rcpon to the nearest0.01 mals %. In the range from5 to 30 mass% sulfur, eport o thenearest .1 mass%.

ing values n only one case n twenty:

17. Precision and Bias

l7.l For Petroleufl Prodacts by lodnte and IR

Methods - The precision of this test method as deter-

nined by statisticalexamination of interlaboratory e-

sults is as follows:

17.7.1 Repeatability - The difference between

two test results obtained by the same operator with

the same apparatus under constant operating conditions

on identical test material woUld, in the long run, in

the normal and conect operittion of the test method,

exceed he following values n only one case r twenty:

Rcp€ahbility

Iodate IRll

17.1.2Reproducibility The differencebetweentwo singleand ndependentesllB obtained y different

sD-15s2

Sulfur,Mals, %Range

O.0 o 0.50.5 101.0l . 0 lo 2 -0

2,0 to 3.0

3.0 o 4,0 .4.0 o 5,0

Reproducibilily

Iodate

0.08

0 . 1 I

0.1'7

0.260.400.s4

L7.2 For Petroleurn Cokes bylodate and lR Meth-ods - The precision of the test method as determined

by statistical examination of interlaboratory results is

as follows:

17.2.1 Repcatabiliry - The difference between

two test results obtaincd by lhe samc opcrator witlr

the sanreapparatusurlder constantoperating conditiol1s

on identical test mate al would, in the long run, in

the lormal and con'ect operatidn of the test method,

exceed he following values n only one case n twenty:

r = 0.05X

where X is the average of the two Lsst csults.

17.2.2 Reproducibilir) - The difference between

two single and independent esultsobtainedby different

operatorsworking in different laboratorieson identical

test material could, in thc long run, in the normal and

correct operation of tbe test method,exceed he follorv-

ing values in only one case in twenty:

R = 0.22X

where X is the average of the two (cst results.

17,3 Bias - The bias of the procedurc in this test

method is being deternrined.

18, Keywords

18.1 furnace; high tcmperature; induction fumace;

iodate titration; IR detection; petroleum; resistance:

sulfur; tiration

IR"

0 . 1 30.21

0.?'l

0.38

0,440.49

Sulfur,Mass,%

Raogc

0,0 ro0.50.5 ro 1.0

1.0 o 2.0

2.0 ro 3.03.0 ro 4.04.0 o 5.0

0.05 0.040.07 0.0?0.I0 0.090.16 0.120.22 0.r30.24 0.16

463



STANDARDTEST METHODFOR

sE-r65

(ldenticalwithASTM Specification 165-95)

1 Scope

1.1 Tl)is t(.srnrerhod overs roceduresor penetrant

cxlLn:inationf rlirterials. hcy are nondestructiveest-ing rncthods or detecting iscontinuitieshat are opento thc surlaccsuchas cracks,seanrs,aps,cold shuts,lantinations,hrough caks, or lack of fusion and arehpplicable o in-p rocess,inal, nd mtintenance xami-nalion.'I 'hcycan bc c[f'ectiyely scd n the examinationof nonPc'rous,rctal l icmaterials, oth fenous and non-lerrous. lnd of nonmctallicnaterials such as glazedol l t l ly ( lcnsil ied ciamics, crtlirr nonporous lastics,xno 3russ.

1.2' l 'his

lcst rclhod tlso providcs rcfercnce:

1.2.1 t ly which a l iquid pencrrantcxanrinationproccss ccon'lrcn(lcd r requifedby individualorgani-zirtionsclr br: r'cvicwcd o iLsccnitiltts lpplicabil i tyilnd corDI)lctcrcss,

1.2.2 .br use n rheprepxration f process pecif i-clt ions dcaliDgwith the liLluidpcnetrantexamination

of niaierirls rnd parts. Agreenent by thc user andthc supplierregnrdingspecific echniquess stronglyreconrntcncled.

1.2-3Frx usc in lhe orglnizationof the facil i t iesi lndpcrsonncl onccrncd ith the iquid peneirant xam-inaton .

1.3 f l l is lcsl Dlctho(ldocs not irxl icrtc or suggcstc{itcriit lor cvaltration l thc inclicatio|ls btrined. tshould be point(.dout, howevcr, hlt after indicationshavebeenproducecl,hey nlustbe iDterpretedr classi-fied lrnd then cvrluated,For this purposc here mustbc.a scpilrirtecodc or specilicationor a specif icasrccnrento define he ype, ize, ociltion, nddirectionof indiciltions onsidered cccptablc,nd thoseconsid-crcd unucccptable-

1.4 The values stated n inch-pound units are to bercgarded as the standard-'Sl uniis are provided for

information only.

1.5 This standard does not purport to address all

of the safety concems, f any, associdled v'ith its use.It is the responsibilitf of the user of this standard loestablish tppropriate safety and health pructices ttnddeternite the applicability of regulatory litnitationsprior to use. For specilic hazardstatements, ee Nores5, 12, and 20 .

2. IleferencedDocuments

2.1 ASTM Standards:D 129 Test Method for Sulfur in Pctroleum Producrs

(CeneralBomb Method)

D 516 TestMethod or Sulfate on in WaterD 808 Test Method for Chlorine n New and Used Petro-

leum Products Bomb Mcthod)

D I193 Specification or ReagentWaterD 1552 Test Method for Sulfur in PetroleumProducts

(High-TemperatureMethod)D 432'1Test Method for Anions in Warer n Chemically

Suppressedon Chromatography

E 433 RuferencePhotographsor Liquid Penetranrn-spection

E 543 Practice for Evaluating Agencies that perfo lNondestructiveTesting

E 1208 Test Method for FluorescentLiquid PenetrantExaminationUsing the Lipophilic Post-EmulsificationProcess

E 1209 Test Method for FluorescentLiquid PenetrantExaminationUsing the Water-Washable rocess

E 1210 Test Method for FluorescentLiquid PenetrantExaminationUsing the Hydrophilic Post-Emulsinca-tion Process

oooaoaaoaaoa

oaooao

oaooao

aaaoao

ooO

oa

LIQUID PENETRANTEXAMINATION

(ilt,

464



E l2l9 Test Method for FluorcscentLiquid penetrantExaminationUsing theSolvent-Removablerocess

E 1220TestMethod for Visible P.e4etanf,Exami4ationUsing heSolvent-Removablerocess, .,

E 1316Terminolo.gyof NQndpstru.pdve;ExaminationsE 1418TestMerhod or VisiblePenbtrant xamination

Using the Water-Washable ocess

2.2 ASNTDocutneu:R""ommenoeopral,i"" Svi-fb-f e fo, irlondestructive

TestingPersonnelQualncatiotrandCertification

2.3 Military Standard:MIL.STD-410Nondestructiveesting ersonneleuali-

ficationandCertification

2.4 APHA Standard:429 Method or the Examination f Waterand Waste-

water

3. Terminologr

3.I1fhe definitionselatingo liquidpenetrantxami-narioni which appear n TerminologyE i316, shauappty...tbhe termsused n this standani.

4. Summary of Test Method4.1 A liquid penetrant hich may be a visibleor a

lluorescentmaterials appliedevenlyover the surfacebeingexamined ndallowedo enteropendiscontinu-ities. After a suitable dwell time, the excess surfacepenetmnts removed.A developers applied o drawthe entrapped penetrantout of the discontinuity andstain the developer.The iest surface s then examinedto determine he prcsenced abserceof indications.

NOTE l: - Thc developcr Dry bc omittcd by rgre€rnentbet*eeopurchaserand supplier.

NOTE 2:Cauaion

-FluoEsccnt pcnclrant

qxaoinalionshall notfollow a visible penerrant xaminationuds*s thc Focdurc bss been

qunlificd in accordrncewith.l0:, becauscvi3ibL dvcs mav causedeteriorationor quenchingof Auorcsc€ltdyar.

4.2 Processing afameters, uchas surfaceprcclean-ing. penehation ime and excesspenetrant emovalmethods,arc determinetiby the specificmaterialsused,the natureof the part under examination that is, size,shape, urface ondition, lloy| and ypeof discontinu-rties expected.

Significance nd Use

sE-r6s

TABLECLASSIFICATTONF PENETRANT XAMINATIONTYPES NDMETHODS

Type - Fliorescentenetrantxaninatiot

MethodA - Water-washableseeTe5tMethodE 1209)MethodB - Post-emulsifiable,ipophiticseeTestMethodE

r208)

l\4ethod - Solvent emovableseeTestMethodE tZ19)MethodD - Post+mulJifiable,ydrophilicseeTest Method

E t21.0)

MethodA - Water-washableseeTestMethodE t4l8)MethodC - Solvent emovableseeTest ethodE

1220)

Each of the various metbods has been designedforspecific uses such as critical service tems, volume ofparts, portability or localizedareasof examinarion.Themethodselectedwill dependaccordinglyon the serviccrequirements.

6. Classification of Pcnetrntions and Mcthods

6.1 Liquid penetrantexaminttion mcthodsand typesare classified as shown in Tablc I

6.2 Fluoresccntpcnetrunl (xaninariolr utilizes pcne-trants that fluorescebrilliantly when excited by btacklight (see 8.9,1.2). The sensitivity of fluorescentpene-trants dependson their ability to be retainei ir thevarious size discontinuitiesdurirg processing, hen tobleedout into the developer oating andproduce ndica-tions that will fluoresce. Fluorescent ndications arcmany times brighter than their surroundings whenviewed under black light i lluminarion.

6.3 Visible penetrantexaninalion uses a penetrantthat can be seen in visible light. The penetrant is

usually red, so that the indicationsproduce a definiteconhast with the white backgroundof the developer.The visible penetrantprocessdoes irot require the useof black light. However, visible penerant indicationsmustbe viewedunderadequate hite ight(see8.9.2.1).

7. Types of Materials

7.\ Liquitl penetrantexaninatiottnrateriob(secNotcs3,4, and5) consist f fluor escenl.nd visibleDenetrants.emulsificrs oil-brse anrl watcr-base; ast and stow

acting), solvent removersand developers.A family ofliquid penetrant xaminationmaterials onsists f theapplicablc pcnetrantand cmulsifer clr rcDro ,er'as rec-

5.1 Liquid penetrant xaminationmethods ndicatethe presence,ocati6riand, to a limit€d extent. thenatureand magnitude f the detected iscontinuities.



s|l-t6s

oa(D

2OOISECTIONV

:ii'i:11"1":1"ii"J::1",i::i:::lfff :;,"$#:::i,?lf_],,-,,X,il#.i;r

for rcciarequ,rcmenrsor urrur.aroscn

d"l{;:ril:r*il1hry"*il,#,',#f,ff;r,:i,::j,'r;;;,;",:,il{#t;""fl""'"'}#:fffi:l"frlHT',];flilx

7.2 penetaus:

,",,1;1ili:i,u,; :{'li:,,:::,,,"^aredesisned.to

itfi l';:1"",;?*#[flTf"..",i#i?il-,1

JiffIl;f;, l ;".ilt"l#Jtil:i :l '#ffT ,: 9"""*",.._*,,"ni1,JT#:H,..,i1T;;:,,','T,:"1,,':,l l:":il:'r:.;":.,";q h ,u,ra".,e"r

,T,,"i1,.::,::1,1,r.,il*"ffi:,'ll,TffilJ:"T,l'",,;i ;J:,"",:I[,ffarion

does oroccur,esutringn

,,,ii ,q,ffi;1,:,i;:l;:,1;;..:tffi.::ll-,.]i'i":.illillryfffi';;:werr

irnc.'.;;,;.

I ;,;ll;:ll,,J"li:x*1,,ti*:i :*i:iTil:li,:g,llL:l::,*;,,lti"_*.";;:;lli$:::fii:::j;T:v i rsncLrr r r t ) l d iscont inu i l i c li l l l x

l:'xl;:l,j.*:;ffiil:J; iJi";l"L',l,ll?

run$*ffiffi

*n#*#*;*,r:*;llij:;l,y;,:x1,":"t'ff:l[{j*'$*fl#if",*r,""""*,*":i?"::#:,7.3E,tut.tiliert; ,,,oJ;,1.i"1,Jr"T.".:J#,

f^;:,;::i:.rs,supprieds

,'",'.ii'" r;iliLIi:ft;::::::xib,iquidsli"#-jfi.,fi1i :x**'r'r:}"ffi:ll,,ll':",,'"1*r;;';""i'J,.Ti:lill::llijLl'J';; i;'J:lgr*"n

r'i.r,"-"*iirr,"li",""nr*.0,",'rr rusron rtrrblishcslhe entulsificrc rtrcr , 'rr.., '

"..,.*i i"-., 'u"o"l irL'rt ion

lime Theyar cng on rhcirviscosity ,i",'ni,i iX;rt"--*is

rypcrd€vetoncrs nrendcdorappr,calion

:j,[;*l:?i,""Hr;:1ru,.:1j,":1,i"*,]f"."

d*ftil{i,,qfif""'",fn.ffiff"flt',*:";t**#*#*t,T:lI

i;;a;;#n1p*,i:m,,n:I,;*:l ,"1,*;,:;T,1il,:; I

ffi r#*$JJf*ff,:"ff*"."*,":

-*lit*t[*:'**T*tln#".I';:tr,r#*Ji,-.r

:I i"J:Tl"j;:l',",I"",r.,"":,il"1,ff1:;il.;li:jf .

t

aI

I

oooao



-:,r^1 i I

ASTSE ?a L]auIDIEYIIIff STANDARDS sE-16s

7.5.4 Liquid Film.Diveloperc are solutionsor 8.4 Removal f SurfaceContaminants:

colloidal suspensions f resins/polymer n a suitablecarrier. These developerswill-form'a-lranSparent .or-. , --*-.&4.1 Freckaning - ."the success f anypenelrant

translucentcoating on the surface of the part. Certain examinationprocedurc s gre.ay dependertupon the. types of film developer nay-be stripped rom the p-art -. surroundingsurfaceanddiscontinuitybeing free cf aay

and retained for recordpurposes see 8,8.5).

8. -. ',Procedure .-.-

LtlThe followinggenerat rocessing uirtelinesapply

lseefigs. 2,3, and4) to bolh fluorescent nd visiblepenetmnl xaminationmethodsseeFig. l).

8.2 TemperalureLimits - The teriperature ol the

penetant materialsand the surfaceof the part to beprocessed houldbe between 0 and 100'F (10 and

38'C). Where t is not practical o complywith thesetemperature imitations, qualify the procedurc as de-scribedn 10.2at lhe temperaturef intended se andas agreetlto by the contractingpanies.

8.3SurfaceConlitioning Pior to PenetrantExamina-rlo,, - Satisfactoryesuls usually may be obtained

on surfacesn the as-welded, s-rolled, s-cast, r as-forged conditions or for ceramics n ihe densifiedconditions). ensitiveenetrantsregenerallyesseasilyrinsedaway and are thereforeesssuitable or rough

surl'aces. henonly oose urface esiduals represent,thesemay be removedby wiping with clean lint-free clo(hs.However, recleaningf metals o removeprocessingesidualsuchasoil, graphire, cale,nsulat-ing materials, oatings, nd so forth, shouldbe doneusing cleaning olvents, apordegreasingr chemicalremovingproccsses.urface onditioning y grinding,nachining,polishing r etching halt ollow shot,sand,grit or vaporblasting o rcmoye he peened kin andwhen penetrantentrapment n surface rregularitiesmightmask he ndications f unacc€ptableiscontinu-iries or otherwise nterfercwith the effectivenesi f

the examination. or metals, nless therwise pecified,etchingshall be performedwhen evidence xists hatprevious leaning, urface eatmentsor serviceusagehaveproduceda surface ondition hat degradesheeffectiveness f penetrant xamination. See AnnexAl.1.1.8 or precerrtions.)

NOTE 8 - wlen agncd betlregn purchasef atd supplier, grit

blasringwirhoutsubscqucnttchingmay bc sn acccptablel€3nin8

NOTE 9: Coution - Sandor sbot blastingmay porsiblyclosediscontinuiliesnd extreme areshouldbe lsed with Erindingandmachining operarions o avoid rnaskirg disconlinuili.s.

NOTE 10- Forstrucluralot elefionic ccraflrcs, sudaceprcparatiodby giinding, sand blasting and crclitrg for pcnetrantcxamination snot recommendedecause f thc polential or damage.

..'contamilant (solid or liqu0 that might interferewith

the penetrant .process.All parts or areas of pafis to be

exaflined. must be clean and dry Aeforc the penetrant. is applied. If only a sectionof a part, such as a weld,

including the heat affected zone is to be examined, all

. conhminants shall be removed from the area being

examinedas definedby the contractingparties. Clean"

is intended to mean lhat the surfacemust be free of

rust, scale, welding flux, weld spatter,grease,paint,

'oily films, dift, and so forth, that might iDterferewith

the penetrant process.All of these contaminantscan

prcvent the penetrant rom entering discontinuities see

Anne,( or Cleaning of Parts and Materials).

NOTE l: Caulion Residuesromclcaningroccsscsuch sskong alkalics, picklin8 solulions aod chromaies, n padicrlat, mny

adversely t.act tvith the penetrant and reduce its sensitivity and

p€rfonnancc.

8.4.2 Dryiry after Cleaning- It is essential hat

the surface of parts be tboroughly dry after cleaning,

since any liquid residue will hinder the entance of

the penetmnt.Drying may be accomplished y warming

the parts in drying ovens, with infrarcd lamps, forced

hot air, or exposure o ambient emperatur e.

8.5 PenetrantApplication - After the part has been

cleaned,dried, and is within the speciiied emperature

range, the penetrant is applied to the surface to be

examined so that the entirepart or areaunder examina-

tion is conpletely covered with peoctrant.

8.5.1 Modes of Applicstion - There are various

modes of effective application of penetrant such asdipping, brushing, flooding, or spraying. Small parts

are quite often placed in suitable basketsard dipped

into a tank of penetrant.On larger parts, and those

with complex geonetrics, penetrant an be applied

effectively by brushing or spraying. Both conventional

and electrostatic spray guns are effective means of

applying liquid penetrantso the part surfaces.Electro-

static spray application can eliminatc cxcess Iiquid

build-up of penetraoton the part, nrinimi:e overspray,

and minimize the amount of penetrilntentcringhollow-

cored passageswhich might serve as penetrant eser-

voirs, causingseverebleedoutproblemsduringexamina-

tion. Aerosol sprays are conveniently porlable and

suitable or loca l aDDlication.

46 7



sr,r-165

oaooot

I

I

I

oI

a

oooooo

Iaoaoa

aeI

oI

o

toooo

?00tsEcTloN

[tlcoMlNc PAnls

PsElLElta

(See 8.4)

P€IITTRA' E

(See 8.5)

R E M O V I

(See .6 )

0 E v E t o P

(See 8.8)

I H S P E C T

(SeeB.9l

P 5 T C t N(See8.10an d

A1 2 "

i:fi";:; -

FIG. FLUORESCENTNDVISIELE ENETRANTNSPECTIONENERALROCESSINGROCEDURESFLOWSHEET

NOIL l2 Caurion - Not al l prnerr,rnr l i , rcf lxt \arc suirable or(rc.-1r.rr . .T .r ' nf tr t rc. l on\. so rcsts houtJ he conctucrcd r ior

\OTlr t .1: \ , , r r) i [ - Wirh spr. iy pl l ic .( ion(. i r is rml lonanr hl rrcDl, l , ,Lo. This is S.nc|: | y . ,cronrpt is lcd hrcu h

r, .1c.t I d \r inL,J \ tr , : r ) hr\1r 'r rndcr i t r . ,u$rystern-

1J.5.2)tttt'truat Dwall T nc _ Aftcr applicatiotl,:r l lou cxcr] l ispcnclrant o drain ll.otrr he pAn (C fe

should be laken to preventpools of penebrnt fromtonnrng.onhcpart),whilc rllowing for proper enetranrowe/r t lme (see TabJe2). The teng(h of t ime th epenctrrnt must rernainon the pan to allow prooerpenelration lrould c rs ecomntcnrledy thc pcnetranrmanufacturer.Table 2, howevel provides a iuide forselection of pcletri|nt dwell times for a varietv ofmaterials.brms, :lnd types of discontinuiry.Unlcsr

''g'

'i$;.r.#t;

(See8.7) (See .7)

OUTGOINGAATS

458



. --::__i: ::.:3s:sai: ij; i "r3i:ri$iiil*:.i.i.:::iil:fiinfrr:l;:::iil:':' _ l

ARTICLE 24 - UQUID PENETRANTSTANDARDS

Psrnubp6r

o.y

Sp.rt

sE-165

PBECLE4TI(s6€ ...1)

DFY(5€€ .1.2,

PA{ETnA|.T

{s4oe.5)

FIIJALRINSE(s€€ -6.11

OEVEIOP(S€€ E.8)

oEvgtoP{s€€ .8}

D8Y(Se€8.7,

ORY

{sd 8.7)

EXAA{IN€Fluores.€nt{$. 8.9..t1 4sjb]o 56€ 8.9.2)

gry

o.v

Ory

FIG'2 ' 'GENE*oL ROCEDURELOWSHEETOR ENETRANTXAMINATTONSINGHE WAIER-ASHABLER'cEssrdsr METH'DrzosFdR'iu';;$;i i ANDEsrMETH.D1220 .RvlsrBLELIGHT)

t . 1

' 4 iothcrwise specified, the dwell time shall not

exceedthe,maximum recommendedby the manufacturer.

)^911-lo , ,F:, -:".c spccifir ppticarionsn strucrurateramicsL'u, xampte.crccunganing'|'csn sID{asr .alcrial),he equirEdpeneFanlwel dmeshould cdetermin;dbc roDScrhan harsho*n o Taulc.laDJ

exp€rimentallyndntay

8.6 Penetrant Removal

8.6.7 Warer t$ashaite:

.,8.6.f.1 Removalo Excesspenetrants_ Afrer

rnc required oenetrationtime, the excesspenetranton(nc,surlace being exarnhed must be removed with

water"iusually a washingtbperation.It can be washed

off manually, y theuseof ilutornatucr sentr_automati cwater-spmyequipmentor by immersion,For immersion

:lnslng,_pansare completely mmcrsed n thc wxrcr

oatnwttn arr or mcchrnicrl sit i t ion. Accuntulr(ionofYater rn pockeh or rcccsscs f th; surflrccnrust bcavoided,

. l fthc finul rilsc stcp is not cflectivc, us

evrdenced y e\cessive esiLlualurface cnelrrni ftcrrinsing, dry (see8.7) and reclean hc part, rhenreapplythe penetrant for rhc prescribccldwell tine.

(a) The temperilture f the rvatershould be rclativc)yconstantand should be maintilinedwithin the range o-f50 to 100'F (10 ro 38"C).

-,

{a),lnra1-y-s3 walerpressurc houldnor bc grentcrrhan40 psi (280 kpa).

469



sri-t65

?

I

I

I

aot

t

a

I

I

I

aI(}

oaa

aat

aot

ooI

a

t

'€r i-a

2001SECTIONV

8.t .2

Scr: 8.5E.5.1

8.5.2

Sc(: 8.6.28.6_2.186.2.2

5c 8.6.?.3€.6.2.'l0.6.?.5

1.. 8.8.30.0.18.8.t

6 . 7 . 2

8.2 Vit ib lcJ

S . . . 8 . 9 - 1

0.9. t . t0_9.r.28.9.1.38.9.1,21

S c . : 8 1 0

FIG. TYPE _ POST I\ lULSIFIABLEROCEDURES-2 FLUORESCENT)ANDB-2 VISIBLE)

Stlecial R.qui..nEatt

Ptoc.dt,. Requirc.u4|l

the surfacewith a clcan, absorbentmaterial dampenedrvith.w.rteruntil theexcess urflce penetrant s renovcd,as dcterminedby examinatien nder black light fo rfluorescertmethodsand white light for visible mithods.

8.6.2 Lipophitic Enulsificarion:

8.6.2.1 Application of Enulsifter _ Aller thcrequired penetration ime, the excess penetrant oD lhepart rnust be emulsified by immersing or flooding

9. 1

9. 2

l 0 . i't0.2

S..: €.9-2€,9.2-r

fc) Rinse inreshouldnocexcced120s unless ther_wise spcci,iedby palt of materialspecification.

)-9.1u-]:..9"11,":'_ Avoidoverwashis. Ercessiveashingan

causepcnclranL o hc washedout of disconiinujties.with fluorelenfncn.trrnl Fc'hods pennnn rbe r insine op€mtior) nder btack iqhrso InrI rr cnir hc drtermincdwhen tbe sud:rcepcndmnr has bcen.dequntcly cmoved.

.1J.6.1.2 enoval by Wipiug_In speciatapplica_

trons,pcnetrant entovalmay be performedby wiping t

tootI

470



,ARTICLE 24 - LIQUID PENETRANTSTANDARDS

Incornlng .rl.

PNECLEAI'I

(ss€6.1.1)

oaY

tS€€8.4.2)

PENETAAr{'APPLICATIOII(S0.8.5)

NE OVE €ICESs

PENETR NT(S€68.0.4)

DB Y

{s6€ 8.7)

OEVELOP(S€o8.8)

oaY(s8e8.7)

EXAMINE

Mod€nlcal

Dry

PEht Strlpp€.

D(f

oeiwgent

^pglySolv€n(-

Flroa€sclnl

Solv€ntWIp€4ll

No.l3quoout

Wol or LJquldFlln O€v€fo €r

Dry

lt€l€r €r|l

ory

the partswith the requiredemulsifier the emulsifiercombineswith the excess utfacepenetrant ndmakesthc mixture-removableith wter rinsing).After appli-cation of the emulsifier, he pars are drained n amanner hat preventshe em sifier from poolingonthe part(s).

8.6,2.2 EmulsifcationDwell Timebeginsas soonas heemulsifier asbeen pplied. he ength f time hat

theemulsifiers allowedo remain n apartand n contactwith thepenetrants dependentn the ypeof emulsifieremployed nd he surface ondition smooth r rough).

Nominal emulsification ime shouldbe as recommendedby themanufaciurcr.The acrualenrulsificationime mustbe determincdexpcrimentally or eachspecili tpplica-tion. The surface inish roughness) fthe pan is a signifi-cant actor n theselection fand in theetnulsificationimeof an emulsifier.Conract ime sbould be kept to the least'possible ime consistentwith an rcceptablebackgroundandshould otexceedhemaximum imespccifiedor hepartor material.

8.6.23 Post Rursirrg Effectivc post rinsingof the emulsified penetrant rom the sulflsg 6xr 6.

nuor6sc0nt(f'6o 8.9.1)Vlslble S€o6.9.2)

POSTCLEAI{(5€6 8.10 andAnn6xon PoslCloartng)

Vapor O€g.e.36 Solv€ntSoax Ulrasonk Cl€3n

Oulqoint P.tL

FIG.4 SOLVENT.REMOVABLEENETRANTXAMINATIONENERAL.ROCEDURELOWSHEET(TEST

METHOD I2I9 FORFLUORESCENTNDTESTMETHOD I22OFORVISIBLE IGHT)

sE-165

41 1



sE-165 2001 EcTIoN v

TABLERECOMMENDEDINIMUMDWELLTIMES

Material FormType f

Discontinuity

DwellTimes/minutes)

Penetrantt Developef'

Aluminum, ragne5ium/teel, ra5s

andbronze,itaoium ndhigh-temperaturel loys

Carb;de-tippedoolsPlast ic

G lass

Ceramic

castings ndwelds

wroughtmaterials extrusion ,lorgingt plaie

all forms

all formsall forms

coldshuts, orositt lackof fusion,cracks all formg)

lapt cratks all forns)

lackof fusion, orositt crackscfacks

crack3

cracks/ orosity

ooaaao

oooooa

oaI

aoa

oaooao

oaoaO

o

oIo

aa

1 0

10

5

l 0

1 0

10

1010

^ For temperatureange rom 50 to 100'F (10 to 38.C) for fluorcscentenetrantsnd50 to L25.F (10 to 52"C) for visiblepenetrant.: \ .4arimun cnerrrnl well ime n accordanceith0.5.2-t Developmentime begins s soonas wet developeroatinghasdried on surface f part5 recommendedmlnlmum).Maxlnum oevetopmentt.rre n ac<ordance;rh8.8,6.

accomplishcd using either manual, semi-automated, rautomatedwater immersion or spray equipmentorconrbinations hereof-

8.6.2.4 nucrsiou - For nrmcrsion ost insing,prrts are cotnpletely inmersed in the water bath witharr or n)cchanic gitation.Thc tinle and tempcratureshould bc kept constant.

fd) The nlaxintunl dip-rinse imc shouldnot exceed120 s unlessorllerwisespecil iedby pan or material

specification.(b) The tempertture of Lhcwrrcr should be relativelycoJrstant nd shouldbe maindinedwithin the rangeof50 to 100"F (1Cr o 38'C). Cndion: A touch-up insexr3), bc nccessary iier imntcrsiotr.

8.6.2.5,Sirro-rPo.il /tir-rirg - Effective postrinsing folio\ring emulsificatiolr an also be accom-plished by eithcr manual or aLtouatic water sprayrinsing of l l tc I)1trtss tbllervs:

fl) Control rinsc wirtcr cllpcriL{urcvithin lrc rangcof 50 to 100"1.10 to 38"C) .

(b) Spray rin-sewater pressur.chouldbe in accord_

ilrce \\,ith llanufaclurcIs' rccotnmcldations.(cJ Tlic rnnxintuiD pray insc irDc houldnot cxcccrl

120 s unlcssolherlvisespecil icdby part or mate.ialsspecificaiion.

8.6.1.6nnrre Elft'ttiwncss If rhc emulsif ica-tion and final rinsc step is not effcctive, as evidencedby excessivc csiduai urface enetnntaftcr cmulsifica-lion and rinsing, dry (scc 8.7) and reclean he part andrcapply the peflerrllrlr or tha prescribcddwell time.

8.63 Hydrop hil ic Emul s f cation

8.6.3.1Prerinsing- Directly after the requiredpenetration ime, it is recommended hat the parts beprerinsedwith water prior to emulsification (8.6.3-3).This step allows for the removal of excess surfacepcnetrant rom the pads prior to emulsilication so asto minimize the degreeof penetrantcontaminatiol inthe hydrophilic emulsifier bath, thereby extending itslife. In addition,prerinsingof penetrated afls minimizes

fossible oily penetrantpollurion in the final rinse stcpof this prccess.This is accomplishedby collecting thcprerinsings n a holding tank, separating he penetrantfrom water.

8.6.3.2PrerinsingControls- Effectiveprerins-ing is accomplishedby either maoual or automaaedwaler sprav rinsing of the pans as follows:

(aJ Water should be free of contaminants hat couldclog spray nozzles or leave a residue on parts,

(b] Colltrol wttcr tcnrpcnrturc ithin tl)e rxoge ol '50 to I00"F (10 to 38"C).

(c) Spray rinse at a water pressureof 25 to 40 psi(175

to 275 kPa).(d) Prcrinsc ime should be tlre lcast Dossiblc irnc( onrinill , 60 s rnaximunr) o providc a consislcntresidueof penetranton parts. lvash time is to be asspccifiedby the part or matedal specification.

(e.)Removewater trapped n cavities using liltcrcdshop air ar a nominal prelsure 25 psi (175 kpa) or asuction deyice to remeve water from pooled areas.

8,6.3.3Application of Enulsifier * After thcrequired pcnetration time and following the prerinsc,

47 2



:--.:i::-:ii: l

the residualsurfacepeneh t on pan(s)must be emulsi-fied by immersing he paft(s)n ahydrophilic mulsifier

bath (8.6.3.4)or by spralng theipar(s) ?with theemulsifier(8.6.3.5) hereby rcndering he iemainingresidual surface penetrantwater-washablen the finalrinsestation 8.6.3.6).

8.63.4 mmersion For immersion pplication,parts are complQtely-mmersed n the emulsifier5ath.The hydrophilicemulsifiershouldbe gently agitatedthrcughout he contact ycle.

la) Batb conc€ntrationshould be as recommendedby the manufacftrer.Most hydrophilicemulsifiers reused within the rangeof 2n to 33% in water.Nominal

use concentration or imrnersionapplications s 207o.(D) Bath temperatures hould be rnaintainedbetween

50 and 100'F (10 to 38'C).(c) Immersioncontact ime shouldbe kept to the

minimum imeconsistent ilh an acceptableackgroundand should not exceed120 s or the maximum imestipulated y the part or material peaificatiol.

(d) Emulsifier drain time begins mmediately fterparts have been withdrawn from the emulsifier tankand continuesuntil the parts are wsshed n the finaldnse station 8.6.3.6).This drain ime shouldbe keptto a minimum o avoid over emulsification ndshould

noLexceed 0 s,

8.6,3.5SprayApplication For sprayapplica-tion foltowing the prerinse step,psrts are emulsifiedby the spray applicationof an emulsifier.All partsurfaces hould be evenlyand uniformly sprayed oeffectively emulsifo the residualpenetant on part sur-faces to render it water-washable,

(4J The concentrationof the emulsifier for sprayapplication houldbe in accordanceith the manufac-turer's recommendations,ut shouldnot exceeA %.

/r) Temperaturc to be maintained at 50 to 100"F

(10 to 38'C).(c) The spray pressureshouldbe 25 psi (175 kPa)

max for air and 40 psi (280 lPa) max for water.

(d) Contact time should be kept to the rninimumconsistent with an acceptablebackgroundand shouldDot exceed-120 s or the malimum time stipulatedbyrhe part or ma@rial pecification.

8.63.6 Posr-Riruing of Hydrophilic EmulsifiedParrs - Effective post-rinsingof emulsifiedpenetrantfrom the surface can ba accomplishedsing eithermanual,semi-aubmdted,or automatedwater mmersion

or sprayequipment r combinationshercof.

sE-I65

E,6.3.7mmersiott ost.Rinsing Pansare tobe completelymmersedn the waterbathwith air or

mechanicalagitation..(a) The emperaturef thewatershould e relatively

constan ndshouldbe maintained ithin the rangeof50 to 100'F 10 to 38'C).

(b) The maximum ip rinse imeshouldnot exceed120 s unlessorherwise pecified y part or materialspecification.autiontA touch-upinsemaybe neces-sary after mmersion.

8.6.3.8 prayPost-Rlzsirg Following mulsi-0cation anscanbepost-rinsedy waterspray insingas follows:

(a) Control insewater empcrature ithin thc rungc

of 50 to 100'F 10 to 38'C).(6) Spray insewaterprcssure houldbe in accord-

ancewith manufacturer'snstructions,(c) Themaximum pray inse ime should otexceed

120 s unless therwise pecifled y part or mate als

specification.

8.6.3.9f tle emulsificationnd inal rinsestepsare not effecdye,as evidenced y exccssive esidualsurface enetrant fteremulsification nd rinsing, dry(see8.7)and ccleanhe panand eapplyhe penetrantfor the presdibeddwell time.

8.6.4SolventRernovableenetran s

8.6.4,1Removal f Excess enetratt Aftcrthe requiredpenetrationime, the excess enetrantsremovednsofaraspossible, y usingwipersof a dry,clean, int-free material and repeating lre opemtionuntil most races f penetrantavebeen emoved. henusinga lint-freematerialightly moistened ith solventremoverhe emainingraces regentlywiped o avoidremovirgpenetrantromdiscontinuities.void the useof excess olvent. f the wipingstep s not effectivc,as evidenced y dimculty in removing the excesspenetrant,ry (hepa( (see8-7),and reapply he pene-

tralt for theprescribed wel[ ime. Flusbing the surfacewith solvent ollowing he application f the penetrantandprior to developings prohibited.

E 7 Drying - Drying the surfaceof the part(s) snecessaryrior to applyingdry or nonaqueousevel-opers r following he-applicationf the aqueous evel-oper.Drying time will vary with the size,nature, ndnumberof pans under€xaminalion.

8J.l Drying Modes- Pans can be dried byusing a hot-air recirculating ven, a hot or cold airblast,or by exposureo ambient emperflaure,rfticu-

larly when he excess urface enetrantwas removed

ARTICLE24 _ LIQUID PENETRANTTANDARDS

471



oo

sIt-165 2001 Ec oN v at

ooaoaooa

oooooI

oeoooa

oooaaa

oot

with a solvenr.Drying s bestdone n a thermostaticallycontrolled ecirculating ot-airdryer. ncal heating fcooling is pernritted rovided he temperaturef tha

'partrcmainsn the range f 50 to 100'F 10 o 38"C)

for lluorescentmethodsand in the range of 50 to

125"F 10 to 52"C) or visiblemethodsnless therwiseagreedby the contracting arties.

NOTE 16:Cautlon- Dryingovcn emperalur€hould ot exceedt 60"F ? "c).

8.7.2 Drying Time I-imits - Do not allow parts

to rcmain in the drying oven any longer than is necessary

to dry the surface. Times over 30 min in the dryer

may impair the sensitivity of the examination.

8.8 DeveLoperApplication:

8.8.1 Modcs of Applicarion * There are various

flrodcs of effectlve appiication of the various types ofdevelopers such as dusting, immersing, flooding orspraying. The sizc, configuration, surface condition,nunrber of parts to be processed,and so fonh, willinfluence he choiceof developer pplication.

8,8.2 Dry Powder Developer Dry powderdevel-

opers should be applied inrmediately after drying in

such a nranner as to ensure complete part coverage.

Parts can be inrmcrsed n a containcrof dry developer

or in a fiuid bcd of dry developer. They can also be

dusted widr rhe powder devcloper ihrough a handpowdcr bulb or a conventionalor elecbostaticpowder

gun, It is conrnron and cffcctiveto apply dry

powder

in an encloseddusl chamber.which createsan effcctive

and controlleddust cloud. Other meanssuited o thesize and gcornctry of thc spccinrcnmay bc used,providcd the polr'dcr s dustcdcvcnly ovcr ths enttteiur(ace being eraurincd.Excesspowdermay bc removcdby shakinr or tapping the part, or by blowing withlow-pressure(5 to l0 psi) (34 to 70 kPa) dry, clean,coruprcssed ir .

NO1li : l7: ( lo l io,r -- I - l rc i r $rrc:r lnorcn\ i ry houkl hi : csruht ishcdcxpcr inrrD(t l ly lr elch apt l icar ior)-

8.li,3 /rTrrcors Det'elcpers Aqueous developers

should bc lppliccl to the pirt inrnrcdiately fter th cexccsspenetrlnt has been relnoved and prior to drying.Aqueous developelsshould be preparedand maintainedil accordance itll the ntanufacturer'snstructions ndapplied n such a nlanrcras to ensure omplete, ven,p3fl covcragc.C:rution houldbe excrcised henusing n aqueous developer with \rater-washablepcnetrantsto avoid possiblc stripping of indications.Aqueousdevelopcrs ay bc appliedby spraying seeNote I?),florving, r ir)lltrcrsinghc parl- t is common o mmersc

the pans in a prepareddeveloperbath. Immersepartsonly long emugh to coat all of the part surfaceswiththe developer se€Note 18). Then remove parts fromlhe developerbath and allow to drain. Drain all excessdeveloper rom recesses nd trappedsections o elimi-

nate ooling f developer, hichcanobscure iscontinu-iues.Dry the pads in accordancewith 8.7. The drieddevelopercoating appearsas a translucent or whitecoatingon lhe part,

NOTE l8r Cttlion - Atomiz6d spraying 9 aor recommended incea spooyfilm may result

NOIE 19: Cg| ion'- If parts arc lcft in thc bath too lon8,indicationemry lcach out.

834 NonaqueousWet Developers After theexcess enetranthas been emovedand the surfacehasbeen dried, apply developer by spraying in such a

manneras to ensure complete part coverage with athin,even ilm of developer. hese )rpes f developercarrierevaporate ery rapidly at norma.lmom tempera-tureanddo not,therefore, equire heuseof a dryer (s€eNote 20). Dippingor floodingpafis with-nonaqueousdeveloperssprohibited,inceheymay lushor dissolvethe penetrantrom within the discontinuities ecauseof the solventactionof these ypesof developers.

NOTE 20: Warning - Tfie vapors f(om $e evaporaling, volatilesolventdcvcloper carricr may be hazardous.Roper venlilarion shouldbe prcvided in all cases. but especially when rhe surface (o beelamined is insidc a closed volume. such 9s a process drum or asmall sto|age taok.

83.5 Liquid Film Developers App)yby spraying

as recommendcdby the manufacturcr.Spray parts in

such a manner as to ensurccomplete part covcrage ofthe area being examined with a thin, evcn film ofdeveloper.

8,8.6 Developing Time - The length of time thedeveloper s to rernainon the part prior to cxaminationslrould bc not less lan l0 rlin. Dcveloping tinrcbegins mmediately after the applicationof dry powderdeveloperandas soon as he wet (aqueous nd nonaque-

ous) developercoatirrg s dry (that is, the solvent carrierhas evaporated o dryness). The maximum perrnitrcd

developing imes are 2 h for aqueousdevelopers an,JI h for nonaqueousdevelopcrs.

8.9 Examination - Perform examination of partsafrcr the applicable developmenttime as specified in8.8.6 o allow for bleedoutof penetrantrom disconrinu-ities into the developercoating. It is good practice roobserve he bleedout while applying the developer asan aid in interpreting and evaluating indications,

oa



,: ] AITTICLE 4 _ UQIND PENETRANT TANDARDS

8.9.1 FluorescentLiShi Emmination:

8.9.1.1 Visible Artbient Light Level- Exffinefluorescentpenetraiit ndications under black light in adarkenedarca"Visible ambient ight should not exceed2 ft candles 20 Lx). The measurement hould be madewith a suitablephoographic-typeisibte ight meteron the surf€cebeingexamined..

'8.9.12Btack light Izvel Control - Black

lighr inrensity,minimumof 1000pWcmz, shouldbemeasured n thesurface eingexamine4with a suitableblack ight meter.The black ight wavelengthhallbe

in the ralge of 320 ro 380 nm. The intensity shouldbe checkedweekly to ensure he requircd output Re-flectors and filters shouldbe checkeddaily for cleanli-ness and integrity. Crackedor broken ultraviolet (lw)

frltersshouldbe replacedmmediately, efective ulbs,which radiate UV energy, must be replaced beforefurther use. Since a drop in line voltagecan causedecreasedlack ight outputwith consequentnconsist-

ent perfor.mance, constant-voltageransformershould

be usedwhen there s evidence f voltage luctuation.

Caution; Certain high-inlensity blact light may emil DnacceplabJermounts of visible light, which will cause luorcacent ndicationso

disappear. areshouldbe taken o usc only bulbscenifiei by lheJupplicr o b€ suitnbleor suchexaminationurposes.

NoTE 2l - The recoruncnded inimum ight intensityn 8.9,1,?is intended for general usag.- Foi critical eraminations, hiSherintensity evelsmay bc ftquircd,

8.9.1.3 Black Light Warm-Up Allow theblack ight to wann up for a minimumof 10 minpriorro its use or measurEmentf the intensityof theulrravioletight emitted.

E.9.1,4 Visual Adaptation - The examiner

should be in the darkened area for at least I minbeforeexamining arls. onger imesmay be neaessary

under somecircumstances.

NOTE 22: Crution - PhotochromicensEs hall not be worndudngc)iamination.

8.9.2 Visible Light Examiwtion:

8.9.2.1 VisibleLight lzvel - Visible peretrant

indications can be examined n either natural.oraftificial

light. Adequate illumination is required to ensure no

loss n the sensit ivity-f the examination. minimumlight intensity at the examination site of 100 fc (1000

Lx) is recommended.

ESj Howekeeping Keep he examination reafree of htefering debris, ncluding fluorescentobjects.Practicegood housekeeping t all times.

&9A Evaluation - Unless olherwise ageed, itis normalpractic€ o interpretand evaluate he disconti-nuity based n thesizeof the indiiation (seeRefercncedPhoaographs 433).

&10 Post Ckaning- Postcleanings necessarynthosecaseswhere csidualpenetant or developer outdinterferewith subsequentrocessing r with servicerequircments.t is particularlymponantwhere esidual

penehant xaminalion'materialsmight combinewithother actorsn serviceo produce onosion.A suitabletechnique, uch as a simple water rilse, wate$pray,machine ash, apordegreasing,olr€ntsoak,or ultra-soniccleaningmay be employedseeAnnexon Post

Cleaning).t is r€xommendedhat f developercmovalis necessary,t should be caricd out as proroptly aspossibleafter examination o that it does not "fix"

on the pan.

NOTE 3:Crution Devclopershoulde emoveddot ovapordegreasing.apor egrcssinganbakehEdevelopern pans.

' 9. Special Rcquirements

9.1 lmpuities:

9.1,1When using penetrantmaterialson austenitic

stainlesssteels, titani[m, nickel-base or other high-

tempeHturealloys, the need to restdct impurities such

as sulfur,halogens nd alkali metalsmustbe considered.

These mpurities may causeembrittlementor corrosion,

particularly at elevated emperatures. ny such evalua-

tion should also include consideration of the form in

which the mpurities arcpres€nt.Son)epen€trantmateri-

als contain significant amoun(s of these impurities in

the form of volatile organic solvents. These normallyeyaporatequickly and usually do not cause problems.

Other materials may contain impurities which are rlot

volatile and may react with the part, padcularly in

the prcsenceof moisture or elevated temperatures.

9.1.2 Becausevolatile solvents leave the surface

quickly without reaction under normal examination

procedures, enetmntmaterials are normally subjected

to an evaporation procedureto rcmove the sclvents

before the materialsare axalyzed for impuriti€s. Thc

residue rom this procedure s then cnalyzed in accord-

ance with Test Method D 129, Test Metbod D 1552,

or Test Method D 129 decomposition ollowed by TestMethod D 516, Method B (Turbidirnetric Method) for

sulfur. The rcsidue nray also be analyzed by Test



sE-16s 2001 EcTroN

ooaaoooaaooa

oooaaa

aaooao

aaooaa

aoo

MethodD 808or AnnexA2 on Methodsor MeasuringTotalChlorineContentn CombustibleiquidPenetrantMaterials for halogens ther han luorine) ndAnnexA3 on Method for Measuring otal RuorineContentin Combustible iquid Penetration atedals for fluo.rine).An altemative rocedure,

rnex A4 on Determi-nation of Anions by Ion Chromatography,rovidesa single instrumentalechnique or rapid sequentialmeasurementf commollanions uchas chloride,luo-ride, and sulfate.Alkali metals n the residuearedetermined y flamephotometry r atomicabsorptionspectrophotometry.

NOTE 24t - Somecuncni staodardsndicatc 6ri impurity levelsof sulfur and hrlogens xceeding % of any onc subpect lamcntmay be considcred xcessive. owevcr, his high a levelmay bclnacaeltable for somcapplications, o heactual naximum cccpioblejmpurirylevel mustbe decideibetw€en uppticr rd useroo a csseby casebasis.

9.?, Evaluated-TemperatureExdrni.ndtion

-Wherepenefant examination is performed on pans that must be

rnaintained at elevated emperatureduring examination,

special materials and processing echniquesmay berequired.Such examinationequircsqualificationnaccordance ith I 0.2.Manufacturer'secommendationsshouldbe observed.

10. Qualincationand Rcqualification

10.7 Persotnl Quulifcatiott When requiredbyuser/suppliergrcement,ll examinxtione.sonnclhall

bequalified/cenifiedn accord&cewiii a writtenproce-durc conforming o the applicable dition of recom-mendedPracticeSNT-TC-IAor MIL-STD-4I0.

10.2 ProcedureQualifuation- Qualifrcationofproceduressing times or conditionsdiffering fromthosespecifiedor for new materialsmay be performedby any of several methodsard should be agreedbythe contractingparties.A test piece containing one ormore discontinuitiesf the smallest elevantsize isused. The test piece may contain real or simulateddiscontinuities,roviding t displayshe characteristicsof the discontiluities ncounteredn productexami-nation.

103 l./ondestrucrive estingAgencyeualification -If a nondestructiveestingagencyas described nPractice 543 s used o perform heexamination,heagencyshall neet the

requircmentsofpractice

E 543.10.4Requalifcationmaybe requiredwhen a change

or substitutions made n the typeof penetant materialsor in the procedure ee 10.2).

11. Keywords

l1.l fluorescenriquidpenetrantesting;hydrophiticemulsification;ipophilicemulsification;iquidpenetranrtesting; ondestructiveesting; olvent emovable; isi-ble liquid penetrantesting;water-washableethods

ANNEXES(Mandatory nfornadon)

A1. Cleaning of Parts and Materials

,A'1,1Choicc of Cleaning Mcthod

A.1,1.1The choiceof a suitable leaningmethodis based on such factoni as: (1) type of contaminantlo bc rcmovcdsincenooncrr:cthodcmoycs ll contrmi-nants equally

weli;(2)

effcct of rhe cleaningmerhodod the pafts; (J) praclicality of rhe cleaning methodior the part (for example, a large pan cannot be putinto a small degreasel r ultrasonic leaner); nd (4 )spccil ic clcaning rcquirenrcnrs f rhe purchrser. hcfirllowing cleaningmethodsare recommended:

F.1.1.1.1Detergc t Clearl?lg Detergcnt lean-ers are nonflarumablewater-solublecompoundscon_taining specially selectedsurfactants or wetting, pene-traling, emulsifying, and saponifying various types of

soils, such asgreaseand oily films, cutting and machin-ing fluids, and unpigmenteddrawing compounds, etc.Detergentcleanelsmay be alkaline, neutral, or acidicin nature,but must be noncorrosive o the item beinqinspected.hecleaning ropenies f derergenr olurionifacilitate omplcte emovalof soils and contamination

from the surfaceand void areas, hus preparing themio absorb he peneirant.Cleaning time should averagel0 to 15 min at t70 to 200.F (77 to 93"C) withmoderateagitation, using concentrations (generally 6to 8 ozlgat or 45 to 60 kglm3) recommendedby thcmanufacturerof tbe cleaning compound.

Ll.l.l.2 SolventCleaning-There are a varietyoi solventclcanershat can be effectivclvuti l ized rodissolve uchsoilsas grease nd oily fitms, waxes ndsealants,paints,and in general,organic matter. Thesc

,-t.::it':.:i ::'.:l r

,.,i;:t::ir:.,':.rl ,:i-t .

oo

47 6



solvenrs should be residue.free,especially*t"n ur.a

as a hand-wipe solvent or as a dip.tank degreasingriolvent. Solvent cleanersare not recommeided for th;removal of rust and scale, welding,flux and spatter,and in gencral, norganic soils. Cautiou Somecleaninpsolvcnts are flammable and can be toxic. Observearnanufacturers' nstructions and precautionarynotes.

A1.1.1.3 Vapor Degreasing - Vapor degreasingis a prefened method of removing oil o. gr"r""ltype soils from the surfacc of parls and from opendiscontinuiries. will not remove norganic-type oils(dirt, corrosion,salts,etc.)"and may not remove esinoussoils (plastic coatings,vamish, paint, etc.). Becauseof

the short contact time, degreasingmay not completelyclean out deep discontinuitiesand a subseouent olventsoak is recommended.

Al.l.l,4 Alkaline Cleaning:(a) Alkaline cleanersare nonflammablewater solu-

tions containing specially selecteddetergents or wet-ting, penetrating,emulsifflng, and saponifying varioustypes of soils. Hot alkaline solutions are also used forrust removal and descaling to remove oxide scalewhich canmask surfacediscontinuities.Alkaline cleanercompoundsmust be used n accordancewith the manu-faclrrrers' ecommendltions.

aution:parts

cleaned ythe alkalineclenningprocessmustbe rinsed ompletelyfree of cleaner and thoroughly dried by heat pdor tothe penetrnnt inspcction process lpart temperatureatthc lime ofpenetrant aFplica(ionshall rot exceed 125.F(52"C)1.

(rJ Steam cleaning is a modification of the hot-tank alkaline cleaning method, which can be used forpreparation of large, unwieldy parts. It will removeinorganic soils and many organicsoils from the surfaceof prns, but may not reach to the bottom of deepdiscontinuities, nd a subsequentolvent oak s rccom-mended.

L1.1.7.5 Ultrasonic Clcaning - This methodaddsultrasonicagitation o solventor detergent leaningto improve cleaning efficiency and decreasecleaningtime. It should be used with water and detergent fthc soil to be removed is inorganic (rust, dirt" salts,conosion products, etc.), and. wirh organic solvent ifthe soil to be removed is organic (grease and oilyfilms, etc.). After ultrasonic cleaning, pans should beheated o rcmove the cleaning fluid, then cooled to atleast 125"F (52"C), before applicationof penetrant.

l{1.1.1,6 Paint Removal - Paint filrns can be

effectively removed by bond release soivent paint re-rnover or disintegrating-type hot-tnnk alkaline paiDt

ARIICLE 24 _ LIQUID PENETRANT STANDARDS sE-r6s

strippgrs. n most cases, he paint film must be com-

pletely removed to expose &e surface of the metal.Solvenrtypepaint removerscan be of the high_viscositythickened type for spray or brush applicaiion or canbe of low viscosity twolayer t)?e for dip-tank applica-tion. 80th types of solvent paint removersare gen-raliyused at ambient temperalures,as received, Hohtankalkaline sfippers are water-soluble powder compoundsgenenlfy used at 8 ro 16 ozJgal (60 ro lZ0 kg/ml ofwaterat 180 o 200.F (82 to 93.C). After paint removal,the pans must be thoroughly rinsed to renrove allcontamination rom the void openings and then thor_ougbly dried.

Al.l.l.7 MechanicalCleaningand SurfaceCon_ditioning - Metal-removingprocesses uch as tiling,buffing, scraping,mechanical nilling, drilling, reaming,grinding, iquid honing,saniling, athecutring, umbieor vibratorydebuning,and abrasive lasting,ncludingabrasivessuch as giass beads, sand, aluminum oxide,ligno-cellulosepellets,metallic shot, etc., are often usedto rcmove such soils as carbon, rust and scale, andfoundry adheringsands,as well as to debun or prorlucea desiredcosmelic effect on the parl .Thet processe:may decrease he ffictiveness of the pc,letront exanli a-tion by smearing or peening over metal surfaces and

flling discontinuities open to the surface, especlall1.for soft meralssuchas aluminum, itaniwn, magnesiun,dnd beryllium allo .

41.1.7.EAcid Etching- Inhibitedacid solurions(pickling solutions) are routinely used for descalingpart surfaces.Descaling s necessary o remove oxidescale,which can mask surface discontinuitiesand ore-vent penefant from entering. Acid solutions/etch;ntsarc also used routinely to renrove smearedmetal thatpeensover surfacediscontinuities.Such etchantsshouldbe uscd in acconlancewith thc manufacturers' ccom-mendations.Caution:

NOTE Al - Etched ns andmalerial$mustbc rinscdcomDletelvfree of etchank, rlc surfacc neutralized snd lhoroughly dri;d biheatprior to application f p€netrana,Acids'and chromates anadverselyaffad thc nuorcscence f fluorcsccnt matcrials.

:{OTE A2 - Wh€never h€rc is a possibiliry of hyd.ogenembritlle-mcnt as a resDltof acid solution/etching,he pan should be bakedat a suitable lcmperaturcfor an ap?rcpriare ime to remove rhehydrogcn before furthcr proccssing.After baking, rhe part sballbe cool.d lo a lempcrsture elow 125"F 52.C) bcforoapptyjnspenetrants-

41.1.1.9 Air Firing of Ceramics- Heating ofa ceramic pan in a clean, oxidizing atmosphere s aneffective way of removing moisture or light organicsoil or both-The maximum emperaturehat will not



sE-165 2001 EcTIoN

aeI

aaI

oaaaaa

I

at

oI

a

aO

I

I

aa

toat

ao

oaooo

cause degradation of the properties of the ceramicshould be used-

, A1.2 Post Cleaning

41.2.7 Removal of Developer - Dry powderdeveloper can be effectively removed with an air blow-off (free of oil) or it can be removedwith water rinsing.Wet developer coatings can be removed effertively bywaler rinsing or water rinsing with detergent either byband or with a mechanical assist (scrub brushing,washing machine,etc.). The solubledeveloper oatingssimply dissolve off of the p.artwith a water rirse..

At.2.2 Residualpenetranrmay be removed hroughsolvenr action. Vapor degreasing 10 min minimum),solvent soaking (15 min minimum), and ultrasonicsolveot cleaning (3 min mininrum) techniquesare rec-

ommended. In some cases, it is desirable to vapordegrease, hen follow with a solvent soak.The actualtinre required in thc vapor degreaser nd solvent soakwill dcpend on the nature of the part and should bedetermjned xpcrimentally.

42. Methods for Measuring Total ChlorineContent in Combustible Liquid penetrant

Materials

A2.l Scope and Application

.1.2.1.1These methods covcr the detemrinationofchlorine in combustible iquid penetrantmaterials,iquidor solid. lts rangeof applicability is 0.001to 5% using

. either of the aliernative titimehic procedures.Theproceduresassume hat bromine or iodine will nor beprescnt- If these elements are present, they will bedetected and reponed as chlorine. The full amount oftheseelementswilt nbt be reported.Chromate nterfereswith the procedures,causing low or nonexistentendpoinls. The method is appticableonly to materials hatare totally comb,lsrible.

A2.2 Summary of M€thods

42.2.1 Tlte sample is oxidized by combustion na bomb containing oxygen under pressure Caution,see 42-2.1.1). The chlorine compounds hus liberatedare absorbed n a sodium carbonatesolutiofi and theanount of chloride present s determined itrimetricallyeilher against_silvernitrate with the end point detecredpotiometrically (Method A) or coulomefiicallywith theend point detecredby cuEent flox, increase MetbodB).

42.2.1.1 Satety - Sbict adherence o all ofthe provisions prescribed hereinafter ensuresagainstexplosive rupture of the bomb, or a blow-out,provided

the bomb s of properdesignand constuctionand ingood mechanical ondition. t is desirable, owever,that the bomb be enclosed n a shield of steel plateat least72 n. (12.7mm) thick, or equivalentprotection

be providedagainstunforeseeableonlingencies.

A23 Apparatus

AJ.3.l Bonb, having a capacityof rot less than300 nL, so conslructed hat it will not leak duringtbe ' est,and that quantitativerecoveryof the liquidsfrom the bomb may be readily achieved. The innersurface f the bomb may be madeof stainless teelor any other naterial that will not be affected by thecombustionplocessor products.Materials used n thebombassembly,uchas the headgasketand eadwireinsulation,hallbe esistanto hcatandchen)ical ction,

andshallnot undergo ny reactionhat will affect hechlorine contentof the liquid in the bomb.

4.2.3.2SanpleClp, plntinum,24 mm in outsidediameter t the bottom,27 n)m n outsidediameter tthe top, 12 mm in heightoutsideand weighing 0 toll g, opaque usedsilica, wide-fonnwith an outsidediameter f 29 nrn at the top, a height of lg mm,anda 5-mL c-apacityNote ), or nickel Kawincapsuleform), op diameter f 28 mltr, 15 mm in height,and5-mL capacity.

NOTE A2.l - Fused silica crucibles arc mLlcb more economic:rland longer-bstilg than platinum. After each use, they should be

scrubbcd out with 6ne, wer emcry cloth, heated to dull red healo\€r a bum€., soaLed n bot wa(fi for I h, then dried alld storedin a desiccator before reuse.

42.33 Firing lVire,platinum,approximately o,2 6 8 & S g a g e .

42.34 lgtition Circuir (Note A2.2), capableofsupplying uf{icient urr€nt o ignire the nylo,r hreador cottonwickingwithoutmelting he wire-

NOTE A2.2rCsution The swi[ch Drhe gnilioncir<uitshaitbeof s type thar rcnrninsopeo, cxcept when h;ld in closcd posirionby drc opcmror.

42.3.5Nylon Sewing hread,or Co on Wickhs,white-

A2.4 Purity of Reagenrs

42.4.1Reagent radechemicals hall be used nall tests.Unless therwisendicated,t is intendedhatall reagents hall conform to the specificationsof theCommittee n Analytical Reagents f the AmericanChemicalSociety,wheresuchspecificationsre avail-able.Other gades may be usedprovided t is flntascetainedhat he eagents of sufliciently ighpuriry

ti,

478



mlna

' .9;

to permit its use without lessening he accuracyof thedetermination. '

A2.42 Unless otherwise ndicated,refercnces owater shall be understoodo mean efereegrade eagentwater conforming to Spe4ificatiohD 1f93.

A2,5 Decomposition .

425.1 Reagen* and,Materi-als:

A2.5.7.1Oxygei, free of combustiblematerialand halogencompounds, vailableat a pressure f 40atm (4.05 MPa).

A2.5,1.2 Sodiun Carbonate Solution (50 gNazCO/L) - Dissolve50 g of anhydrousNa2CO3 r58-5g of Na2CO3H2O)or 135g of Na2CO3 lOti20in water and dilute to I L.

42.5.1,3WhiteOrl, refiner.

42.5,2 Procedure:

L2.5,2,1 Preparatioi of Bomb and SampleCut a pieceof firing wirc apprcximalely 00 mm inlength. Coil the middlesection about20 mm) andattach he free ends o the terminals. rrange he coilso that it will be aboveand o onesideof the samplecup. Place 5 mL of Na2CO3 olution n the bomb(NoteA2.3),placehecover n hebombandvigorouslyshake or 15 s to distributehe solution ver he nsideof the bomb. Open the bornb,place the sample-filledsamplecup ir the terminalholder,and inserta shonlength of threadbetween he firing wire and sample.Use of a sample weight containingover 20 mg ofchlorinemay cause onosion f thebomb.The sampleweightshouidnot exceed .4g if lheexpectedhlorinecontent s 25Voor above. f the samples solid,notmore than 0.2 g shouldbe used.Use 0.8 g of wiriteoil with solidsamples.f whiteoil will be used Note

A2.4), add it to the samplecup by meansof a dropperat rbis time (Csution, seeNotesA2.5 nd A2.6).

NOTE A2.3 - Aftcr tep€ated scof rhebornb or chlo.incdetermina.tion, a 6lm may bc loticed o the inncr ru.facc. This dullncssshould b€ retnovedby Friodic polishin8of tic bomb. A satisfactorymethod fo. doing this is ro iot tc thc bomb in { larhc at abour 300rpm and polish thc ihside surtacc with Crit No. 2/0 or cquiyaleorpaper coatedvith a light rnlchitrc'oil o prevcntcutti 9, and thenwith a pasteof grit-frec cbmmic oxrdc atrdwatdr.This proccdurcwill removc all but vcry dccp prtf and put a high polish on rh€surface.Befo.e using thc botrh it shoutd bc wa,rbedl,itlt rorp srdwater o rcmoveoil or pastc cft from tbe polishingopcration.Bomtlswith porousor pincd surfacesshouldncvcr bc used bccauscof thctendcncy to rctain chlorinc frD|n laqlc to ramplc. Csutlon: Donot use morc lhsn I g total of sanple ad wbitc oil or otherchlorinc-

frce codbustible mat€rial

NOTE A2,4 - lf |}|e ;;pb is nor radily miscible with whir€ oil.some other nonlolatil., chloriDc-fr€4combustiblcdilucnt may be

^The mlnimumpressuresre specifredo proyideslf,icjert oxygetforcompleteombustionnd he maximum ressuresresent safetyreouirement.

employedn placeof whiteoil. Howevcr, hecombiledweighrofsamplcand nonvolatilc ilucnr shall not exceed g. Some sol;d6dditivesro relari\,cJynsoluble, ut mry be satisfactorily umedwhcncovcrEdwith a layerof whiteo;1.

NOTE A2J - The practica f runnirrgattemately amples ighand ow io chlorinccontent houldbe rvoided whenever ossibte.It is difficult o ririse he lnst traces f cblorine rom rhe wr'rs oldc bomband he tendencyor residuai hlorine o carryover fromssmple o samplehasbeenobservcdn a nunrber f laboftrtories.Wbena sanplehigh in chlorinehrs preccded ne ow in chlofinccoDlenthe estor lhe Jow-cblorjrearnple houldbe repertcdandoneor borh of the low values hus obtained houldbe coDsidered

suspectf lheydo DotagEe wirhin he limirs of repearability f thistiethod.

M,5.2.2 Addition of Oxygea - Place Lhc sa ple

cup in position and arrange the nylon thread, or wisp

of cotton so that the end dips into the sample. Assemble

thb bomb and tighten the cover securely. Admit oxygen

(Caution,Note 42.6) slowly (to avoid blowing thesample rom the cup) until a pressures reachedasindicatedn Table A2.1.

NoteA2.6: Caution Do nol add oxygenor ignite rhc sample f

the bombhasbeeqarred,dropped, r tilted.

[t2.5.23 Combustion - Immerse the bomb in

a cold-water rth. Connect he te:rmina,so the openelectrical ircuk. Close hecircuit o ignite he sample.Remove he bomb from the bath after immersion orat least en minutes.Releasehe pressure t a slow,uniformratesuch hat the operatioo equiresnot lessthanI min. Open hebomband examjnehe contents.If traces f unbumedoil or sooty deposits re found,discard he determination,nd thoroughlyclean thcbomb beforeagair putting t in use (Note A2.3).

A2.6Analysis,Melhod A, PotertiometricTitrationProcedure

TABLE 2.1GAGEPRESS RES

Gage ressure,tm MPa)

Capacityol Bonb, mL

300 to 350350 to 400 -

400 to 450450 o 500

38 (3,85)

30 (3.04)

27 (2.14)

40 (4.05)

37 C.75)

32 0.24)29 Q.94)

479



42.6.7.2GlassEleulode,pH measurementype.

42.6.1.3Buret,25-rnLcapacity,.05_mL radu-ations,

42,6.7,4Millivolt Mere4or expanded calepHmeteicapableof measuring to 220 mV.

Note A2.7 - An automaric iraror is highly reommended n placcof ilems42.6.t.3 throuShA2-6.1.4.Rcpeahbilirynd scnsiriviiy fthe me[\od are-rnuch Dhancedy thc auiomadc quiprnenlhr'lemuch €diouseffo( is avoided.

A2.6.2 Reageus and Materials:

42.6.2.1 Acet o ne, chlorine-free.

42.6.2.2 M e hanol, chlorine-frce.

42.6.2,3 SitverNitratc Solution 0.0252N) __Dissolve 4.7910 * 0.0005 g of silver dft,te (AgNO3)in water and dilute to t L.

42.6.2.4 Sodiun Chtoride Solution (0.02g2Nl - Dry a few grams of sodium chloride (NaCI) for2 h at 130 to t50.C, weigh our t.6480 t 0.0005 sof rhe dried NaCl, dissolven wrter, anddilute o I Ll

42.6.2.5 Sul,furicAcid (I + 2) _ Mix I volumeof conccntratedsulfuric acid (H2SOa. p. gr l.g4) with2 volumesof water,

A2,6.3 Collcction of ChlorineSolrrtioa Removethe sample cup with clean forceps and place in a 40O-mL beaker. Wash down the walls of the bomb shellrvilh a llne stream of metbanol from a wash bottle,and pour the washings into the bcaker. Rinse anvrcsiduc nto the bcaker.Nex(, rinse the bomb coverand terminils into the beaker.FinalJy, inse both insideand outside of the sample crucible into the beaker.Washiogs should equal but not exceed 100 mL. Addmcthanol o make I00 mL.

42.6.4 Deterntination of Chlorine - Add 5 mLof H2SOa 1:?) ro acidify the solurion soJution houldbc acid ro litmus and clearof whiLeN:r2CO3 recipibte).Add 100 nrl- of acetone.place thc electrodes n thesolution, staft the sdner (if ntechanical tiner is to beused), and begin titrarion. If tikirrion is manual, settlre pH |lrctcron the expanded rjll ivolrscaleand notetbe rcading. Add exactly 0.1 mL o[ AgNOr solutionfronr the burct- Allow a fcw secondsstirring; thenrecord the new millivolt reading.Subtract he se{ondreading from the first. Continue the tikation, notins

sE-16s

42.6.1 Apparatus:

A2.6.1,1 Silvcr Billet Electode.

each amount of AgNO3 solution and the amount ofdifference between the present rcading and the lastrcading.Continueadding0.1-mL increments,makingreadingsand determiningdifferenccsbetween eadinesuntil a maximumdifference etween eadingss o-b-

tained. he total amomt of AgNO3solution equiredto produce his maximumdfferential is ihe end ooint.Automatic ihatorscontinuously tir the sample,addtitnnt, measurc he potential difference,- a.lculate hedifferential, nd plot'the differentialon a chart.Themaximumdiffercntial is taken at the end poinr.

NOTE AZ8 - For mmi[rum 6.lsitiviry, 0,m282 /V ABNO3sotutionmay be uscdwirh th. auromatic i ,ator, This dilurc riagent shouta*t b-

F_dlviti largc samplci or whcr€ chlorine conrJnt *"y b*

ovef 0,1% sincc thrsc tesB will cattsc cnd ,oints of l0 mi orhi8h€r.Thc large amom( of $,at€furcd io such tit|atioos reducesthc

lff€rcltirl betwc€r re.rdioSs,ma-kin8hc cnd point ve.rydiffiJrto detecl Fot chlodnc contcrt dvcr l% io sample$of O.g I orIarStr, 0.282 lVASNO3solutiotrwill bc rcquirDd o avoid exc€€;in;thc lo-n[ *,ater ditution lieit

42.6,5 Blar* - Make blank determinationswiththe amountof white oil rrsedb|]t omitting the sarnple.(Liquidsamples ormally equireonly 0.15 to 0.25 qof whiteoil while soljds equire0.? to 0.g g.) FolloJnormal procedure,makingtwo or three test runs to besure the results are within the limits of repeatabilitvfor the est.Repeathisbtankprocedurehenevernewbatches f reagents r whiteoil are used_ he pumoseof the blank un s ro measuehechlorine n *re wtriteoil, thereagents,nd hat ntroduced y contarnination.

42.6.6 Standardizatioz Silver nitrate solutionsare not permanenuytable, o thc Aue activity shouldbe checkedwhen the solution is first made uo andthen periodically uring he tife of the solution.Thisis done by titration of 6 klown NaCl solution asfollows: Prepare a mixture of the amounts of thechemicalsNa2CO3olution,H2SO4 olution,acetone.andmethanol) pecifiedor the test.piDetin 5.0 mLof 0.0282-^NaCl solutionand jrrate o rhe endpoint,Preparend iuatea similarmixtureof all thechemicalsexceptheNaCIsolution,husobtaining reagent lankreading.Calculatehe normality f theAgNO3solutionas follows:

^ , _ 5 .0xdx" 61/YAsNO. = --;;----;;-

' r A - v A

where:NegNo, norm;lity of the AgNOj solution,

JVN"cr normalityof the NaCl solution,Vr = millilitres of AgNO3solutiot used or the

titration ncluding he NaCl solution.and

2OOISECTIONV

480

oa

eI

oeaaaaaa

oaaot

o

aooooa

Ioaoaa

aoo

t aa



ARTICLE 24 _ LIQUID PENETRANT STANDARDS

481

where:

Vs --

;

Chlorine,weight% =(ys- I/a)L x 3'545

Vr =millilitresof AgNO3solutionused or thetitration of the reagentsonly.

A2.6.7Calculation- Calculate he chlorinecon-tent of the sampleas follows:

millilitres of AgNO3 solution used by thesample,

Va = millilitresofAgNO3 olution sed y theblank,ly' = normaliryof theAgNO3solution,andW = gramsof sampleused.

A2.6.8 Precisionand Accuracy:

A2.6.8.1 The following criteria shouldbe usedfor judging the acceptabilityf resulis:

A2.6,8,1,7Repeatability Results y rhesameanalystshould not be considereduspe6t nless heydiffer by more than 0.006%or 10.5%of the valuedetermined,whichevers higher.

42.6.8.1.2Reproducibiliry Resultsby differ-ent aboratorieshould ot be considereduspectnlesstheydiffer by more har 0.013% r 2l-3% of the valuedetected,whichevers higher.

A2.6.8.1.3Accuracy - The average ecoveryof the method s 86% to 89% of the actualamountpresent.

A2.7 Analysis,Method B, CoulometricTitration

A2i7.l Apparatus:

42.7.1.1 CoulometricChloride Titrator.

42.7.1.2Beakers,wo, 100-mL, r glazed ruci-bles(preferablywith ly2 in.-outside iameter ottom).

42.7.7,3Ref ge ator.

42.7.2 Reagents:

A2.7:2,1Acetic Acid, Glacial.

A2.7-2.2 Dry Geladnrtixure.

A2.7,2.3 Nitric Acid"

L23.2.4 Sod.iwn hloride Solution 100 meq

C/1. Dry a quantityof NaCl for 2 h at 130 o 150.C.Weighout 5.8440 0.0005 of ddedNaCl n a closedcontainer, issolve n water,and ditute o I L.

sE-r6s

A2.7 3 Reagent Preparation:

NOTE A2.9 - The nofinal reagent prepara(ionprocesshas beenslighdy change4 duc to thc itlerfercnce fmm thc 50 rn|, of wateraequircd o wssh the bomb. This modified processeliminarestheintcrfcrrncc a4d does not alter lhe quality of rlrc tirration.

M.73J Gelatin Solution- A typical prepara-tion is: Add approximately L or hot distilled ordeionizedwater to the 6.2 g of dry gelatinmixturecontainedn one vial supplied y tbe equipmentmanu-facturcr.Gendyheatwith contiluousmixing unti] thegelatin s completely issolvcd.

42.7.3,2Divide nto aliquots achsuffrcientorone day's analyses.Thiny millilihes is enough orapproximately leven itrations.)Keep the remainderin a refrigerator, ut do not freczc.The solutionwillkeep for about 6 nonths in tlre refrigerator.Whenready o uset nrmersohe day'saliquot n hot waterto l iquefy he gelatin.

/12,7.33Glacid AceticAci.l-NitricAcid SoIu-tror A typicalatio s 12.5 o (12.5 arrs II3COOHto I prrt HNO3).

42.7.3.4Mix cnoughgclatin solutionand of' aceticacid-nitricacid mixture for one titration. (A

qpical mixturc is 2.5 mL of ge)atinsolutionand 5,4mL of acetic-nitric cid mixture.)

NOTEA2.10 Thesolution 3ybeprcmjxedn a Iirgerqurnrityfor convenience.ut maynotbeuseablefrer24 h,

42.7.3.5 Run a least thrce blank values andtake an avenge according to the operating manual ofthe titraaor.Determinescparateblanks for both 5 dropsof minetal oil and 20 drops of mineral oil.

A2.7.4 Titration:

42.7.4.1 Weigh to the nearest0.1 g and recordthe weight of the 100-ntl- beakcr.

4,2.7.4.2 Removc the sample crucible tom thecover assemblysupportring using a clean forceps, and,using a wash bottle, rinse both the inside and theoutside with water inro the 100-mL beaker.

42.7.43 Empty rhe bomb shell into the I00-mL beaker.Wash dou,n the sides of the bomb shellwith water.using a waqh bo lc.

A2.7.4.4 Remove (he cover assembly from thecoyer assembly support, and, using the wash bottle,rinse heunder ide, lteplxf inumwirc, and he erninals



sE-165

taaI

ooaaI

o

?001 EcTIoN

where:

R -

inro the same 100,-mL beakcr. The total amount ofwashingsshouldbe 50 t I g .

42.7.4.5 Add specifiedamounrsof gelatin mix_turc and aceticacid-nitric acid mixture,or gelatin mix_

acedc acid-niric acid mixture, if this was premixed,into the 100-mL beaker that contains the 50 g ofwashings includiog the decomposed ample.

t2.7.4.6 TilJate usjng a coulometric itrimeter,according to operaiing manual proccdure.

42.7.5 Calculationr - Calculate he chloride ionconcentration n the sample as fojlows:

Chte,rinr, cighr q" - (r - B)x M

43. Meahod or MeasuringTotal FtuorineContent n CombustibteLiquid penetrantMaterlals

A3.I Scopeand Application

43.1.1This methodcovers he determination ffluorine.incombustibleiquid penetrantmaterials, iquidor solid,that do not containappreciable mounti ofintcrfcring lemen6, r haveany nsolubleesidue ftercombustion.ts range of applicability s I to ?00000ppm.

A3.1, Themeasurefthe fluorine ontent mDlovsthe fluorideselectiveon eleckode.

A3.2 Summaryof Method

A3.2.1The samples bxidizeaUy combustionn

a bomt containing xygenunder pressure Caution,seeA.3.2.1.1).he ffuorinecompoundshus liberatedareabsorbedl a sodium itrate olutionand heamountof fluorinepresent s determined otentiometricallythrough he useof a fluorideselectiveon electode.

43.2.1.1Safety Strict adhercnceo all ofthe provisions rescribed ereinafcer nsuresasains(explosiveupture f thebomb,or a blow_out, rovidedthe bomb s of properdesignand consrrucrio; nd ingood mechanicalondition. t is desirable,horvever.that the bombbe enclosedn a shieldof steel plareat eastyz in. (12.7mrn) hick,or equivalent rotection

be provided gainstunfor€seeableontingencies.

A3.3 Intcrferences

A33.1 Silicon, calcium,aluminum,magnesium,andothermetals ormingprecipitates ith fluoride onwill interferef theyarepresentn sufficient oncenr.a-tionto exceedhesolubilityof their espectiveluorides.Insolublecsidue ftercombustion ill entrain luorineeven f otherwise olublc.

A3.4 Apparatus

A .4.1 Bonb, havinga capacityof not less ha,l300 mL, so constructedhat it will not leak durinsthe test, and that quantitative ecovery of the liquidifrom the bomb may be readilyachieved.The innersurface f the bomb may be made of stainless teelor any othermaterial tbat will not be affected by thecombustionrocess r products.Materialsused n thebombassembly,uchas the headgasketand leadwireinsulation,hallbe resistanto heatandchemical crion,andshallnot undergo ny reactionhat will affectthefluorinecontent f the liquid in the bomb.

counterreadingobtajnedwith the sample,averagecouoterreadingobtainedwith averageof the threeblank readings,

standardization onstllnt.This is dependent nthe nsLnrmentan8e c(t ingn uje and he ead-ing obtainedwith a known amount f the 100rneqof Cl per itre ol solurion, ndweight ]f silmpleuscd.g.

RSD,%0 . l 0

2. 5

5. 9

t

o

a.l

at

aa

at

ot

at

IaI

oI

o

tooao

A?.7,6Precisiottand Accurrtcy:

42.7.6.1Duplicateesults y thesame peratorcanbeexpcctcdo cxhibit hc ollowing clati.,,ctandarddeviations:

Ajrproxinr:rte % Ctrlorinc1.0 and above

0.10.003

42.7.6.2 The nlethodcan bc expected o rcportyalucs thilt t,ary

from the truc valuc by the follorvinganrounts ;

0.1% chlodne and abovc 120.001 to 0.01% cl or ine g% .

42.7.6.3 If brominc is present,36.52dcf thetrueamountwill bc reported.f iodine s present,0.720of the true amount will bc repcrtcd,Fluorine will notbe detected.

482



.

A3.4.2 Sample Cnp, nickel, 20 inm in outsidcdiameter at the bottom,28 mm in outsidediameteratthe top, and 16 mm in height;or platinunr, 4.mm inoutside diameter at the bonom, 27 mm in outsidediameter at the top, 12 nm in beight, ard weighingl0 to l l g .

A3,4,3 Firing Wire, p[1ins61 approximatelyNo.2 6 8 & S g a g e .

43,4.4 lgnition Circuit ([email protected]), capableofsupplying sufficient cunent to ignitr ttt€ nylon threador cotton wicking without melting the wirc.

NOTE A3.l Caudon - The rwiich in tl|c ignitiol cfucuitshall beof a typc that a€Eains opcrl crccpt Eheo h.ld id closcl posirionby thc opcr"ator.

43,4.5 Nylon SewingThread ot Corton Wicking,white.

43.4,6 Funnel,polypropyleneNoteA3.2).

43.4,7 VolumetricF/as( polypropyleng 100-mL(Note A3.2).

A3.4.8 Beaken polypropyleng 150-mL (NoteA3.2),

A3.4.9Pipet, 100-pL,Eppendorf-typeNoteA3.2).'

43.4.10Magnetrc Srirer andTFFcoat€d magneticstirringbar.

A3.4,ll Fluoide Specifc lon Electrodeand s\it-able refercnceelectode.

43.4.12 Mi ivob \leter capableof measuririg o0.1 mV.

NOTE A3.2 - Classwareshould ncvcrbc uscd o baddb e nuoridesolution as t *ill remove luoddr ioss ftold solutioD r onsub$equeotuse carry fluoride on from a cooccntratd solutiotr o ode dhrc dilutc.

A3.5 Reagents

43.5,1Purity of Reagerrr Reigentgradechemicalsshallbeusedn all tests.Unless therwisendicated,it is intended that all reagentsshall conform to thespecificatioasof theCommitteeon Analytical Reagentsof the AmericanChemicalSociety,wherc suchspecifi-cationsare available.Othergr-ades ay be used,pro-vided it is 6rst ascertained hat the reagent is ofsufficientlyhigh purity to perrnit ts usewithout ess-ening the accuracy f the determination.

A35.2 Punty of Water- Unlessotherwise ndcated, all references o water shall be understgod omeanTlpe I reagent

iiiterconforming o Specification

D l 1 9 3 .

Sample WhireOilweighi,g

0.40.6

o.7

0.7

Caution: Do not usc more than 1 g total of sampleandwhite oil or other fluorine.freecombustibtematerial.

A3.6.2 Addition of Orygen - Place rhe samplecup in position and anange the nylon tbread, or wispof cotton so that the end dips into the sample.Assemblethe bomb and tighlen the cover securely.Adnlit oxygen

ARTICLE 24 _ UQT'ID PENETRAM STANDARDS sE-165

4353 Fluoride Solution, Stock (2000 ppm) -Dissolve4.4200r 0.0005g of predried at 130 to150'C for I h, then cooled n a desiccator) odiumfluoride n distilled waterand dilure to I L.

43,5,4Oxygen, ree of combustiblematerialandhalogen ompounds,vailableat a pressure f 40 atm(4.05 MPa).

t3.5.5 Sodiun CitrarcSolution Dissolve27 cof sodium iuatedihydraten wateranddilute to I L:

435,6 SodiumHydroxideSolution (5 N) - Dis-solve 200 g

of sodiumhydroxide NaOH) pellets nwater nddilute o I L; storen apolyethyleneontainer.

43.5.7 WashSolution Modiled TISAB,Total onicStrength djustnentBuffer) To 30CmL of distilledwater, dd32 mL of glacialacetic cid,6.6g of sodiumcitrdtedihydrate, nd 32.15g of sodiumchloride.Stirto dissolve nd thcn adjust he pH to 5.3 using5 ir'NaOH solution.Cool and dilure to I L.

A3.5.8 lVhite Oil, refined,

43.6 Decomposition,rocedure

A3.6.7 Prepuration of Bomb and Sample Cuta piec€of firing wire approximately00mm in length-Coil themiddlesecrion about20 mm) and artach hefree ends o the terminals. rrange he coil so that itwill be above nd o oncside f thesample up.place

10 mL of sodiumcirate solution n the bomb.Dlacethe ccveron the bomb,and vigorouslyshake or 15s to distributehe solutionover he nsideof thebomb.Open he bomb,place he sample-filled ample up intheterminal older,and nserta shod engthof threadbetween he firiqg \.vireand the sample.The sampleWeightusedshould not exceed g. If the sample sa solid,adda few drops of wbite oil at this time to

ensurc gnitionof the sample.

NOTEA3.3 - Us€ of sampteweiShts onrriningovcr 20 mg ofcmori& may causeconrsion of thc bomb. To avoid this ir isrccommendedhat for samples ontainingover2% chlorine, hesample cight be basfd on rhe foltowing rble:Chlorinc

Content,%

5 r o l 0

l0 to 2020 ro 50

wclgor,

0,4

0.20 .1

0.05

483



sE-165 2001SEcTtoNv

oaaoot

oaa

a

oaaaoo

ooooI

a

oaI

ooa

OaaoO

" Theminimum rcssr lre rc specifredo provide uff icientrygenfor Completeombustionnd hemarimum ressLlresresent safetyrequrfemeni.

(Caution, Note A3.4) slowty (to avoid blowing thesample from the cup) until a pressure s reachedasindicated n Table A'3.1.

NOTEA3.4:Caution Do noraddoiygcn r ignite hcsampleif tbf bornb rs beenarred, ronpcd,r titted,

43.6,3 Conbustion - lnmerse the bomb in acold-wxter barh. Connect the terminals to the openelectrical circuit. Close rhe circuit to ignite the sample.Renrove the bomb fiom the bath after immersionforat leas(10 rnin. Releasehe prcssure t a slow,uniformrate such thai the operation rcquircs not less than imin. Open the bomb and exanrine he contents_ftraccs of unburned oil or sooty deposits are found,discard the determination, and thoroughly clean the

bonrb bcforc againpurring r in usc,

43.6,4 CollectiortoJ Fluorine Solution- Removethc samplceup with clcrn ftx.ccps nd inscwith washsolution into a 100-mL voluncrric flask. Rinse th ewalls of thc bomb shell witL a fine streamof washsoludon front a wash bottlc, and add the washings othe dask. Ncxt, rinse thc bornb cover and terminalsinto thc voluntctrjc lrsk. I:inalJy, dd wash solutionto brirs lhc cottcntsof tl)c llxsk to thc lir)c.

A3.i I,rocedure

r\.1.7.1Ascenaiu hc slole (nrillivolrs er ten-fold

changc rr conccntration) f rhc clectrode s describcdbv tl)c nrrnuliclurcr.

A3.7.2 Obraina blrnk soiution y perfomring heprocedurewithorrta sarnplc.

A3,7.3 Imll'Ierse he fluo de and referenceelec-trodcs n solutionsand obtain hc equilibrium eadingto 0.1 mV. (The condirion f tL)e lectrode eierminesthc lcnglh of tine necessaryo rcachequilibrium.Thismay be as l i t t lc rs 5 nrin or ls ntuch as 20 min.)

43.7.4Add 100pL of stock luoridesolutionandobtain the readingafter the same ength of time neces-sary for 43.7.3.

A3.8 Calculation

.43.8,1Calculatehe luorine onaentf thesamnleas follows:

wherc:,CE| = pi11iuo1t

"hangen sarnple olutionon addition

of 100 pL of stock fluoridesolution,482 = q;111uo1,

"hangeir blank solution on addition

of 100pL of the srock luoridesolution,S : slope of fluoride electrode as determined n

A3.7.1, ndW : gramsof sample.

A.3.9Preclsionand Bias

43.9.1Repearability The esults f rwodetermi-nations y thesame nalyst hould oi be considereds[spect unless hey differ by more than 1.1 ppm(0.00011%)r 8.0%of theamounr etected, hicheveris greater.

' 43.9,2ReproducrbrTiry The resultsof two deter-minationsy differentaboratoricshouldnotbe consid-eredsuspectnlesshey differ by 6.7 ppm or 129.0%of (hc anlountdetccted,whichevers greatcr.

43.93 Bl'as The averageecoveryof the methodis 62 to 64%of the amountactuallypresentalthough83 to 85Vo ecoveries an be expectedwith propertechnique.

A4. Determinationof Anions by IonChronratographyvith Condustiyity

MexsutementA4.1Scopc nd Apptication

A4.1.1 This rnethod s condensediom ASTMproceduresnd APHA Method 429 and cDtimized orthe analysis f detrimentalubstancesn oisanicbasedmaterials,t provides single nstrumenteiechniquefor rapid, cquential easuremcnrf commonanionssuchasbromide,hloride,luoride,nitrate, itrite,phos-phate, nd sulfate.

TABLE 3.1GAGEPRESS RES

Gage ressurgtm([4Pa )

CapacityF8omb,:nL min

300 o 350350 o 400

400 o 450450 o 500

40373229

38

30

484



ARTICLE 24 _ IJQUD PENETRANTSTANDARDS

A42 Summary of Method

A4.2.1 The material mustbe put in the form ofan aqueoussolution beforeanalysiscair be attempted.The sample is oxidized by combustion r a bombcontaining oxygen under, ressuraThe products iber-ated are absorbed n the eluantpresent n the bomb'at the time of ignition: .This solution s washed romthe bomb, filtered, and.diluted io a known volume.

L4.2.1.1 A nftena afquot of sample s injectedinto a steam ofcsrbonate-bica6onateluantandpassedthrough a series of ion exchangers.The anions of

interest are separakd on the .basisof their relativeaffinities for a low capacity,stotrgly basic anion ex-changer(guard and separator olumn). The separatedanions are direct€donto a stotrgly asidic catiotr ex-changer(suppressor oluma)where he-yarc convertedto their highly conductiveacid form and he carbonate-bicarbonateeluant is converted o weakly conductivecarbonicacid. The separatednions n their acid formare measuredby conductivity.They arc identified onthe basis of retention time as comparcd o standards.Quantitation s by measurementf peak arca or peakheight.Blanks are prepared nd analyzedn a similarfashion.

A4.2.2, nrerferences Any substancehat hasaretention ime coincidingwith thatof any anion o bedeterminedwill interfere. or examplg elativelyhighconcentretionsof low-molecular-weight rganic acidsinterferewith the deteminationof cblorideand luoride.A high doncentrationof any one ion also interfercswith the resolutionof others.Sample ilution over@mesmany interferences. o resolveuncertairtiesof identif-catior or quantitationusethe methodof known addi-tions. Spuriouspeaksmayrcsult from contaminantsnreagentwater, glasswarc, r sampleprricessing ppara-tus. Because mall sample olumes rc used,scrupu-lously avoid contamination.

L423 MinimumDetectableConcentrationThe

minimum detectable@ncentrationof an anion is afunction of sample size and corductivity scale used.Generally,_rninimum etectableoncentrationsre inthe range of 0.05 mg/L for F and 0.1 mg/L for Bi,Cf , NO3-, NOt, PO43-,and SO42-with a 100-p.Lsample oop and a lGpmho nrll-scalesettingon theconductivitydetector. imilarvaluesmay be achievedby usinga higherscale eningandan electronicnteg-rator.

A4.3 ApparatusA4.3.1Bomb,h'aving capacity f not less han

300 mI-, so constructedhat it will not leak durine

sE-16s

the test, and that quantitdtiveecoveryof the liquidsfrom the bomb may be readily achicved.Tbe innersurface f the bomb may be madeof stainless teelor any other material hat will not be affectedby thecombustion rocess r products.Materialsused n thebombassembly, richas the headgasketand eadwire

. insulation,hallbe esista[t o heatandchemicdaction,and shall not undergoa.ny eaction that will affect thechlorineconrentof the liquid in the bomb.

L43.2 SampleCu2,platinum,24 rnm in outsidediameter t the bottom,27 mm in outsidediameter tOIe op, 12

mm in heightoutside, ndweighing O toll g; opaque usedsilica,wide-formwith-an outsidedia$eterof 29 mm at the top, a height of 19 mm,and a 5-mL capacity Note A4.l), or r,ickel (Kawincapsule orm), top diameterof 28 mm, 15 mm inheight,and 5-mL caplciry.

wOTB e+.t - Fusedsilica ctrcibles are ,tuch morEeconomicaland longer asting har plali nl. Afrer cach use, they shouldbesoubtrd out with finE, wet emcry clolh, heared o dull red heatovcr a bllrr,€r, oated n hor wrter for I h tben dried and sroreditr a desiccatorbelore reuse,

1t4,33 Firing lVirc, platinum, approxin.atcly No.

2 6 B a n d S g a g e .

'443.4 lgnirion Ci?.c t (Note A4.2), capable ofsupplying sufficicnt curent to ignite the nylon threrdor cotton wicking without melting the wire.

NOIEA4.2:Clution Theswitchn the mi(ioncircuil halt cof a g'pc hat cmrins pcn, rccplwhenrct,l n cloredpositionby ihc oPcrator.

A43.5 Nyloz Scwhg Tlvead, or Corton Wicking,whiie.

443.6 lon Chronatogrcph, including an injectionvalvg a sample loop, gurrd, separator,and suppressorcolumns,a temperature-compensatedmall-volumecon-ductivity cell (6 tr,L or less), and a strip cban recordercapable of full-scale response of 2 s or less. Anelectronicpeak ntegrator s optional. Thc ioo chromato-graphshall be capable of delivering 2 to 5 mL eluant/

min at a pressureof 1400 fo 6900 kPa.

1t4.3.7Anion Separator Column,wi:h styrenedivi-nyl-benzene-based ow-capacity pellicular anion-ex-

change resin capable of resolving Br., Cf, F-, NOj-,NO2-, PO43-, and SO+?-;4 x ?50 mm.

4,43.8 Guard Colwnn, identical to scparatorcol-umn except 4 x 50 mm, to protect scpacatorcolumnfrcm fouling by prrticulrrcsor orrlnics.



stt-165

at

aaoaI

ll

t

oaa

I

t

tf

I

t

ooI

ooo

oItoC

o

aoat

o

2001SECTIONV

t\4.3,9 SuppressorColumn, h\gh-capacitycation-cxcbangeresin capableof convettilrg aluant3nd sepa-rated anions to their acid forrns.

/14.3.10Syringe,minimunlcapacityof Z mL andequippedwith a male prcssure itring.

A4,4 Reagents

44.4.7 Purity of Reagenl.r_ Reagentgradechemi-salsshall bc uscd n all cests. nlessotfierwiie indicated,it is intended that all reagentsshall corform to thespecificationsof thc Committecon Analydcal ReagenrJof the American Chcmical Socicty,wheresuchspecifi-catlons are available.Othcr gradesmay be used,pro-vided it is first ascertained hat the reagenthas s;ffi_ciently hlgh purity to permit its use without lesseningtl le accuracyof t l lc determinijtion.

44.4.2 Deionizcd ot Dis ed lVater, free ftom

intcrferencesat the mininum detection limit of eachconsttucnt and llltcred through a 0.2_p,mmembranefilrer to avoid plugging columns,

44.4.3 Lhttut,Sct/utrorr,cdiurnbicarbonate-sodiumcarbonare,0.003ir,1Nal{cor- 0.0024M Na2coj: dis-solve 1.C08 NallCO3 and 1,0176I NazCOj n waterand dilure to 4 L.

44.4.4 flagcncruutSolutiou , H1SOa, N, useIhls regencrant \ l tcl sullprcssors not a continuouslyrcgenerated oc _

44.4.5 RegcnerantSolnbn 2, H2SO4,0.025 N,

dilutc 2.8 nL conc I.{2SO4o 4 I_or 10C nl- regemrantsolutjonI to 4 I_. Use ltis rcgenerant ith continuousregenerationiber suppressorvstcrn.

1,4.4.6 Srandtrd Atrian Solutiotts,100 n)g/L, pre-parc :J sericsof rtlndard aniorr olutions y weighingthc indicatcd nlolrnt.ofsait,dried o I constant eightat 105"C, ro 1000 mL. Srore n plasticbottles n arefrigerator; thesesolutious arc stable fot at leastonenrorth.

clL

t_6485

2,2toor.2876

| 3101L49981.4330

l.8 l4 l

Iight;contains 0 mg/l- eachof Cl-, F, NO3-, NO2-,andPOa'-, I mg Br-lL, and 100mg SOa2-/L. reparcfresh daily.

44.4.8 CombinedWorkingStandanl Solution, nwRange Dilute

100 mL combinedworkins standardsolution, igh range, o 1000mL andstore -na nlasticbottle protected mm light; contains1.0 mslL eachCl-, F, NOi, NO2-,and pO43_,0.1 mg ni-rt, anOl0 mg SO42-/L. reparereshdaily.

14,4.9 Altemative Combined Working StandnrdSolutions - hepare appropriate combinations ac_cording to anion concenhation o be determined. IfNO2-and POaLarenot included, hecombinedworkingstandards stable or onemonth.

A4.5 Decomposition rocedure

44,5,1 Preparation of Bomb and Sample_ C.tta p_iecef firingwire approximately00mm in length.Coil the middlesection about20 mm) and artach hefreeends o the terminals. rrange he coil so that itwill be aboveand o onesideof thesample up.place5 mL of Na2CO3/NaHCO3olution n thebomL.olacethecoveron (hebomb,andvigorously hake or 15s to distributehe solution ver he insideof the bomb.Open hebomb,place he sample-filledamp)e up intheterminalholder,and nsena short enethof thieadbetwcenhe firingwire and he sample. he sampleweightusedshouldnot exceed g. If the sample

(a solid,adda few drops f whireoil at this ri; le roensuregnition of the sample.

NOTE A4.3 - Use of samplcwcighrs onr.ainingvcr 20 mB olcnrofine may cause corrosion of the bonb. To avojd rhis ri i,r€commcndedhar for samplcs ontainingovcr Z% chlorinc, hcsampleweightbe bas€i on the follorvinp:Chlorine

.ontent,

2 t o 5J r o l 0

l0 (o 2020 to 50

Samplc WhiteOilweight,t

0.4o.20. 10.05

CAUTION;Do notusemor€ fur I g total of:sainple ndwhileoil

ol o(herluorine-freeombustibleaGrial.44.5.2 Addition oI Oxygen _ place the sample

cup in position and arrange he nylon thread,or wispof cotton so that the end dips into tbe sample,Asscmblethe bomb and righten the cover securely.Admir oxygcn(Caution, Note A4.4) slowly (to avoid blowing

-ttre

sample from the cup) until a pressure is reached asirdicated in Table A4.1.

NOTE. 4.4:.Caution Do notaddorygcnor ignite hesrmplerr tnc t'omb las bcen jarrcd, droppcd, or tjlted.

werghl.I0. 40.6

0.7

0 , /crt.-Ilr-

Nor-No:_

Poor-

Sooz-

S:Jt

l.*aCl

NJIIr

NxNOr

NaNOr

KII2I}O:

KrSO4

L4"4.7Conbircd \4orkingStandardSolution,HighRtlnge* Conlbinc i0 nrL of thc Cl-, F, NO3-, NOz-,and POa3- tandrrdanion solutions, mL of the Br--lnd 100 nrl ol rhc SO4l- sl:rnLlrrrdolutions, ilute o1000 nrl-, ald store in a plastic bottle protected rom

48 6



.ARTICLE 24 UQUID PENETMNT STAN'DARDS

TABLE 4.IGAGEPRESSUES

Capacityf Bomb, L

GagePressures,tn

mina-

rnar

300 to ,50350 o 40 0400 to 450

450 o 500

38

3027

.37

' The mlnlmum pressures re speclfed o providesufficient oxygenfor completeombustionnd hemaximum ressuresrcrenta atetyrequirement.

A4,53 Combustion Irnmerse he bomb in acold-water bath. Connect the terminsls to the openelectrical ircuit.Close he circuit o igdte the sample.Remove he bomb from the bath after immersionorirt least 0 min.Releasehepressuret a slow,uniformrate such hat the operation equiresnot less han 1min. Open the bomb and examine he contents. ftraces of unbumedoil or sootydepositsare found,discard he determination, nd thorougltlyclean hebombbeforeagainputting t in use.

A4.5.4Collection f Solution Removehesam-ple cup with clean orcepsand rinse with deionizedwater and filter the washings nto a 100-mLvolumetticflask. Rinse he walls of the bornbshell with a finestreamof deionizedvater ftom a washbottle, and addthe washingshrough he ilterpapero the flask.Next,rinse bebomb overand erminals ndadd hewashingsthroughthe filter into the volumetric lask. Finally, adddeionized water to bring the contentsof the ffask tothe line. Use aliquots of this solution for the ionchromi.tographylC) analysis.

44.6 Procedure

A4.6.1 SystemEquilibration-'lurn on ion chro-

matograph ndadjusteluant low rate to appmximatethe separationachieved n Fig. A4.1 (2 to 3 mumin).Adjust detector to desircd sening(usualty l0 pmho)

and let systemcome to equilibrium 15 to 20 min).A stable b-ase ine indicates.equilibrium conditions.Adjust detector offset to zem-out eluadtconductivity;with the fiber supprcssor djuiJt he regenerationlowrate to maintainstabiliay, sually2.5 to 3 ml/min.

44,6.1.1Setup the on chromatographn accord-ance with ihe manufacturer'snstructions.

L4.6.2 Calibrabn - Inject standards ontaininga singleanionor a mixturcanddetermine pproximateretention imes.Obsen d times varv with conditions

I f , 1 0 r l '

FIG,A4.1 TYPICAL NION ROFILE

but if standard eluant and anion separatorcolumn are

used, retention always in the order F, Cf, NO?-,

POa3-, Br-, NOs-. and SOa2-. Inject at leirst three

different conceltrations for cach anion to be measured

andconstruct calibrltioncurveby plott ingpeakheight

or area againstcolcentration on lincr grapl) paper.

Recalibratewhenever the deteclor setting is changed.

With a system requiring suppressor egenention, NO2-

ilteraction with thc suppressormay lead to enoneous

NOt results;make this dcterminaLion nly when the

suppressors at the same stage of exhaustion as during

standardizationor rccalibrrte frequently. In this type

of system the water dip (see Note A4,4) nray shift

slightly during suppressorexhausLionand with a fast

run column this may lead to slight interference or F

or Cl-, To eliminrtc h is inlcrferencc , nalyze tandards

that bracket the expected result or elinrinate the water

dip by diluting ihe samplc with eluant or by adding

concentratedeluant to the silmple to gjve the sameHCOt/COJ- concentration s in thc clurnt. If sample

adjustments are made, adjust stand rds and blanks

identically.

NOTE 44.4 - Watcr dip .)ccurs bccausc wilcr cooductivity ir

sample is less lhan eluant conductivity (€luanl is dilutcd by water)-

44.6.2.1 t linearity s establishedor a 3ivendete€tor setting, it is acceptable to calibratc. with a

single standard. Record dre peak height or area and

retention ime to pernritcalculationof tlie calibration

factor. F.

A4.63 SampleAnaly.rr.r Renrovesanrplepanicu-

lates, if necessary,by filtering through a prewashed

0.2-pm-porediam menrbrane iltcr. Using a prewashed

sE-16s

48"t



sE-165 2001 EcItoN v

oao

: aoaoao

n '

oa

oooooo

oaoaoo

oaaaoo

oa)

oo

syringe of 1 to l0 mL capacity equippedwith a malcluer fitting inject sample or standard. nject enoughsainple to flush sample loop several times: for 0.1mL sample loop inject at Icast I mL. Switch ionchromatographfrom load to injcct mode and rccord

peakheights and retentjon imes on strip chart recordcr.After the last pcak (SO42-) has appearedand theconduccivity signal has returned to base ine, another

sanlplecan be injected.

44.6.4 Regenerati.or For systemswithout fibersuppressor egeneratewith I N H2SOa n accordancewith the manufacturer's nstructionswhen he conductiv-ity base line excecds300 pmho when the suppressorcolumn is on l ine.

A4.7 Calculation

44,7.1 Calculate cr.nccntrationof each anion, in

rug/L, by refcrring to the appropriate alibration curve.Alternatively, when the response s shownto be linear,use the following equation:

C = H x l : x D

rvherc:

C = ntB anion/L.

ry : peak height or arca,

F = response lctor - conceltration of standard/hcjght or arca)of srandard,nd

D = dilution actor or those amples equiring i-Iu l ion.

, TABLE 4.2PRECISIONND ACCURACY BSERVED ORANIONSAT VARIOUSCONCENTRATIONEVELS N REAGENT

WATER

Amaunt AmountAdded, Found,

Aniofl mglL mg/L

Siogle-

overall operator SignifrcantPreclsion, Precision, Bias 5%

ms/L nglL Level

F- 0.48 0.49F- 4.84 4.b4ct 0.76 0.86cF 17 r7.2cf 455 471N0 , , , 0 .45 0 .09Nor 2r.8 19.4Bf- 0.25 O.25Br- 13.7 72,9Poot- o.t8 o.1oPoot- 0.49 o,i4

N0r- 0.50 0,3)N0r- t5. l 14,8soor- o.5r 0.52S0o'- 43.7 43.5

0.O3 No

0.46 No0 .11 NoO,41 No

13 No

0.04 Yes,neg

1.3 Yes,neg0.02 No0.6 l lo

0,03 Yes,neg

0.I7 Yes,neg

0 .03 No0 .9 No

0 .03 No

2 ,? No

0.050.520.380.82

46

0.09

0.041, 0

.0.060.15

0.16

0.07

48 8

A4.E Precisionand Bias

A4.E.1Samples f reagentwater to which wereaddcd hecommon nionswereanalyzedn 15 abora-torieswith the resultsshown n Table A4.2.

. .n r...



liquid PenetrcntnspectionRevised y J.S. Borucki.Ardrox Inc., qnd Gqil Jordon, HowmetCorporofion

LIQUID PENETRANT INSPECTIONis a nondestructivemethod of revealingdiscontinuitieshat areopen o thc surfacesof $olid and essentially onporousmateri-als. Indications f a widespectrum f flawsizes anbe found regardlessf thc config-urationof the workpieceandregardless fIlaw oricntations.Liquid penetrants ecpinto various ypes of minutesurfaceopen-

ingsby capillaryaction.Bccause fthis, theprocesss well suited o thedetection falltyp6 of surface cracks, laps, porosity,shrinkage reas, aminations,and similardiscontinuities,t is extensively sed or theinspection f wroughtand castproductsofboth errousand nonferrousmetals.Dowdermetalluryyparts, cemmics,plastiCs,andgLassbjects.

In practice, he liquid penetrant rocessis relativelysimple o utilize and control.The equipment sed n liquid p€netrantn-spection an vary from an atmngement fsimpleankscontaining enetraflt, mulsifi-er, anddeveloper o sophisticatedomput-er-controlled utomated rocessing nd n-

spectiansystems.Establishing roceduresand standards or the insp€ctionof specificpartsor productss critical or optimumendresulls_

The liquid penetrantmethoddoes notdependon fe.romagnetism as does, forexample,magnetic articlenspection), ndlhe arrangementfthe discontinuitiess nota factor.The penetrantmethods effectivenot only fo. detecting urfacelaws n non-magneticmetalsbut also or revealing ur-face laws in a variety ofother nonmagneticmaterials.Liquid penetrant nspection salsoused o inspect remsmade rom femo-magnetic teels;generally,ts sensitivitys

greater than that of magnetic particle in-specnon.

The major imitation of liquid penetrantinspections that it can detectooly imper-fcctions hat are open o the surfacai omaother mcthodmust be used or detectingsubsurface laws. Another factor that canlimit thc us€ of Iiquid penetrdnts s .surfaceroughness r porosity.Suchsurfaces ro-

duce excessivebackgroundand interfcrgwith inspection.

Phyrlcol Pdaclpler

Liquid penetmnt inspection depc[dsmainlyon a penetmnt's ffcctivclywettingthe surfaceof a solid workpicceor speci-men, flowing over that surface to folm acontinuous nd easonably niform pating,and then migrating nto cavities hat areopen o the surface. he cavities f interestare usuallyexceedingly mall,often nvisi-ble o the unaided ye,The abilityofa givenliquid to flow over a surfaceaDd entersurface avitiesdepends rincipallyon thefollowing:a Clearliressof tbe surface. Confrgurationf thecavity. Cleanlinessf the cavity. Sizeof surfaceopeningof the cavity. Surfaceension f the iquid. Ability ofthe liquid o wet the sudace. Contactangle f the iquid

Thecohesiveorcesbetweenmolecules f aliquidcause urfaceension.An example fthe influence of surface tefision is the ten-dencyof free liquid, suchas a droplet ofwater, to cotrtlact iDto a sphere. In such adroDlet. urfaceension s counterbalanced

by the intemal hydrostaticpressure f theliquid,When he liquid comes nto contactwith a solid surface, the cohesive o.ceresponsibleor surface ension competeswith the adhesiyeorce between he mole-culesof the liquid and the solid surface.These orces ointly determine he contactangle,0, between he iquid and he surface(Fig. l). If 0 is less han 90" Fig. la), the

liquid is said to wet the surface, or to havegoodwettingability: f the angles equal oor greater han 90' (Fig. lb and c), thewettingability s considered oor.

Closely elated o wettingability is thephenomenonf capillary iseor depression(Fig.2). Ifthe contactangle,0, betweenheliquidand the wall of the capillary ube isIess han 90' (that s, if the iquid wets thetubewall), he iquid meniscusn the ube sconcave,and the liquid rises in the tube(Fig. 2a). If 0 is equal to 90', there is nocapillarydepression r rise(Fig,2b).If 0 isgreat€r han 90", he liquid is depressednthe ubeanddoesnot wet the ubewall, andthe meniscuss convex(Fig. 2c). In capil-lary rise (Fig. 2a), the meniscus oesnotpull rhe liquid up the tube; rather, thehydrostatic ressuremmediately nderahemeniscuss reducedby the distributionofthe surfaceension n the concave urface,and the liquid is pushedup the capillarytubeby the hydraulically mnsmittedpres-sureof the atmosphereat thefr€e surfaceofthe iquidoutside he capillary ub€. Figure3 clearlyshows he forces hat cause iquidto rise n a capillary ube.

The height to which the liquid rises isdirectlyproportionalo the surface ensionof the iquidand o the cosine f theangle fcontact,and t is inverselyproportional o

good well n9 -

f ig. t y1'ff"tT:fi:jics o5 rl@i€d by ihe onsle. e, hrrwn d droplel of liquid ondc rclid *rfoe. Good *{ine t obtoiftd *hd 0 < eo'(o); poor w€nin€. w}l€n



E - o Ri € or dep'e|rion in sdlollvcrticol copillo.y lub. , d€rernii€d by d'€ conrod ongl€ 0, b€re€€no liquida .qilhry h,b. Io)

g < 9C: dpilldrt ris. (b) 0 = 9o': m @pillory deFdrion or ds.(c) 0 > 9Oo:coFillory d.pr.lsion

72 / t$erhods of Nondestructive Eyqluqtion

thedensity of the liquid and to the radius ofthe capillary tube. If, as in Fig. 4, thecapillary ube s closed,a wetting iquid willstill rise n thc tube: however. herewill be

extra pressure esulting rom the air andvapor compressedn the closed end of thetube, and the capillary rise will not b€ asgreat,

These examples of surfaca wetting andcapillary rise illustrate the basic physicalprinciples by which a penctrant enters finesurfacc discoltinuities even though thepractical cirCumstances ncounter€d n theuse of liquid penetrantsafe more complexthanthe6eexamplesmay suggest.Cracks,for example,are not capillary ubes, butsimulate he basic interactionbetweenaliquid and a solid surface, which is respon-sible for the migrationof penetrantsntofine surface cracks.

Theviscosityof the iquid s not a factorin thebasicequation f capillary ise. Vis-cosity is related o the rate at which a liquidwill flow under some appliedunbalanced

stress;n itself, viscosityhas a negligibleeffect on penetrating bility. In general,however,very viscous iquids are unsuit-ableaspenetmnts ecause hey o not lowrapidly eoough over the surface of theworkpi€ce; onsequently,hey requireex-cessivelyong periodsof time to migrateinto fine laws.

Anothernecessary ropertyof a pene-tant is its capabilityof dissolving n ade-quateamount f suitableluorescent r vis-ibl€-dye ompounds. inally, hepenetrantliquid must be removablewith a suitablesolvenUremoverr emulsifierwithoutpre-cipitatinghe dye.

Just as it is imponant hat a penetmlt

ent€rsurfacelaws, t is also mportant hatthe penetrantbe retained n the flaws andemerge rom the flaw after the superficialcoatiflg s removed rom the surlaceand thedevelopers applied. t is apparently par-adox hat the same ntemctionbetweenaliquidanda surface hatcauseshe iquid oentera fine opening s also esponsibleorits emergencerom that opening.The reso-lutiol of the paradoxs simple:Once hesurface asbeen reedofexcess enetranttbecomes ccessibleo th€entrappediquid,which, under the effect of the adhesiveforces between iquid and solid, spreadsover the newly cleanedsurfaceuntil anequilibrium istributions attained Fig.5)-

Alrhough |t somecases he amountofpenetrantn a surface ead t equilibriumis suff iciento b e detectedisually, ensi-tivity is vastly increased y the useof adeveloper, of which there are severaltyp€s available formsA, B, C, and D)-When applied, a developer orms a finesurface ilm, that is, a spongelike ystemof very ine, random apillarypaths. f thepenetrant ontacts hepowder, hepowderthen competeswith the freshly cleanedsurface f the workpiece or the penetrantas t flows out of the defect. f thc devel-

Fd= zTtrzhEo

Upward lorce (r. ) i.s €qual to the surlacetension tim€€ th€ FeiiBete ot the Eeruscus:

Fg = (?cos d) (2rrr)

Wher€ r i the inside rsdius of th€ capiUarytube, I ;s th€ h€isht oI the liquid in th€ tube,a is acc€teratior due 1o sravity, , is deDsity olthe liquid, ? is sudace t€nsioD, and 0 is the con-tact anale.

E:- .t Sd€moti. rho{,ins th. fcrc€, invod inr rU' e .(pillory rie, th6 dowMrd fo@ fromEisln of *E lhuid Golumn,qnd $c uorord foe {rm3urloc€ srrion oloog tl|. m.ni . 3 p.rin6i.r

oper is properly designed, t readily ad-sorbs the p€netrant rom the flaw. Thepenefiant ontinues o migrate y capillaryaction, spreading hrough the dev€loperuntil an equilibriums reached. his mi-gratingactiofl is illustmted schernaticallyin Fig. 6. The visibility of thc entrapped

Fis. H:ffi:iH:"fl9#**:rc*pixe rurfoce, ttn pcmlront rcmoir ns in o dii.on-lino'ty Grcrg€ b rhc srfo.. u.lil on cquilibr,um F

Fis.4 rH"ifu'*fi:sHiiil"l,*ff;offe.J.d hy lhe comFer*d ak fttrcpFd in th€ .lor€d.nd. Cohpore h€ighr of liquid in tube +an i. Fig. 3wi$ rhot in the tubs h€re.

Doriiward lorc€ (Fd) k €qual to the weishtof th€ liquid colurm:



r rg.c fflilij""i""ilJif:ll*,'hffif

Denetrantwithin the flaw is greatly in-

ircasedby thc spreading r enlargement f

thc indication.

tvolutlo.| ol tho Prccerc

Tho exact origin of liquid penetrant in-

sDection is not known, but it has beena.ssumedhat the method evolved from theobservationhat the rust on a crack in a

rteelplate n outdoorstorage assomewhatheavier hanthe rust on the adjacentsurfac'esasa resultcf water seepitg nto thecrackand forcing out th€ oxide it had helped to

oroduce.The oblious conslusionwas hat a

iiouid purposelv introduced nto surfacecri"t. ind then brought out againwould

reveal he ocationsof thosecracks.The or y material that fulfilled the known

criteriaof low viscosity,good wettability,and eadvavailabilitywask€rosene.I was

found,however.hai althoughwidercracksshowedup easily, finer on€s wete some-times missedbecauseof the difficully ofdetectirig,by purely visual means, he small

amountsof kerosene exuding ffom them.The Eolution rvas to provide a contrastingsurfac€ hat would reveal smallerseepagesThe properti€s and availability of white-washmade t the oeicalchoice'This meth'

od, known as thi kerosene-and-whitingtest,was he standardor manyyears.The

sensitivity f thekerosene-and-whitingest

could be increasedby hitting the objectb€inc estedwith a hammerduring estingTh€ esultingvibrationbroughtmoreof the

keroscneout of (he cracks and onto the

whitewash.Although his test was not as

sensitiveas thosederived rom it, it was

quick, inexpensive, nd rearonablyaccu-rate.Thus. t orovideda vast mprovementoverordinaryvisualexamination.

Thefirst step €adiu to themethods ow

availablewas he devetopment f the fluo-

rescentDenetrantrocess y R.C. Switzer.

This liquid, used ointly wirh a gr'owder

developer,brought penefiart iNp€ction

from a relatively crudeproc€du.e to a morescieotific peration.With fluolescent ene-

trant. minutc flaw$could be readily detcct-od wien erposed o ultraviolet ight (com-

monlvcalledblack ighO.This dev€lopmentrepreienteda major breakthroughn the

detectionof surface laws.Switzer'swork also ncluded he devcl-

oDmentof the visible-color contrast meth-od, which allowed for inspectionundcr

white ightconditions. lthougi not assen-

sitive as luorcsc€ntpenetrant nspection' it

is widely used n industry for noncritical

inspection.Through he developmentse-

"cribedabov", liquid pen€tmnt nspection

hasbgcomca rnaiornondestructivenspec-tion method.

Pe||slr.tnt molhcdt

Because f the vast differences mongapplicarionsor penetrantlspection. t has

biin necersary o refineand develop h€

two tvDes f penetrantslyp€ , lluorescent,

and iire rl, tisible) nto our basicmelhodsto accommodalehe wide variations n rhe

followingprincipal actors:

a Surface ondition fthe workpiece einginsD€cted

o Chtracteristiasof the flaws to be d€tect-ed

. Time andplaceof inspectiono Size of the workpieceo Sensitivity equired

The four melhodgare broadlyclassiheda5:

Liquid Pen€trant lnsPection / 7

. Water washable,method A

. Postemulsifiable ipophitic, metho'dBr Solvent emovable,methodC. Postemulsiliableydrophilic,method

These our methodsare describedbelow.Wotsr-worhoble Penetrqnl (meth(

A) is designedso that thepenetrao

diiectly waterwashablerom the surface

the workpiece; l do€snot requirea scp

rate emulsification step, as do€s tlpostemulsifiableenetrantmethods.h cr

be used o processworkpiecesquickly at

efliciently. Ir is important, however, th

the washing operation be carefully co

trolled becausewater-washableenetran

aresusceDtibleo overwashing. he esse

tial operaiionsnvolved n this melhoda

iltustrated chematicallyn Fig. ?Portemulsifiqble peneirqnt$ (m€tho.

I ond D) aredesignedo ensureh€-detecti(of minuic flaws in some materials.The'

Denetrants re not directly water washabl

ll€causeof this chat"acteristic,he d&ngerover'rashing hepenetrant out of the flaws

reduced,The difrercnc€betwe€nthe wat€

washableand Dostemulsifiablemethod ies

theuse of an;mulsifier prior to final rinsiDThe emulsifier rEkes the tesidual surfa'D€netrant oluble n water so that the exce

surface penetrant can be removal by tl

water rinse. llerefore. che emu.lsificatit

time mustbe carefully controlled so that tl

surfac€D€netnntb€comeswater solublebthe oeretrant i( the llaws does not. T1

opeAtions nvolved n the postemulsifiab

methodare llustratedschematically n Fig

for the ipophil;c yslemand n Fig. 9 for tl

trvdropfrlfii system. Despitc the addirion

Droc4ssinsteDsnvolvedwith thepostemusfiabte rnerhoitsS and D, th€s€methodsa

the most reliable or detectingminute flaw

Solvent-rcmovoblcPenctrqnl (methc

G) is availableor usewhen it is necessalto inso€ctonlv a localizedaf.eaof a wor'

pieccor to inipect a workpieceat the si

iather than on a production nspectionb

sis. Normally, the same yPe of solvent

used or precleaning nd for removinge

cess penetranl.This pe[etrant process

convenient nd broadenshe rangeofapp

cationsof penetrantnspections.Howeve

operoiionWot er -wosh emovo lo f

l i qu idp€ne l ron t roh su r f oce

t ig, 7 ri* **tlot op"rqtiqr {s liquid Fdncrtqir inip'<iion q3i's rh€ worera$hoble v5r'h



74 / Methods of Nondestructivc Evoluqtion

O9€rotion oFerotio.?Appl icot ionf iquid aopl icot iont €muGil ie/Denelronlo su.toce to iouid enerronr

Fig. 8 op"."rion' 1i" odd ion ro prlcteonins) for the

becausehe solvent-removable ethod slabor intensive, it is not practical for manyproduction applications,When properlyconductedandwhen used n theappropriateapplications,he solvent-removableethodcanbe one of the mostsensitive enetrantmethodsavailable.The operations or thisprocess re llustrat€d chematicallyn Fig.to.

Whicheverpenetralt method s choseo,the degree and speedof excessp€netra[tremoval dependon suchprocessingconditronsas spmynozzlecharacteristics, aterprcssure afld temperature, duratioD of lhennsecycle, surface onditionof the work-piecc,aDd nherent emovalcharacteristicsof thepenetrant mployed.

OpeErion 3 Operotion 4Combination oI Woter,rssh removol of

emuls i f iera.d lqo id pene l ron t rom sur foce

liquid peneiranr

poltenuliiffobls, mG rd t lipopl'ilic liquid F.l'.tront sy.r.m

De3.rlptior ol the Procerr

Regardlessf the typeof penetrant sed,that is, fluorescenttype ) or visible typeII), penetrant iospectioo requires at leastfive essential teps,as ollows.

SurfqcePrrpqrofion. All surfaceso beinspected,whether localized or the entireworkpiece,mustbe thoroughly cleanedandcompletelydried before being subjectcd openetrant mpection. Flaws cxposed o thesudac&mustbe ree Fom oil, water.or othercontaminatts f they are to bedetected.

PenetEtion. After the wod(piecc hastreencleaned,pcnetrant s applied n a suit-able mannet so as to form a film of thepenetrant ver he surface. his ilm should

r€mainon the surfaccong enough o allowmaximum penetrationof the penetrant intoanysurfaceopeningshatare prcsent.

Removol of Exc€ssPenelrcnt. Excesspenetrant musl be rcmoved from the sur-face. The removalmethod s det€rminedbvthc

ype ofpenetrant sed.Some enetrantican be simply washed away r ith water;others require the use of emulsifiers (lipo-philic or hydrophilic)or solvent/removcr,Uniform rcmoval of excess surface pene-trant is necessaryor elTectivenspection.but overremovalmust b€ avoided.

Developmsnt.Depending D he form ofdeveloping Bent o be used, he workpiecels driedeitherbeforeor directlyaffer appli-cation of the developer.The developerformsa lilm over the urface. It acts as ablotter to assist the natural seepageof th€penetrant out of surface openings and tospreadt at the edges o as to enhancehepenetranandication.

Inrpedion. After it is sufficientlydevel-oped, he surface s visuallyexaminedo.indications of tnnetrant bleedback fromsurface penings, hisexaminationmustbeperformedn a suitable ospection nviron.ment, Visible pcnetrant nspections per.tormed n goodwhite light. When luores.cenl pen€trant is used, inspection isperformedn a suitablydarkened reausingblack (ultraviolet) ight, which causes hepenetranto fluoresce rilliantly.

foterlols Ulod lnPetrotr{rnl Incpecilon

In addition o th€penetrantshemselves,liquidssuchasemulsifiers, olvent/cleanersandremovers, nd developers re requiredfor conductingiquidpenetrantnspection,

Penetr.onls

Thereare two basic yp€s of penetrants:

a Fluorcscent,ype I. Visible, ype II

Emulsifi€d liquid penel.qni

Prerinse,wateFwash Application of emulsifie.

o l(qui<tpenetrani

Operation 4 Ope..fon 5Coftbination of Watepwash rcmovat olemutsifier and tiquid pe^etant hom surtacs

l i q i d pene l . an t

Fig. 9ory..t"- 1i"odditiono p{dldnins) or E

Each ype is available or any oneof the fourpoitemulsifioble.rhod ,hydropl'iliciquid en€ronr methods (water washable,postemulsifiable

lipophilic, and postemulsifiablehydrophilic,

Emuls i f i ed iq i d pener ran t



Fig. tO Op-"ri"* 1inoddirion ro pr6<loonins) or th6 lohenr-dnavobb liquid Fi.t€nt ly3tsm

Operolion I . Operotion eApplicorion ol liquid Solv€nlcleoner removol ofp€netront lo surfoce liquid penelront trom swfoce

Op€f o i i o . 3 Opero l i onApplicotion of Insp€ction

Liquid Penetrcnt Inipection / 7l

methodB, lipophilic,andmethodD, hydrcphilic. Both can act over a rangeof durations from a few seconds to severaminutes,depending n the viscosity,coceritmtion, method of application, an,chemical omposition f the emulsifier,awell as on the roughness f the workpiec

surface.Th6 length of tirDean emulsifieshould emain n contactwith thepenetrardepends n the ype of emulsifier mploye,and he oughness fthe workpiece urface

Method B, lipophilic emulsilierr areo:based, reusedas supplied, nd unctionb:difrusion Fig. ll). The emulsifierdiffuseinto the penetrantilm alld renderst spontaneously mulsifiablen watgr.The rate awhich it diffuscs nto th€ penet.antestablishes he emulsificationime. The emulsifier is fast acting, thus making he emulsificatiol operation very critical. Th,emulsifier ontinueso act as ongas t is ircontactwith the workpiece; herefore, h,rinseoperation hould akeplacequickly r

avoidoveremulsifiation.Method D, hydophilic emulrifiers ar,

water basedand are usually suppliedaconcentrateshat are diluted in water tconcentrationsof 5 to 30%for dip applicationsand0.05 o 5% for sprayapplicationsIlydrophr'lic emulsifiers unction by displacing excesspenetrant rom the surfaceof th,partby detergent ction Fig. 2)- The forcof thewatersprayor theair agitation fdiltanksprovidesa scrubbing ction.Hydrophilic emulsitier s slower acting han th,lipophilicemulsifier; herefore, t is easreto control he cleaning ction. n additiol t(the emulsifierapplication,methodD alsrrequires prerinsc,UtiliziDS coarsewate

spray, heprerinse elps emove heexces.Denetranto minimizecontamination f thLmulsifier.Of greatersignificarce,only ;very hinanduniform ayerofpenetrantwilremainon the surface, hus allowingeaslremovalof the surfaceayerwitb minimunopportunity fremovingpenetrantrom thflaws. This step is requiredbccause hpenetrantsnot misciblewith thehydrophilic emulsifier.

Thepenetmntmalufacturer should eco[mend nominal emulsificatioo times for thsp€ciJiq yp€ of emulsifier n use. Actu,emulsification times should be determineexperimentallyor theparticular pplicatiorThe manufacturershould also r@ommenthe concentrations or hydrophilic emulsif,ers.

SolYent Cleoner/Removers

Solvent cleaner/removersdiffer fronemulsifiersn that they remov€excess urface pen€trant hrough direct solvent a(tion. There are two basic ypes of solvenremovers: lammableand nonflammableFlammable leaners re essentiallyree (

halogens but are potential lir€ hazardlNonflammable leanets are widely use(Howev€r, heydo containhalogelat€d o

andsolvent emovable)mentionedn the sec-tion "Penetra[t Methods" in this article.

lype I fluor€scent penet]lnt utilizespeoetrantsthat arc usually green in colorand tluorescebrilliantly uder ultravioletlight. The sensitivity ofa fluoresceatp€ne-trant dependson its ability to form indica-tions that appear as small sourcesof light io

an otherwise dark area. Type I pcneffantsare available in dillerent sensitivity levelsclassified s ollows;

. Level t/2|Ul ralowa Lerel li Low. Level 2: Mediumo Level3: High. Iatel 4i Ull.J.a,high

lype ll visible penetrqntemploys pen-ehant that is usually red in color and pro-duces ivid red ndicationsn contrast o thelight backgound of the applied develop€runder visible light. The visible pe[etrantildications must be viewed under adequatewhite ight. The sensitivityofvisible pen+

trants is regardedas Level I and adequatefor many applications.

Peneliqnt selcctionqnd u:e dependonth€criticaliry of the iDspectioD,be condi-tion of the workpiece surface, the type ofptocessing, nd he desired ensitivity seethe section Selectionof PenetraltM€th-od" in this article).

Method.A, water-washableenetrcntsare designed for the removal of excesssurface penerant by water rinsing directlyafter a suitable penetmtion (dwell) time.The emulsifier is incorporat€d nto the wa-ter-washableenetraot.When this type ofpenetrant s used, t is extrcmely importantthat the removal ofexcess rurface p€netrantbeproperly controlledto preventov€rwash-ing, which can cause the p€netraot tb bewashed ut of the flaws.

Methods R and D, Iipophilic ond hydro-philic pos emulsiftablepenetranl,tarc itl.sol-uble n water andther€for€noa e.novablcbywaterrinsing alone.They are designed o b€sel€ctivelyremoved rom the surfac€of theworkpi€€eby theuseofa separate mulsifier.Theemulsifrer,properlyappliedand €ft fo. asuitableemulsification ime, combineswiththeexcesssurfacepenetranto form a water-washablesurfacemixture that can be rinsed

from the surfaceof the workpiec€.The p€n-etrant that remainswithin the flaw is notsubject to overwashing.However, properemulsification ime must be establishedex-perimentallyand maintained o ensure hatovercmulsification,which results n the lossof flaws.doesnot occur.

MethodC, solvent-rcmovableenelrunts

areremovad y wipingwith clean, int-freematerialuntil most mcesof the penetranthavebeen emoved.The remaining racesareremoved y wipingwith clean, int-freematerial lighdy moistenedwith solvent.This type of pcnetrant is primarily usedwh€re po.tability is required aDd for theinspection f localized reas.To minimizethe possibilityof removing he peoetrantfrom discontinuities,he use of excessiveanountsof solventmustbe avoided.

Phyricolond Chemicolchorc€terirtic..Both fluorescent and visible penetrants,whetherwaterwashable, ostemulsifiable,rsolvent emovable,must haYe enainchemi-cal andphysicalcharacteristi'csf tbey are to

perform heir ntendedunctions, heprinci-palr€quirements f penetrants reas ollows:

. Chemical stability and uniform physicalconsistency

. A llash point not lower than 95 C (200

"F); penetrants hat have lower flashpointsconstitutea potential fire hazard

. A higlt degreeof wettabilirya I-ow viscosity o permitbettercoverage

and minimumdragout. Ability to penetratediscontinuitiesquick-

ly and completely. Suffrci€ntbrightnessand permanenceof

color. Chemicalnennesswith materials eing

iospect€d ndwith containers. Low toxicily o protectpersonDel. Slowdryingcharacteristicsr Ease of removal. Inoffensive dor. Low cost. Resistanceo ultraviolel ight andheat ade

EmulsifiersEmulsifiersare liquids used to rendet

excess enetmtlt n lhe surface f a work-piecewaterwashable. herearetwo meth-ods used n the poslemulsifiablemethodl

_-.



Diffu.ion p.oc€edsAi.sing

Flg. | | er-'*.r. n rt* frD.iioni,rs t tipopriticeNtsifi€r,

_ Required PEpertioi. To carry out |lsIuncttons o the fullest possibieextent,aoeyelopermusthave he following proper_ues ot characterislicsrarelyare all rhesecharacteris(icsresent o optimumdegreesrn anygven materialor formulation,but all

mustbe consideredn selecting developer):

a The.developermust be adsorptive omaxrmizelott inq

o It musthave ine-grain izeanda particleshape hat will disperse nd expose nepenetrantat a flaw to produce strongandsharply defined indications of flaws

a It mustbecapable fprovidinga conrrasrbackgroundor indicationswhen color-contrastpenetrants re used

a It mustbe easv o aDDlv. It must orm aihin. uniiormcoatingouer

a surtacea k mustbeeasilywette.d y theDenetrant

at the law (the iquid mustbeallowed ospread vcr the particlesurfaces). It must be nonfluorescentf used wilh

fluorescent enetrantsI It must be easy o removeaftcr inspec-

uona It must not contain ingredientsharmful to

pans being insp€ctrd or to equipmentusedn the nspection peration

. It mustnotcontainngredientsarmfulor

76 / lvlerhods of Nondestrucllye Evoluslion

lhmor36 in rqueous

Solutlon .ad dfitlsion

vents, which may render hernunsuitablelor someapplications.

.Excess urfacepenetrants removedbywprng, using int-freeciothsslightlymoisr-enedwith solventcleaner/remover.t is [otIecommendedhatcxcess urface enekantbe_cmovedby floodingthe surfacewithsolventcleaner/remover,ecause he sot_vent will dissolve he penglranlwithin thedefectand ndicationswillnot beproduced.

Developers

. The purpose f a developers to increasethe bnghtnessntensityof fluorcscentndi_

cations and the visible contrast of visible-penetrantndications. he developeralsoprovidesa blotting action, which sirves todraw p€netrant rom within the flaw to thesurface,spreadinghepenet.antandeDlarg-ing the appeamnce f the {law,

- The developer i$ a critical part of therDsp€ction rocess;borderline ndicationsthat mightotherwiseb€ miss€dcanbe madsvisibleby thed€velop€r.n all applicationsof liquid penetrant nspection,usc of adeveloper s desirablebecauset decreases

insp€ction.timeby hasteninghe appear-anceot tnotcallons-

toxic o the op€rator

Agit.tion.nd Rinsingomutsiricaiiod

Fig. t 2 Ebmenr, in d,e frJ.oionins of Lydrophitic ed,kiti.rs

Developer Fonns. There are four fomsof developersn commonuse:

. FormA, dry powdera FormB, watersoluble

o Form C, water susD€ndiblea FormD; nonaqueousolvent uspendible

The characteristicsf each orm are dis-cussedbelow.

.Dry powder developers (form at arewrdely used with fluorescena enetrants,but should not be used with visible-dyepenetrants ecause heydo not produc€asaustactoryontrast oatingon the surfaceor-lheworkpiecc, deally,dry powderde-veropers houldbe light and luffy to allowlor easeof application nd shouldcling todry surfacesn'a ine ilm. Theadherencefthe powdershouldncitbe excessive, s heamountof black ight available o energzelluorescentndications

will be reduced.For purposes f storage nd handhng swellasappllcations,owders houldnoi benygroscoprc,nd heyshould emaindry. Ifthcy pick up moistur€whenstored n areasof highhumidiry.heywi lose heirabiliryto flow anddusteasily, nd hey mayag-glomerate. ack.or lump up in containersor In developer hambers.

For reasons f safe(y.dry powderdcvel-opersshould ehandledwithcare.Likc anvotherdustparticle,t candry the skinan itmtate the liningof the air passages,aus-lngrmtation. fan operatorwill be workingconlrnuouslyt a deveiopertation,ubber



glovesand respiratorsmay be desirable,Modern equipmentoften includesan 9x-haustsystem n the developer prayboothor on the develop€r ustchamber hat prc-ventsdust rom cscaping. owder ecoveryfiltcrs are included n most such nstalla-t ions.

Water-solubledeveloperr(fom B) caltrbeused or both fluor€scenttype ) or visible(type I) postemulsifiablcr solvent-remov-ablep€netrants.Water-soluble evelopersare not recommendedor use with water-washable enetmnts, ecause f thepoten-tial to wash he penetrantrom within tlleflaw if the developers not very carcfullycontrolled. Water-solubledevelopersaresupplied as a dry powder concenhate,which s then dispersedn water lr recom-mendedproportions,usually rom 0.12 to0.24WL (l to 2 lb/gal.).The bath concen-tration s monitoredor specific ravitywiththe appropriat€ hydromet€r. Necessaryconstituents f the developersncludecor-rosion nhibitorsand biocides,The advan-tages of this form of developer are as fol-lows:

. The preparedbath is completely solubleand therefore do€snot require any agita-tion

. The deyeloper s appliedpdor to drying,thus decreasinghe developmentime

. Thc dried developer ilm on the workpieceis completely water soluble and is thusessily and completely removed ollowinginsp€ction y simplewater insi[g

lVater-suspendibleevelopersf(nm C) cabe used with either fluoresc€nt(typ€ I) orvisible (type

II)penetrants.With fluorescent

penetrant, the dri€d coating of developermust not fluoresce,nor may t absorbor filterout the black ight used or inspection.

water-susp€fldible evelopersare sup-pliedasa dry powderconcenkate,which sthen dispersed n water in recommendedproportions, sually rom 0.(X o 0.12kg/L(% to I lb/gal.).The amountof powder nsuspensionmust be carefully maintained.Too much or too little develop€r on thesurfaceof a workpiece can seriously afrectsensitivity.Specificgravity checks shouldbeconductedoutinely,usinga hydrgmeterto check the bath concentration.,Water-soluble developers contain dispersing

agents o help retardsettlingand cakingaswell as inhibitors o preventor retard cor-rosionof workpiecesand equipment,andbiocides o extend he working ife of theaqueoussolutions. ln addition, wettingagents re prcsento ensure vencoverageof surfaces nd easeof removal after in-spection.

wat€r-suspendible eveloper s appliedbeforedrying; therefore,developing imecanbe decreased ecausehe heat rom thedrier helps o bring penetrahtback out ofsurfaceopenings.n addition,with the de-veloper ilm already n place, he develop-

idg actionbeginsat once. Workpieces reready or insp€ctionn a shonerperiodoftime.

Nonaqueous olvent-suspendibleevel-opers(form D) arc commonlyused or boththe fluarescent and the visible penerantprocess. his orm of developer roduces

white coating on the surface of the part.Thiscoating ields he maximumwhitecol-or contrast with the red visible penetrantindication and extremely brilliant fluores-cent ndication.

Nooaqueous olvent-suspendibleevel-opcrsare suppliedn the ready-to-useon-dition and containparticlesof developersuspendedn amixtureof volatilesolvents.The solvents are carefully sele€rcdor theircompatibilitywith the penetrants.Non-aqueous solvent-suspendibleevelopersalso contain surfactants in a dispersantwhose unctionsare to coat the padiclesand reduge heir tcndency to clump or ag-glomerate.

Nonaqueous olvent-susp€ndibl€evel-oDersare the most sensitive orm of devel-operusedwith type I fluorescentpenetr&ntsbecausehe solvent action contributesotheabsorption ndadsorptionmechanisms,In many cases wher€ tight, small flawsoccur, the dry powder (form A), water-soluble (form B), and water-susp€ndible(fom C) developers o not contact theeotrappeCp€netmnt, This results in thefailureofthe developero create he neces-sary capillary action and surface t€nsionthat serve to pull the penetrant from theflaw. Th€ nonaqueous olvent-suspendibledeveloper ntem he law aoddissolvesntothe penetrant.This action increases hevolumeand reduces he viscosityof thepenetrant.The manufacturermustcarefullyselect and compound he solvent mixture.There are two types of solvent-basedev€l-ooers:nonflammable chlodnatedsolvcnts)a;d flammable (nonchlorinated solvents).Both types are widely us€d. Selectionsbasedon the nature of the application andthetype of alloy being rlspected.

3olecrlon olPenGt clt mdhod

The size, shape, and weight of work-pieces,as wcll as the numberof similar

workpieceso be nspected, ftennfluence

the selectionof a p€netrantmethod.Sen itiyity ond Coit. The desired egree

of sensitivity nd cost are usually he mostimportant factors in selecting the properpenetrantmethod or a givenapplication.The methods apable f the greatest ensi-tivity arealso he mostcostly.Many nsp€c-tion operationsequire he ultimate n sen-sitivity,but therearea significant umber nwhich extreme sensitivity s not requiredandmay evenproducemisleadingesults.

Liquid Penetrqnt Inspection / 77

varietyof produclion nspection perationsthan the visiblepenefant methods,whichare utilizedprimarilyfor localized nspec-tions.As statedearlier,penehants reclas-sifiedon the basisof penetrantype:

t Iype fi Fluorescent|

rype /I: Visible. MethodAi Waterwashable. MethodRi PostemulsifiableJipophilica MethodCt Solvent emovable. MethodD, Postemulsifiable-hydrophilic

Penetrants re also classified n terms olsensitivity evels:

a Level t/2',Ultralowa Level i l-,owc Level2: Meditmt Level 3: Iligho Level 4: Ultrahigh

Advqnlqger qnd limifolions of Pcn€-trqnl Methodr. Each pcnetrantmethod,wbethcrpostemulsifiableeither ipophilic

or hydrophilic),solvent cmovable,or wa-ter washable, sing luorescent r visible-dye pcnetrants,has inherent advantagesand imitations.

The postemulsifiableluorescentpene-tran, method s the mosl reliableand sensitivc pc[etrantmethod,This procedurewilllocate wide, shallow laws as well as tightcracks and is ideal for high-productio0work. On the other hand, emulsificationrequiresan additionalop€ration,which o-creases ost. Also, this method equiresawater supply and facilities for inspectionunder black light. The postemulsifiable,lipophilic fluorescentpenetrantmethod sless seositiveand less reliable than thehydrophilic method. Its use is thereforedeclining.

Thesolvent-rcmovableluoresce4lpene'trant methode$ploys a proceduresimilalto that used or the postemulsifiable luores-cent method,except hat cxcesspenetranlis removedwith a solvent/remover. hitmethod s especiallyecommendedor spotinspection r wherewatercannotbe conve.dently us€d, t is mor€ sensitive han th(water-washableystem, but thc gxtrem(

caution and additional time required forsolvent emovaloftenprecludets use.

The waterwashable luorescent pene'trant method s lhe fastestof the fluorescenlprocedures,t is alsohighly sensitive, eliable,and reasonably conomical.t can beused or both small and large workpiecesand s effective nmostpartsurfaces. ow'ever, t will not r€liably revealopen,shal-low flaws foverwashed nd n somecases.depending n the sensitivity evel of th€penetmnt,will not lo€ate he very tightesrcracks. There is also the dang€r of overwashing y applyingwater or an excessiveperiodof time or with a pressure ufficiento r€move th€ penetrant from the flaws.

On a practical asis, he fluorescenten- The postemulsljiable visible PenetrunetEnt methodsare employed n a wider method is used whenever sensitivity re



78 / fllethods of Nondestrucfive Evoluation

quhed s greater han that providedby thewater-washableisible penetrantmethod,However. the addirionalstep of applyingemulsifiermakes his sys(emmorecostlythan the water-washableisible pcnetrantdye method hat requireswater, but other-wise no ocation imitationsare mposed.

The solvent-retuovableisiblepenetruntmethodhasa distinctadvantagen that allthe nec€ssaryngredients re portable;ac.cordingly, it can be used in a practicallylimitlessnumberof lo€ations,both in theshopand n the field. Bccause f the Drob-lems nvolved n penetrantemoval,howev-er, themethods gen€rally onfined o spotinspectionor to inspectionunder circum-stanceshatprohibit he useof othermeth-ods because f workpiecesize or location.

The watetwashable visible peneuantJy.rtea is the fastest and simplestof allpeneuant echniques. t is, however, heleastsensitivebecause hg p€rletfant s like-ly to be removed rom wide, shallow laws.Therefo.e, t is most useful n thoseappli-cationswhereshallow and relativelywideflaws are not significant.This method salso the least sensitave or locating tightcracks. t rcquiresa water source,but canbe performed n almost any locatioo be-causeneithpra darkened reanor electric-ity is required.

Equlprnent RequliomontrThe €quipment sed n the penetrantn-

spectionprocessvaries from sprayor aero-sol cans o complex,automated, omputer-driven processingsystems. Some of the

moregenerally

sed ypesofequipmentaredescribedn the followingsections.

Portcble EquipmentFor occasionalnspections,speciallyn

the field, where equipmentponabiliti isn€cessary, inimalkits for eithervisibleorfluorescent enetrant nspectionare com-mercially available. (Cenemlly, portablepenearantpplications re limited to local-ized areasor 6pot inspections ather thanentirepart surfaces.)

Sucha kit for visiblepenetranrnspectionwork includesa precl€aner,a p€netrant,and a penetrantemoveranddevelop€r, llin pressurizedpraycans.Penetrantemov-

al requireswipi.rgwith lint-free clothsorpaper owels.A similarkit is available or fluorescent

work; a precleaner, penetrant, enefantremov€rand developerare likewise sup-plied n pressurizedans.Cleaningr ai-complished y wiping wirh lint-freeclothsor paper owels.This kit includesa small,ponableblack ligh( for conducring he in-sPection.

Stotiondry Inspection EquipmentThe type of equipmentmost frequently

used in fixed installationsconsistsof a

seriesof modular$ubunits.Each subunitperformsa special ask. The numberofsubunitsn a processinginevarieswith thetyp€ of penetrantmethodused. The sub-unttsare:

a Drainand/ordwell statiols

a Penetrant ndemulsiner tationsa Pre-andpost-wash tations. Drying sationa Developer tation. Inspcction tation. Cleaning tations

The drain or dwell stationsare aatuallyroller-top encheshat hold hepartsduringthe processing ycle. The usual arrange-ment s to positiona drain or dwell srauonfollowingeachof the dip tanks,the washstation,and he dryingov€n. The suoun[sare described n more detail below,

PcnetrqntStqtion,Theprincipal equire-m€rt of a penetraotstatioD s that it provid€a means for

coating workpieces withpenetrant----eitherll over, for smallwork-pieces,or over smallareasof largework-pieceswhen only local inspcction s re-quircd. In addition, means should beprovidedor draining xcess enetht backinto the penetranteservoir, nless hc ex-pendableechniques beingused,Drainingracks usuallyserve hc additionalpurposeof providinga storage lace or partsduringthe time required or penetration dwellumet.

Small workpieccsare easily coatedbydipping hem nto a resewoirof penetrant.This maybedone ndividually r in batchesin a wire basket,

The peneftant aontainer should beequippedwith an easily emovable over oreduceevaporationwhen not in use. Adraincock shouldalsobe provided o facil-itatcdraining f the ank or cleaning.Con-tainersare usuallymade f steel,but stain-le$ssteel containers hould be usedwithwater-baseenetrants.

For largeworkpieces, enetrants oftenapplied y spmying r flowing.This s donemainly or convenielce ut also or econo-my, becausehevolumeofpenetmntneed-ed o mmcrse arge bjectmaybesogreatas to increaaeunnecessarilyhe originalcost of installation,A small reservoirofpenetrantequippedwith a pump, a hose,

anda $prayor flow nozzles usuallyalmostai fast a meansof coating argeobjectsasthe dippingoperation, or this type of op-eration, he penetrant tationconsists f asuitablyve[tilatedbooth with a rotatablegrill plaiformon which heworkpieces set.A drain under he platformretums pene-trant runofTo the sump, rom which it ispumpedback to the spray nozzle-Thebqothenclosure reventshe oversprayingof penetrant n areas utside he penetrantstatroo.

In somcapplications,t hasbeen ound hatonly a smallamountof penetrants r€cover-

able and reusable,and this has led to theadoption of the expendable echnique forsomevery largeworkpieces.n this tech-nique, penetrant s sprayedover the work-piece n apenetrantstationsimilar to tne onementioriedpreviously.The penetra[t isstoredn a separate ressure

ank ntted with ahoseand a spraynozde. The spraybooth isnotequipped ith a sump o recoverexcesspenetrant.nstead, he booth s fitted withwaterspraynozdes anda dmin so that it canservethe multiple purposeof draining andwashing.A decision to use the expendabl€techniqueand related equipment should b€basedon a careftrlanalysisand considerarionofcost, ime, aleofproduction, ndhandlingproDlems.

Emuhifier Stqtion. The emulsifier iquidis containedn a tank of suflicicntsizeanddeptho permitmmersionfthe workpreces.either ndividually r in batches.Coversaresometimespmvided to reduce €vaporafion,

and drain valves are supplied for cleanoutwhen the bath has become contaminated.Suitable drain racks are also a part of thisstationand areused o p€rmitexcessemulsi-fier to drain back nto the tank,

If largeworkpiecesmust be coatedwithemulsifier,methodsmust b€ devised toachieve he astestpossible overage.Mul.tiple spraying r copious lowing of emulsi.fier from troughsor perforated pipescafl beusedon some ypcs of automatic quipment. For the local coatingof largeworx-pieces, prayings often satisfactory, sugtheexpendableechnique escribedor theapplication f peoetmnt.

Prc- qnd PorhinseSlotionr. The warer

rinsing (washing)of small workpieces sfrequently oneby hand,either ndividuallyor in batchesn wire baskets.The work-pieces reheld n thewash ank andcleanedwith a hand-held pray using water at tappressure nd emperature. he wash roughor sink shouldbe large enough and deepenough so that wolkpieces can be easilytumed o cleanall surfaces.Splashshieldsshouldseparatehe rinse statidn rom pre-ceding(p€netrantor emulsifier)and iuc-ce€dingwetdevgloper) tations.Rinsesta.tio s arealwaysequippedwith at leastoneultiaviolet ight so that the progress f re-movaloffluorcscent eletrantcan beeasilyfollowed.

The automatic rinsing of small work"pieces is satisfactorilyaccomplishedbymeansof a rotating table. Tbe basket isplacedon the table,and water-spray eadsare properly ocatedso as to rinseall sur-facesof theworkpieceshoroughly.

Specially built automatic washers forrinsing workpieces hat are large and ofirregular ontou are often nstalled.Spraynozzlesmustbe ocated o suit the individ-ualapplication.

The removalof exc€ss enetrant y sim-ply submerginghe workpiece n water isgenerally or recommended.owever, n



somecases,simple submersionn an air-agitated water bath is satisfactory.

The rinse station s subject o corrosion,Allsteelshouldbeprotectedby rustproofingandpainting.Mo$ sarisfactory,but more cos0y,is the use of stainless tcelequipment,

Drying Stqtion. The rccirculating hot-air

drier is one of the most mportantequipmentcomponents.The drier mustbe arge enoughto easily handla the type and number ofworkpiecesbeing nspected.Heat input, airflow, and rateof movement f workpiecesthrough the drier, as well as tempemturecontrol, areall factors hat must be balanced.The drier may be of the cabinet type, or itmaybe designed o hat theworkpiecespasstliough ona conveyor. fconveyor operationis us€d, the sp€edmust be consideredwiththc requireddrying cycle,

Electric-resistancelementsre requent.ly used as sources of heat, but gas, hotwater, and steam are alsoused. Heat inputis controlled by suitably located thermo-

statsand s determined y workpiece ize,composition, nd ate of movement.

Integrated quipmentnvariablyncludesthe recirculating hot-air drier mentionedpreviously.Makeshiftdriersare sometimesused----oftenecausenothingbetter is avail-able. El€ctric or gas hot-air blowers ofcommercialdesign have been used, butbecause o controlof temperatures possi-ble, theseare very unsatisfactory nd areordinarilyusedonly on anemergencyasis.Infrared ampsare not suitable or dryingwashedworkpieces,because he radiantheatcannotbe readilycontrolled.

Equipment designed o handle work-pi€cesof special izeandshape equiresa

speciallydesigneddrier- Each drier is aseparate ngineering roblem nvolving aspecial ombination f workpiece omposi-tion, mass, surfacearea, speedof movc-ment, and other considerationsniquetothe circumstances,

DevelopsrStqtion.The yp€ and ocationofthe develop€r tationdepend n whetherdry or wet developer s to be used. For drydeveloper, the developer station is down-str€am tom thedrier, but for wet developerit immediately recedeshe drier, ollowingthe rinse station.

The dry4eveloper starior.usually consistsof a simple bin containing hepowder,Driedworkpiecesar€ dipped nto lhe powd€r,andthe excess powder is shakenoff. targerwo*pieces maynot be soeasily mmers€d nthepowder,so a scoop s sually provided orthmwing powder over the surfaces, afterwhich he exc€sss shaken ff. The developerbin shouldbe e4uipp€dwith an€asilyrcmov-ablecoverto protect he develop€rrom dustanddirt when not n use.

Dust control aystems are sometimesrcededwhendry developeris sed.Controlis accomplishedy a suction pening crossthe back of thebin at the op, which drawsoff any developer dust that rises out of the

bin. The dust-laden ir is passedhroughfilter bags, rom which the develop€r ustcan be reclaimed or further us€(Fig. l3).

Developer powder can also b€ appliedwith air pressure, his system equiresnobin, but it does equirea boothor a cabinetand alsomakesdustcollectionmandalory.

Equipmenlor the automaticapplicationof dry developer consists of a cabinetthrough which the dried workpieces arepassedona conveyor. The air in the cabinetis ladenwith dust that is kept agitatedbymeansof a blower. As workpiecespassthrough, all surfacesare brought into con-tact with developerpowder carried by theair. Air mustbe exhausledrom thecabinetand eitherrecirculaled r cleaned y beingpassed hrougha dust-collecting ilter.

Wet develope4whenused, s containedin a tank similar to that used or p€netrantor emulsifier.The hnk should be deepenough o permit workpieces o be suumergedn the developer. hereshouldalso

be a rack or conveyor on which parts canrest after dipping. This will pennit excessdevelooer o run back into the tank.

Suspendible eveloperbaths settle outwhen not in use; therefore, a paddle forstirringshouldbeprovided.Continuous g-itation s essential €causehe settling ateis rapid. Pumpsare sometimesocorporatedinto the developer station for {lowing thedeveloperover largeworkpieces through ahoseandnozzleand or keepiog he devel-op€r agitated.

In automaticunits, specialmethodsofapplyingdeveloperare required.Flow-onmethods are frequently used. This tech-nique requires a nozzle arrangement hat

permits the workpieces o be covered hor-oughlyandquickly.

Inrpe<tionStotion. Essentially, he in-spection station is simply a worktable onwhich workpieces calr b€ handled uoder

tiqurd Penelrdnt Inspection / 7'

Fis.13H#m,:iH:$H*. *

proper ighting. For fluorescentmethodthe table s usuallysurrounded y a curtaior hood o excludemost of the white ligtfrom thearea.For visible{ry peoetrants,hood is not necessary,

Oenerally,black (ulhaviolet) ights (10

W or greater)are mountedon brackets ror

which they can be lift€d and movedabolby hand.Because f aheheatgivenoff bblack ights,goodair circulation s essentilin black ieht booths.

For automatic nspection,workpicces armoved through booths equipped with splcunains, either by hand, monorail, or bconveyor. In some arge iospcction instalLtions, fully enclosed ooms have b€en buifor black ight nspection.Acc€ss o thc roolis providedby a lighl lock. Inspectionroonmustbe aid out etrrciently o prevent sJect€workpi€ces rom reentering the prcductioline. Figurcs 14 and 15 llustrate typical pel

etrant nspection omponents nd their layotin an nsp€ctionstation nstallation.

Automdied InspeclionEqulpment

For manyyears, h€ p€netrantnspectioof production parts has been a manual ol

Stotion5Drying

Sla l i o . t

Slolion 3

Stotio. 2Oroininq

l i9hr

Fig. 14 lf*ril#T#fs"cqliPftd unii fo' in'F<tins rc*Pi6<€' bv *E EtcFwchot



Liquid developer onk ( ro r )

EiartArro[99mg.tof3qUir,n€nluredinonefoundryforthc| jquidF.ncrrodiBPecl io.ofo|or9ewrieiyo{cd6| ing |or ig id+€. i I i .or ioE.[{dnyof l | |sCo3l in9 r€i i .hondl;is bl. cMe or rcll6r @nvaybr.

80 / l|tethods of Nondeslructive Evoluotion

emtion of moving parts from station tostation through the penetrant ine. Properlytrainedand motivatedoperatorswill do an€xcelleritob of processing nd inspectingparts as well as conholling the process.There are, howeyer, many situations n

which manualprocessingsimply cannotkeep up wiih the production ratesrequiredor conrol theprocess roperly.

Theuseofautomatednspectionystems,therefore, asbecome significantactor nperformingp€netrantnspections f high-

volumeproduction arts.Modern automat-ed penetrant nspectionsystemsprovideprecise nd epeatable rocess ontrol, m-provednspection eliability, ncreased ro-ductivity,and ower nspection osts.

Automated enetrantnspection ystemsincorporateprograrnmableogic control(PLC)units,whichareprogrammedo con-

trol the handliDs fparts

fhrough he sys-lem. o control heprocessingycleprecise-ly, and to monitor the functiols at eachprocessing tation.Figures16 to 18 showtypical automatedpenelmntsystemscur-rently n use.

Procleonlng

Regardlessf the penetrant hosen,ade-quate precleaning f workpiecesprior topenetrantnsp€ctionsabsolutely ecessaryfor accurate esults.Without adequate e-moval of surface contamination, elevantindicationsmaybe missed eaause:

. Theperretrartdoesnot enter he flaw. Thepenetrantoses ts ability to identifythe law becauset reactswith somethingalready n it

. The sulface mmediately urroundingbeflaw retains nough enetranto mask hetrue appearancef the flaw

Also, nonrelevantfalse)ndicationsmaybccaused y residualmaterialsholdingpene-Irants.

Cleoning methodr are generallyclassi-fied as chemical, mechanical, olvent, orany combination f these.

ii||rx{i {I

lch d lfie .obor 3hoM (owr left) to tronrfer

i' f ' l : t

, i rt

,Sl$ ;;i: I

rffi:::;g'rI. X '

r e

Iffilttlrritfflic"rEBS K ar5;

rie. r o ffi l,Hriiffi#'tsi;ti lti.#.iilh1n?r,:1ffi:;*.5y:,."trffg,H /( Automoted nep€<r'on q'ripd€nl setup upp€r €fr) wiih d@-op of op€rororchdkins PtC ponel pF'- ris[l), wtri.fr includero *ren dlploy (l@er righ). ne rerup fforpororos mdrenidlhondlinsdevi..rhe .obor 3hoM (lowr left) ro tronrfer workpi*s from toiion to 3loriono.d to oppl), perekdnh ond orh€r

$lurio.s n€edpd to insDecl .omoonentr.



Fig. | 7 rypi.ot *romot€d flooresent peErrdnr iNpcction i.lrollotio.

Chemicol cleaning methods ncludealka-line or acid cleaning, icklingor chemica.letching,and moltensalt bath cleaning

Mechanical cleaning methodr inch)detumbling,wet blasting,dry abrasive last-ing, wirebrushing, nd high-pressureateror steam cleaning.Mechanicalcleaningmethods houldbe usedwith carebecausetheyoftenmask lawsby smcaring djacent

metal over them or by fillirg them withabrasivematerial.This is more ikely tohappenqith soft metals han with hardmetals.

Solventcleaning methods tlcfude vapotdegreasing,olventspraying, olventwip-ing, and ultrasonic mmersionusing sol-vents.Probablyhe mostcommonmethodis vapor degreasing. owever,ultrasonic

tiquid Penetranl Insp€Gtion / 8l

immersion s by far the most effectivemeans f ensuring leanparts,but t canbea very expensive apitalequipmentnvest-ment.

Cleaningmethods nd heir common sesare isted n Table . A majo. factor n theselectionfa cleaning ethods he yp€ i

contaminanto be removedand he ype ofalloy being cleaned.This is usuallyquiteevident,but costlyerrorscan beavoided yaccuratedentilication f the contaminant.Beforehedecisions made o usea specificmethod,t is goodpracticeo test he meth-od on known laws o ensure hat t will notmask he flaws.

Equallymponantn choosing cleaningmethod s knowledge f the composition flhc workpiece eingcleaned.For example,abrasive umblingcan gff€ctivelyremoveburrs from a machinedsteel castingandleave surfacehat s ully inspectable.hismethod. owever.s notsui(ableor alumi-numor magnesium,ecauset smearshese

metalsand frequently hides flaws. Particu-lar caremustbe taken n selecting clean-ing method or workpiecesabricatedrommore han one alloy(brazedassembliesrenotable examples);a chcmical cl€aningmethod o removescale,stgpoffmatedal,or flux mustbe chosen arefully o ensurethat neither he brazenor the compon€ntsof the assembly ill be attacked.

Ihe rurfoce inirh of the workpiecemustalwaysbe considered,When further pro-ccssings scheduled, uchas machining rfinal polishing, r whena surface idishof3.20 m (125 in,)or coarscrs allowed, nabrasivecleaningmethod s frequentlyagoodchoice.Generally,hemical leaning

methodshave fewer degrading ffectsonsurfaceinish hanmechanical ethodsun-less he chemical sed s stronglycorrosiveto thematerial eing leaned). team lean-ing and solventcleaning arely have anyelfecton surface inish.

Some materialsare subject to delayedreactions s a resultof impropercleaning.Two notable examplesare high-strengthsteeland itanium. f it is ever necessaryochemically etch a high-strength steelwork-piece, t shouldbe bakedat an appropriatetemperatureor a sumcient im€ to avoidhydrogenembrittlement.This should bedone as soonafteretchingas possible utno later than I h. Titanium alloys can be

subject o delayedcracking f they rctainhalogenatedompounds nd are then cx-posed to temperatures xceeding480'C{900

F). CoDsequen, halogenated ol-ventsshould otbe used or titaniumand tsalloys f their complete emovalcannotbeensured.

Choice fcleaningmethodmay bedictat-ed by Occupational afetyandHealthAd-ministration nd Environmental rotectionAgency heallh and safery regulations-Quantitiesof materials hat will be used,toxicity, i tering,neutralizationnddispos-ig. r 8 i:Tffi1#mi*:::*:lll**.'1";;x",m1JJ.g',9"

o'*"rkpeces'<h5



82 / tnethods of Nondestru.tiye Eyolustion

T-oble- Applicqtions of vqrious .hethods of precleoning lorliqsid penetrcnt inrpection

Abrasive rmbling . .. .. , . .. Removingiehl scitr, bu6, wetd,nS ux, b.azestopoff, us1, riti.g hotd, andcoremareriat; hould

nor b€ urd on softm.ralssuchasaluhinum.maSn€stum,. titanium

Dry abrasiv€ riiblastine. .. Removineighr r heavy .ab, nor, sropoff, ust,castinsmoldsd corc mr€rial, spraycd oalings.carbon €posils-inseneral, ny riabledepo3il.Can

wei abrasive.itbralrins. . ."Y.tfjfi'"f"ffi1herc depo,ils.e ishr,euersurface d better ontrolofdim€nsions re requircd

Wir€ 'rushins.. ,. . . . . . . . . . . Removingight qosi tsof s. i te, lux, d stopof iHirh-F€lsur€ ater ndsteam... . . . . . . .. - . . . - . . . . . Ordinar i lya€d i ihan alkdine tean€r. detarg€nr;

r€movinsypicalmachine hop oilssuchas culringoils.polishjngompounds,er€ase, hips,anddeposil$rom €lecticaldhchargemachiningi sedwhcnsurfaccinirh mustbc mainrained;nerpensive

UltEsoric ckani.€ . ,.... -. .. Ordinarity s€d irh d€tergent ndwa:a.o. wiih ̂solv€nt; emovin8 dhercnt hopsoil rom tarSequanlitiesof sdall pans

Alkaline l€aoin8..... _. .... Removins mze topoff, ust, scate, iL, 8rcas€s,

polisbingmllerial, and carbon deposits:ordinarilyusedon hrg. a nicbs wber€ andmerho&@ roolaboriousi lsoused n alumi.ln fo. grossmetal

AcidcteaninS.. . . . . . . . . . . . . Strong olur ionsor r€movingeavy cate; it dsolutionso.lighr scale:weak elching) olutionsor

Morrenartarhreanins . .jiliilliiJ':11"""ffi,# fl:f,l ,"","Solrr[t nethods

Vaporde$€aiing-..... . . .. ,. Renovins ypical hop oil, oit, sndsrcas€; suanyemploys hlorinat€dolv€ntst ot suirabteor

Solventwiping .-.-..-.- ..,. San€ as or vapor csreasinSxcepla hanooperauontmay mp loy nonch'orinaredolvcntst sed orlocalizedow-volum. leanina

workpieces, ndrequired ustomer pecifi-cationsor process arameters.

Postemulsif iable MethodTheprocessingycles or thepostemuisi-

fiableprocesses, ethodB (lipophilic;anomethodD (hydrophilic) re llustratedn theprocessinglow diagrams Fig. 19 and 20,respectively).The major difference be-tween he two methods,as described e-low, is the additionalprerinsesteputilizedin methodD.

Appli<otion of Penelront. Workpiecesshouldbe thoroughly nd uniformlycoatedwrth penetrant y flowing,brushing, wab-bing, dipping, or spraying. Small work-pieces equiringcompletesurface nspec-tion are usually placed in a basketanddipped n the penetrant. argerworkpiecesar€usuallybrushed r spmyed.Electrostat-ic sprayapplications also very effectiveand economical.After the workpiecehasbeen oatedwith a ightnlm ofpenerant, tshould epositioned o hat t candminandso that excesspenetrant annot collect npools. Workpiecesshould not be sub-merged uring he entire penetration welltime. Heating the workpiece s also notnecessary r recommended. ecause er-taindisadvantagesanoccur, suchas vola-tilization of the penetrant,difficulty inwashing, nd a decreasen fluorescence.

DwellTime.After thepenetrarthasb€enapplied o the workpiece urface, I shouldbeallowed o remain ongenough or com-pletepenetrationnto the flaws.Dwelltimewill vary, dependingmainly on the sizeofthedefects ought, leanliness fthe work-piece,and sensitivityand viscosityof thepenetrant.n mostcases. ow€ver.a mini-mumof l0 minanda maximum f 30 nin sadequateor both fluorescent- nd visible-p€netrantypes.A lengthydwell imecouldcause he penetranto begindryingon thesudace,resulting n difficult removal. Ifdryingdoesoccur, t is necessaryo reapplythe penetranto w€t the surfaceand thenbeginhe removal teps,Recommendationsfromthepenetrant upplierwill helpestab-lish the time, but experimentation ill de-termineoptimumdwell time.

Prerinse. fllrcn usingmethodD (hydro-phil ic).a coarsewaterspray rerinsesneededo assistn penetmntemoval nd oreducecontamination f the emulsifier.Acoarse ater pmy srecommended.singpressuref275 o 345kpa(40 o 50psi).Theprerinsewater emperature houldbe l0 to.l{} "C (50 to 100 F)- The prerinse imeshouldbe kept o a minimum rhat s, 30 o90 s) becausc he purpose s to removeexcess enetrant o hat he emulsifier oesnotbecome ontaminatcduickly.

Emulsifier pplicotion, t is very mpor-tant that all surfaces f the workpiecebecoatcdwith the emulsifier t thesame ime.Smallworkpieces redipped ndividually rin batchesn basketsron racks,whichever

al techniques,ndworkerprotection ll are

crucial factors.

Pcn€lrunt IntpettlonProrecrlng P.rarhotert

It is extremely mportant o understandthe significance f adhednc o the estab-l ished rocess arametersor a givenap,plication. ailure o control he processparameterswill affect the quality of the

insp€ction.For example,excessiveover-

washingor overemulsification can removethe penetrant from the flaws; minimalwashing or und€remulsification can resultin excessive background, whish couldmask the flaws and render them undetect-able.

Processing time in each station, theequipment used, and other factors can varywidely, depending on workpiece size andshape, production quantities of similar

Fig, I 9 e.**'i"s nd dios.dm or rheposremukifiobte,othod , tipoFtriti.aqoid erer.oo yjrm



Fig. 2O e.*"i"s {|ow diosromf,' rhe po3r,.muhiffobl., ettrod o, tydrophili. liquid p..€trdrt ryr,eD

l iquid Peneiront Insp€rtion / 83

ately prior to drying by dip, flow-on, orspray echniques. o agitation f thedevel-oper bath is required,Removalof the de-veloper coating from the surface of theworkpiece s required and easilyaccom-plished ecausehedrieddeveloper oatingis water solubleand thereforecompletelyremovable y a waterrinse.

Woter-suspendihleeveloperformC) isappliedust after he final washand mme-diately beforedryiag. Dip, flow-on, andspray rc commonmerhods f application.Caremustbe aken o agitatetredeveloperthoroughlyso that all particlesare n sus-pe$sion;otherwise, ontrolof the concen-tration of theappliedcoating s impossible.Removal f the waier-suspendibleevelop-er can best be achieyedby water sprayrinsing, f allowed o remainndefinitely nthe workpiece, he develope.cao becoDedilncult to remove.

So(vent-suspendibleonaqueous evel-oper JormD) is always pplied fterdryingby spraying, itherwith aerosol ontainersor by coDventional r electrostaticmeth-ods.Proper praying roduces thin.uniform layer hat is very sensitiven produc-ing either tluorescent or red visibleindications.The volatility of the solventmakes t impractical o use n open anks.Not only would th€rebc solvent oss, re-duciog he effectiveness f the developer,but therewould also be a hazardousaporcondition,Dipping,pquring,and brushingare Dot suitable or applying solvent-sus-pendible eveloper.

Deyeloping ime. ln general. 0 mih isthe recommended inimum developingtime regardlessf the developerorm used,The developing ime begins mmediatelyafter applicatioo f the developer,Exces-sive developingime is seldomnecessaryand usually esultsn excessive leeding findications,whichcan obscure law delin-eat|0n.

Inspection$,After the prescribed evel-opmenr ime, he inspectionhould egin.The inspectionarea should be properlydarkened or fluorescent enetrantnspec-tion. Recommeod€dlack ight ntensity 51000o 1600 wcm?. The intensityof theblack light should be verified at regularintervals y theuseof a suitable lack ightmeter such as a digital radiometer.Theintensityof the black light shouldbe al-lowed to warm up prior to use-generally

for about l0 min. The inspectorshouldallow ime or adaptingo darkness; 1-minperiod s usuallyadequate.White ight in-tensity shouldnot exceed20 lx (2 ftc) toensure he best nspection nvironmen(.

Visible-penetdnt ystemsprovidevividred indicationshat can be seen n visiblelight. Lighling ntensityshouldbeadequateto ensureproper nspection;320 o 540 x(30 to 50 ftc) is recommcnded. ightingintensity hould everified t regularnter-vals by the use of a suitablewhite light

is the most convenient.For large work-pieces, ethods uslbedevisedo achievethe astestpossible overage;wo methodsoftenusedare spraying . immersing. o-calizedemulsification f largeworkpiecescanbe achieved y spraying. he tempera-tureof theemulsifier s not extremely rit-ical,but a rangeof 20 o 30 C (70 o 90 F)

is preferred.EmulsiJication ime-The lengthof time

the emulsifier s allowed o remainon theworkpiece nd n contactwith thepenetrantis the emulsification ime and dependsmainlyon the typeof emulsifier mployed,its concentration, ndon thesurlace ondi-tion of the workpieces.Recommeodationsby the manufacturer f the emulsifier anserve sguidelines,ut beoptimumimefora specificworkpiecemustbe establishedyexp€rimenution. he surface inish, size,andcompositionfthe workpiece ill deter-mioemorepreciselyhe choise femulsifierandemulsificationme.Emulsificationimemngesrom approximately0s o 3 minandis directly elated theconcertralion f tbeemulsifier.f emulsificationime is exces-sive, penetrantwill b€ removed rom theflaws,making etectionmpossible.

Rinsing,For all methods, emoving hepenetrantrom the workpieces probablythe most mportantstep n obtainingepto-ducible esults, f penetnotremovals per-formedproperly,psnetrantwill be strippedfrom he surface ndwill remain nly n theflaws. More variabi,ity n individual ech-niqueentcrs nto this particuiarphaseofinspectionhanany other step.Therefore,removalmustbe performedwith the samesequcnce f operations ime aft€r time ifresults re o be rcproducible. his s espe-cially rnportantwhen nspectingor tightorshallow laws.

Rinseimeshould edcrerminedxperi-mentallyor sp€cificworkpieces;t usuallyvaricsrom 0 s o 2 min.Forspray insing.waterpressuie houldbe constant,A pres-sureof about275kPa(,$ psi) s desirable;

too muchpressur€mayremovepenetrantsfro:n the flaws. A coarsewater spray isrecommendedndcanbe assisted ith air(the combined water and atr pressureshould otexceedheprcssureecommend-ed for water alone).Water tempemtur€shouldbe maintained t a relativelycon-stant level. Most penetrants an be re-movedeffectivelywith water n a rangeofl0 to 40"C (50 o 100F).

DryiDg s best done jD a recirculatinghot-air drier that is thermostaticallyoII-trclled. The temperature n the d.ier tsnormally etween 5and95 C (150 nd200oF). The tempcratureof lhe workpiecesshouldnot be permitt€d o exceed70 "C(160'F).Workpieceshould ot remainnlhedrjerany onger hannecessaryl ryingis normallyaccomplishedithina few min-utes,Excessive ryingat high emperaturescan mpair he sensitivity f the nspection,Because rying time will vary, the exacttime shouldbe determined xperimentallyfor each ype of workpiecc.

Devclopingdepends n the form of de-velopero beused.Variousypesof devel-opersare discussed€low.

Dry-developerowder formA) is appliedafler the workpiece has beefl dried and canbe appliedn a varietyof ways. The mostcommons dusting r spraying. lectrostat-ic sprayapplications alsoveryeffective.nsomecases, pplicatiol by immersingheworkpiecenlo hedry powder eveloperspermissible. or simpleapplications,spe-

cially ia/h€n nly a po'iign of the sudace ofa large part is being nspected, pplyingwitha softbrush s oftenadequate. xcessdeveloper an be removed rom the work-pieceby a gentleair blast 1,10 Pa, or 20psi, maximum)or by shaking or gentlerapping. hichever ea ns f applicarionschos€n,t is impodanl hal the workpiecebc completely ndevenlycovered y a fioefilm of developer.

Water-solubleeveloperformB) is ap-plied ust after he final washand mmedi-



E4 / ,Vt€thodsof Nondestructiye Evqluqtion

meter suchasa digital radiometer.Detailedinfomation on inspection techniques savailablen the sections InspectionandEvaluation"and"specificationsand Stan-

dads" in this article.Wofer-Wdshqble Method

- _As ndicated y th€flow diagramn Fig.21, heprocessingycle or thewater-wash-able method is similar to that for Inepostemulsifiablemethod. The differencelies lr the penetrant emovalsteD.As dis-cussed n the section Material; Useo nPenetrantnspection" n this article, thewater-washableenetrants avea built-inemulsifier,hus€liminatinghe need or anemulsilication tep.One rinse operatronsall thal is required,and he washing pcra-tion shouldbe carefully ontrolled

-because

water-washableenetrants re susceptible

to overwashing,linre time shouldbe determined xDeri-mentallyor a specific orkpiece;t usuallyvaries rom l0 s to 2 min.The bestpracticalwayofestablishinginse ime s o view heworkpiece nder black ighrwhile insingandwashing nlyunlil the luorescent ack-gxounds removed o a satisfactorydegree.On some pplica{ions.uchascait ings, nrmmerston nse ollowed by a final sDray

rinsing s desirable o remoye €naciousbackgroundl uorescence. his techniqrie,however,mustbe verycarefully ontrolledto en5urchatoverwashingoes otoccur.

ForspEy rinsing,a nominalwaterpres-sure of 140 o 215kPa (20 to 40 pai) isrecommended;oo muchDressure an re-sult n overwashing,hat ;. the removalofpenelrant rom within flaws, Hydro-airspraygunscan be used.The air pressure,however.shouldnot exceed170kpa (2jpsi).The temperature f the watershouldbe controlledo l0 to 40 C (50 o 100 F).

Drying,developing, nd ospection rocesspammetersre he sameas he Dosaemulsi-fiablemethodprocessparameteridescribedin the section Postemulsifiable ethod',in thisarticle.

Solvenl-Remoyoble llethod

Thebasic equencefoperationsor thesolvent-rcmovable€netrantystems gen-erallysimilar o that ollowed or theotnermethods- typicalsequences shownbythe flow diagram n Fig. 22. A norabtidifferences lhat rvith he solvent-remov-able method he excesspenetrants rc-movedbywipingwith clean,lint-freemate-nal moistened ith solvent. t is imoonanrto undershndhat flooding he woikpiece

to remove xcess urt-aceenetrant illalsodissolve he penetrant rom within theItaws,

Theprocessingaramete$or theuseofdeveloper re the sameas thosedescribedabove for the postemulsifiablemethod,Dry-powderdevelopers, owever,are no(recommeldedor us€ with the visiblesol-vent-removableenetrantmethod.

Portcl,ecnlngSome esiducwill rcmainon workprcces

afterpenetrantnspections compleGd.nmanycases,hisresidue asno delerenouseffects n subsequentrocessing r in ser-vice. There are. however, nstancesnwhich postcleanings required. Reslduescan result n theformation f voidsduriossubsequent eldingor unwanted topoff nbrazing, n thc contamination f surfaces(whichcan cause rouble n heat reating),or in unigyol3 1g saqtions n chemicarpro-

cessing pcrations.Drasticchemical r mechanicalmethods

areseldomequiredor postcleaning. henjustiliedby the volumeof u,ork. an emur-sioncleaningine is effectiveand rcason-able ncost. n special ircumstances,llra-sonic leaningmaybe he only satisfactoryway of cleaningdeep crevicesor smallholes. However, solventsor detersent-aidedsteamor water s almosialwavisuf-f icienl, he useof steam ithdetereenrsprobablyhe mosteffective f all me-thods_It hasa scrubbing ction hat removesde-velopers, he heat and detergent.emovep€netrants, t leav€s a workpiece hotenougho promote apid,evendrying,and

il rsharmlesso ncarlyall materials.Vapordegreasings very effective or removingpenetrants.ut t is practicallyworthlessorremoving evelopers.t is fr€quentlyusedIn combrnatronilh steam leanins.f thiscombinations used, he steam leaningshouldalwaysbe done irst because aDordegreasingakes ndeveloperi lms,

Where onditions o not-warant

or Der-mit permanentleaoingnstallations,an dwipingwith solventss effective,Driedde-veloperilms canbebrushcd fr, and esid-ual penetrantsan be rinsedoff by solventspraying r wipedoff with a solvent-damD-enedcloth,

Qrollry Arrorlnce ofPoretrc|rl lnrpectlolrfleierlolr

It is important to provide the conrrolsnecessary o ensure that the Denelrant ma_terials and equipment are operating at anacceptable evel of performance. The fre-quency of the required checks should bebased on a faci l i ty operaring or a fu l l ,one-shifl oreration daily. ln general. iI isSooopracttce o check the overal l systemperlonnance on a daily basis. This check

Fig, 2 | r*"i"e f|ow diosrom or rhaword-wqshobtciquidFeironr ,rrren

Eig. 22 Procesing llo* didgrdm for rhe rot*nr-remoyobt. liqurd pemtronr rysrcm



shouldbe pcrforme.d y pr(rcessing knowndefect tandardhroughhe ine,usiogappr+pnateprocessingarimcters ndcomparingthe indicationshus obtained o thoseot .taioedwith fresh,uDused enetrantn.dterialsample\. henthcperformencef the n-urematerialsallsbelow hatofthe unusedmate-

rials, he in-uscmaterialqualityshouldbechecked with the appropriate ests (as de-scribedbelow)and corrected rior to con-ductingany furtherpenetrantnspection.

Key qualityassuranceests o be period-ically conducted on in-use penetrants.€mulsifiers,and developersare listed inTable 2. Also listed are the intervals atwhich the light sourcesand the overallsystem erformadcehouldbe checked.

Military Standard 866specifieshe spe-cific testprocedureo use or the lestsde-fined n Table2-Penetrantspplied y sp|ayapplicationrom sealed ontainers re notlikely to be exposed o th€ same workingenvironmentswith op€ndip tanksandare

therefore ot equiredo be ested sdefinedinTable2 unless ontaminationssuspected.

mt|hlerlncc ol fllterlnlJ

With constantopen-bnkuse, penctrantmatedals re nherently ubject o potentialdeterio.ation.Such actorsas evaporationloss€s and contarnirralionrom variousso[rcescancontributeo deterioration.t isessential,herefore,o monitorthe onditionof thesematerials sdescribedn Table2.

Theevqporotionof the volatileconstitu-entsof penetrantsan aller their chemisaland pedormance haracteristics,hus re-suiting d changesn inherentbrightness,

removability, nd sensitivity.Liquid pene-traot materialsqualified o MIL-I-25135D(and slbsequeDt evisions)have a flashpoint requiremqnt f a minimumof 95 C(200"F) (per PenskyMartens lash pointtest procedure), ssuringhe minimizationof evaporationoss€s.

The <ontqminotion of water-washablepenetrantwith water s the most requent$ourc€ fdilficulty. Whenpresent eyondcriticalpercentage,his contamination il lrender the penetrant ank useless,Forpostemulsifiableenetrants,watercontam-ination s notascriticala problem, ecausewater s usuallynotmisciblewith postemul-sifiablepenetraots nd will separateromthe penehant,which

can then be subse-quently emoved.Watercontaminationanbe minimized y implementingnd ollow-rlrgproperprocessingrocedurcs.

It is important o recognize hat acidcontaminationca[yover fromprecleaning)will render luorescentDenetrantsneffec-tive. Acid contamination haneeshe con-sistencyof the penetrant ndlamagesordestroys he fluorescent ye.

Dusl. dirl and lint. and simild. oreignmaterials et nto the penetrantn the ordi-narycourseof shopurage.These olttami-

Toble 2 Intervols ot whichsol.rtionr, fight sou"6e5, and syttemperformcnce should be checked

bnshtness . . . . . Quanedy

Liquid Penetrcnt Inspection / 85

Conlaminationof the emulsifer mustalso be considered.Method B, lipophilicemulsifiersnherentlybecomecontaminat-ed by penetranthrough the normalpro-cessing fparts coatedwithpenetFntbeingdipped nto the emulsifier. t is imperative,therefore,hat he ipophilicemulsifier ave

a high olerancethat s, l07o) or penetraltcontamination.Watercontamination f th€lipophilicemulsifier s alwaysa potentialproblemdue to the natureof the process.Generally, %watercootaminationanbetolerated.

Method D, hydrophilic emulsifiersarcnot normally subject to appreciableamounts f penelran(ontaminalion,ain-ly because f the prerinseprocessingtep,whichremovesmost of the excess urfacepenetrdntbefo.e emulsificatioo.Becausehydrophilic emulsifiersare water based,water contaminations not a problem,ex-ccpt or the act hat hebathconcenratidnmustbemaintainedt theprescribedimits.

In general,emulsifiers hat becomese-verelycontaminated ill notproperlyemul-sify the surfacepenetrantor the parrs.Periodicmonitorings ess€ntial.

Developermust also be maintaiq9 toensure roperperformance. ontamifiitionof the dry.powderdeveloperwith water ormoisturen theair caoresult n caking.Drydevelopersmust rcmain fluffy and freeflowing f they are to performproperly. naddition,contaminationrom the fluores-centpenetmntmugtnot occur.Fluorescentspecksn the developerpowdercould bemisinterpreiedsan indication.Wet devel-oper(soluble r suspendible) us(not be-come coDtaminated ith penetrantor any

contaminanthat could affect ts ability towetand evenlycover he workpicce.

lrerlnlng errrdCertlllcotionol Pertonn€l

The apparent implicityof th€ peoetrantmethods deceptive. ery slightvariationsin performinghepenetrant rocess nd heinspection an nvalidatehe inspection e-sultsby failing o indicateall flaws. There-fore, many companies equire that pene-trant inspectianbe conducted only bytiained and certifiedpersonnel.Minimumrequirementsor personnelrainingandcer-tificationare described y variousmilitary

and industry specificatiors suchas MIL-STD-410 nd ASNT SNT-TC-lA). Thefol-lowingareexamples fthe mostcommonlyfollowed rainingprograms;however,spe'ciflc cusiomer training requirementsareusuallydefinedwithin the contract,

lroining is mioimal or level I penetrantinspection p€ratorspersonnelesponsiblefor theprocessing).owever, he penetrantprocessmust be correctly performed oensuleaccumtelsp€ction. Op€rator rain-ing consists f the satisfactory ompletionof a periodof on+he-job rainifl9,as deter-

lr.qhn.t R.quifrn.nt

Removabilily{methodA wal€rw r s h o n l y ] . . . . . . . . M o n l h l y

w.ter €onrent(nelhod A water

o n l y ) . .. . . . . . . . M o n t h l yContaminat ion.. . . . .W€ekly

EmulsifiersRemovabiiity ... . -. W€ekly

(merliodB,l ipophi l ic). . . . . . . Mo.thly

(methodD,l,ydroFbilic)..,, .. weekly

Conlamin on , . . . . Weekly

Develop€rsD.y-dev.lop€rorm-.Daily

Contaminarion.. . . . .Dai ly

Not l€ss han907.

E4ual o

Equal o

Eqml lo

3%abovennial

Musrbe luJly,

102mm (4 ..)

speciiiedMinimum mo

tnm lJ in.)Minimum ?m x

{200 lc)

Acu.ous (solubleand

develoDer

Wctlid r'coverage. . , - Daily

ContaDiDation . -.. .. Daily

Concenllarion. . . . . . . Wcekly

syslcm perfomance . . . Daily

nantsdo no particularharmunlesspresent othe extent that the bath is scummy withfloating or suspended foreign material. Rea-sonable care should be taken to keep thepenetrdntclean. Workpieces containingad-hering sand and di.t from the shop floorshould be cleaned before bcing dipp€d intothe penetrant.



t6 / methods of Nondestruclive Evoluotion

Tqble 3 Common types, locqtions, qnd choracteristics of flowg ordiscontinuit ies reveqled by l iquid penetrqnt inspection

of flaws that can be found by penetrantinspection, together with their likely loca-tions and their characteristics.

Intpe<lion Toolt, Ao inspectormust havetools that are capable of providing thr re-quired

accuracy.These tools usual lv in-clude suitable measuringdevices, a flash-light. small quantities of solvent, smallquantitiesofdry developersor aerosolcansofnoDaqueouswet developers,pocket mag-nifieE ranging rom 3 to l0 x, and a suitableblack light for fluorescent penetrants orsuflicient white light for visible penetranrs.Photographicstandardsor workpieces thathave specific known flaws ar€ somelimesused as inspectionaids.

A typi(ol in.pe<rion beginswith an over-all examination o determine hat the work-piecehasbeen properly processetland is insatisfactory condition for inspection- In-spection should not begin until the wetdevelopers

are completelydry. IfdeveloperIilms are too thick, if penetraot bleedoutappearsexccssive,or if the penetrantback-ground s excessive.he workDiece houldbe cleanedand reproccssed-hcn rhe in-spector is satisfied that the workDiecc rsinspectable, t is examinedaccording to aspecifiedplan to be suaeno arcasbave beenmissed. An experienced nspector canreadi ly deternjne which indications ar ewithin acceptableimitsand which onesar cnot. The inspcctor then measuresall otnerindicat ions.f thc lengthor diameterof an

indication exceedsallowable limits, it mustbe evalualed.One of the most common andaccuraleways ofmeasuring indications s tolay a flat gageof the maximum acceptabiedimensionof discontinuity over the indica-tion. If the indication is not coopletelycovered by the gaBe, t is not acceptable,

Evoluol ion. Each indication that is no tacceptableshould be evaluated, It may ac-tually be unacceptable, it may be worsethan it appears, t may be false, it may bereal, but nonrelevant,or it may actually beacceptable upon closer examination. Onecommon method of evaluation includes thefollowjngsteps:

. Wipe the area of the indication wirh asmall brush or clean cloth that is damp-ened with a solvent

. Dust the area with a dry d€veloper orspray it with a light coat of nonaqueousdeveloper

. Remeasureunder lighting appropriateforthe type of penetrant used

If the discontinuitv originally appeared tobe of excessive ength becauseof bleedingof penetrant along a scratch, creyice, ormachining mark, this witl be evident to atrained eye. Fioally, to gain maximum as-surance hat the indication is properly inter-preted, it is good practice to wipe the sur-face again with solvent-dampenedcottonaod examine the indication area with amagnifyinggla,:sand ample white lighr- Thisfinal evaluation may show that the indica-tion is even arger than originally measured,but was not shown in its entirety becausethe ends were too tight to hold enoughpenetrant to reach the surface and become

visib le.Dirporition of Unocceptoble Work.pie<er. A travel ticket wi[[ ubually accam-pany each workpiece or lot of workpieces.Provision should be made on this ticket toindicate the future handling ofunacceptablemarerial. rhat is, scrapping, rework, repair,or review board action. There is oftcn roomon such tickets for a brief descriDtionof theindicatiqn, More often, indicationsare iden-tilied directly on the workpiece by circlingthem with some type of marking that isharmless to the material and not easilyremoved by accident, but removable whendesired.

Rewoil<ing an unacceptable law is often

allowable to some specified limit; iodica-tions can be removed by sanding,grinding,chipping.or machining.R€pair weldrng ssometimes needed: n this ca e. the iddica-tion should be removed as in reworkinebeforc t is repairwelded, or weldingma ymove the flaw to a new location. In addi-tion, it is imperative that all entrappedpcn,et.ant be removed prior to r€pair welding,because entrapped penetrant is likely toinitiate a new flaw. Verification that theindication and the entrappcd penetranthavebeen removed is required.

ShnnkaAeracks... . . . . . - . , . . . . Casr ingsal lmetals)---ont,r l urfaccsH o r e a r s. . . . . . . - . . . - . . . . . . _ . . C a s l i n g sa t t m e r a h l - a tn s i d e

C o l d h o t s. . . . . . . . . . . . . . . . . _ . . C i s t i n s sa l l m e t a t s F a rh a n s e snc.ossscction

Foldr. . . Casr ing\al lmerr l . t anywhcrel n c l u s i o n s . . . . . . . . . . c c s r i n s s .o r e r n g . . . h e e r .

brr-anywhereMicroshrinkageores .. . , . . . - . Cast ings+nywh€.ek P s . . . . . . - - . . . . . - . - . - . . . .F o r g i n g s ,a r a n y w h e r eForSinS racts. . .. .. . . - .. . _. . . Fo.sines{r inside r ourside omcrs

andat charge3n fioss s€ctiotr

l p . . : . . . . . . . . . . . . . F o r c i n s \ .a r -n e a , . o m e r r ce n r e rL2mrna0ons.. . . . . Sheer---srdgesc e n t e r e a d r a ( k \ . . . . . . . . . . . . . . w e t d s + rc e n r e rf r e , n f o r c e m c n rCracks n hed-affectedooe .. .. - W€lds+r edSe { tiDtorcemenlCEler cracks . . - . . . . . . . . . . . Welds----atnd of headporol i ry. . . . . . .. . . . - . . . . . . . cnsr ings. eldsGrindins acks. . . . . . . . . . . _ . . . Any ha.dnerat-ground udacesQuenchracrs.. ., . . . . . . . .. .. . H€;t rcaled reelSl.ess-conosionmcks.. . , . . AnymetalFal iSuefacks.. . . . . . . . . . .. . . Any nreial

NoDElevrra ndi€tions(s)Weld parirr . . . - . . . . . . . . . . . . A.c weldsIncomplete en€t.arion. .. .. . .. . Pilter eldsSu.facexpulsion. . . . . . . . . . . . Res;stancectdsS.ulTmarks . , . . . . . . . . . . . . . . Seam €tdsPrcss-f i lnt€rface.. . . . . . . - -- . . . Pressf i rsBra2€unotr.. . . . . . . . . . _ . . . . . Braied arlsBuns . . . . . _ . . . . . _ . . . . . . _ _ Machin€d a.sNicks, ents, cratches,. . . . . . . Al t rarts

Tishl, shallow

Ti8ht, shallowTi8hi. shallow, intermirent

Sponsy

Tight or open

Tiehl or openTiShr or op€n

Sph$icalTi8ht. shallow, randomTisht to ope\, oxidizedTighl lo oF€ni may show conosionTighl

Orr.D, flrll weld lenstlRaised metal at weld edSeSurfee of s€am welds

Edse of cxcessbmzeBleedsheavilyVisibl€ r{iihout per.trant aids

(.1 Th.* @y b. prchibit d tlavi, bur ar€ usMllr iosiddcd no.i€t.rant in p€ichnt t.siins.

mined by immediate suEErvision.conduct-ed undgr the Suidanccof a certified level Irnspector.

Training for level ll inspectors(personnelresponsible for the inspection and evalua-tion) is more extensive than that

for rnelevel I operatorr.Trainingusuallyconsisrsof 40 h of formal faining, followed byseveral \rreeksof on-lhe-job lraining underthe supervision fa designatedrainer,usu-ally a cenified level II oterator.

Certificolion. Personnel of sufficientbackgroundand training in the princip le5ano procedures l penetrant nsnection rcusually certified by the successiul comple-(ion of a practical Iest, \rhrch demonstrate5their prcficiency in penetrant techniqucs,and a written test, which documcnts thcirknowledgeof pcnetrant nspect ion-Cerl i -l ied personnel realro normally cquired opass a periodic eye examination, whichincludes a color-vision test. Certificationcan be obtainedon-site hrougha cert if iedlevel l l l inspector who may be with anoutside sourcccontncted to certify person-nel or a company empioyee who has beencertified as a level III inspector by thcappropnate agency.

h3pe.tlon and Ev.rluoflonAfter the penetrantprocess s completed,

rnspection nd cvaluat ionof the workFiecebegin.Table I lists the more common types



ASTM-E-165.. . . . . . . . . . . . . . . . . - . . . , . . . . . . Standardracr iceor Liouid-PenetBntnsDect ionethodASTM-E 70 .. . - . . . . Standardef inrt ion\fTems Relat 'neo Liqud-Penetrmr

.{STM-E-I?06 . . ... .. Sle&rd Metbod or Fluore:|cenljquid-Pen€trantxaminationUlinC h€ Lipophilit PostEnulsificalionPrff.ss

ASTM-E-1209 . -. .. ., Stadard Method or Fluorescenl-Pen€trantxaminalion sinsthc WaleFw8fi a6le P.Gess

ASTM'E-1210 . . - . .. . StandardMetbod or Fluorcscent-PenelrantEminationU$inerhe Hydroph'licPosrEmuhificdtion roces\

ASTM-E-1219 .. - . -. SlandardMerhod or Fluo.csc€nGPenet.antxahinationUsirslbc SolvcncReft vablcPrm€ss

ASTM-E-I?20 . .. .... SlandanlMethod b. Visible,P€n€Iran xaDjrrljon Usirs rbeSolvenrRemovablerocess

ASTM-E-I 3J . .. .. . . Srandard estM€thod o. Comparingh€ Brighth€ls fFluoresc€nl €netrants

ASTM-D-2512 . . . . - . Compalibiliiy f MalerialswithLiquidOJ(ygenllJnpactSensitivityireshold Techdique)

T.st for AMSSAE spelficqtions

l.tble 4 Prrttiol listing of siondqrdt cnd lpccificotions for liquidp€netrarnl inspeation

Tnk d .rpLdlld ol Ctnded d ip..iadrlon

. ... - Flooresc.nt eoetmattrsp€ction-AircEfl ard EnsiftComDoncnt aintenaoc€

ASME rpd'llcllid|s

U,S.hilit rr sd gowmhedl speclftitiort

M I L - S T D { E 6 6 . . . . - . - . - . . . . . , . . . . . ., . . . . . . . . . M i l i t a r y S t a n d a r d I n s p e ct i o n , L i q u i d P e n e t a n tMIL-STD-4|0.. . , . . . . . . . . . , . . . . , . . . . - . . . . . . . Nondestruct ivc€sr ing crsonnelsal i f icaaions

M I L - 1 4 1 3 5 . . . . . . . . . - . - . . . . , . . . . . . . . . . . . , . . . l n s D € c t i o n M a t e r i a l s . P e n e l r a n tM I L - I - 2 5 1 0 5 . . . . , , . . . . . - . . . . . . . , . . . . . - , . . . . , tn s i , e c l i o n U n r r , n u o r e s c e n t P€ n e i r a n t , T y p e M A - 2MILI-2510,6..,. . . . . . . . . . . . - . , . .. - , . . . . . . . , . InsFct ion ni t ,Fluorescentcnetmrt, yt 'cMA-3MILSTD-?7I (Shipst. . . . . , . . . . . . . . . . . . . . . . .- . Nondcs.dclive Tcstios Re4uiremcDtso. lr.lal

Fis. 2s ffffiJ#Lii*.:,ii:il (il""ffi:iTfl:.f# *lif,,f;#H,wJl)wdtd-woiioh.iquid

Becauseeworking s usually equired, tis goodp.actice o finish t olf with moder-ately fine sauding, ollowed by chemicaletching o remove meared etal.All traces

ofthe etching luid should be rinsed off, andthe area should be thoroughly d ed beforercprmessingfor reinspection.Reprocessingcan be the samc as original processing or

Liquid Penetrant lnspeclion I 87

penetrantnspection, r canbe done ocallyby applying hematerialswith smallbrush-esor swabs.

Folseond Nonrelevoni nditqtions. Be-aausepenetmnt nspectionprovidesonlyindirect ndicationsor flaws, it caonoral-waysbe determined a irst glanc€whether

an indication s real, alse,or nonrelevant,A real indication s causedby an undesir-able law,suchasa crack.A false ndicalionis an accumulation f penetra.tt ot causedby adiscontinuityn theworkpiece, uchasa drop of penetranteft on the workpieceinadvertently. nonrelevantndicationsan eotrapmentof penetraotcausedby afeature hat is acceptable ven though tmay exceedallowable ndication engths,suchasa press-fitnterface,

Speclflcctlonrttnd Standerdt

It hasnot beenpracticalo establish ny

typ€ of universalstandardization, ecauseof the wide variety of componentsaIIdassemblies ubjected o penetrant nspec-tion, the differencesn the types of discon-tinuities common o them, and the ditrer-ences n the degreeof integrity required.Generally, ualitystandardsor the typ€s fdiscoltinuities detectedby penetrant n-spection reestablished y oneor rhoreofthefollowingmethods:

. Adoption of standards hat have beensuccessfullysed or simjlarworkpieces

. Evaluation of the results of penetrantinspection y destructive xamination

. Experimental nd heoretical tress nal-

ysrs

Spocifcqtioni, Normally, a specificationis a document hat delineatesdesignorperformanceequirements. spesificationshould nclude he m€thodsof inspectionand he requirementsasedon the inspec-tion or test procedurc.With p€fletmnan-spection, his becomes imcult. Too oftenthe wording n qualityspeciticationss am-biguousand meaningless,uch as "work-pieces shall be free from detrimeDtaldefects" or "workpieceshavingquestion-able ndicationc hallbe held or reviewbythe properauthorities,

Specification$pplicable o penetrantn-

spectionare genenlly divided into twobroadcategories:hose nvolvingmaterialsandequipment, nd hose oncemingmeth-ods and standards.Therc a.e, however,several tandardsndsp€cificationshatarein commonuse;someof theseare isted nTable 4, Because he equipmentused orpenetrantnspection overssuch a broadscope, hat is, raogingrom smalldiptaflksetups to large au(omated nstallattons,most emphasisn standards nd specifica-tionshasbeenplaced n the materials $edin this nspection rocess-



88 / Methods of Nondeslructive lvalustion

Control SFtems. In conjunction with the

sD€cifications listed in Table 4, several

methods and several types of standardsare

used to check the effectiveness of liquidpenetrants. Ooe oi the oldest and most

frequently used methods involves chroml-

um-cracked panels, which are available in

sets containing fine, medium, and coarsecracks. Many other types of inspection

standards have been produced--often for

sp€cilic indicalions needed for a unique

ferent sensitivity hat werechromium-cracked

e applied o acontaining ine

aoplication. A comparisonof indicat ions

f;om two water-washablepenetrantsof dif-

rromium-crackedalel containing ineacks

rsshown n Fi8, 23.

A.aepfqnceqnd reiection tqndotds for

principalactorbeing hedegree f inlegrityreouired.Al onc extreme. or certalnnon-criiical items, the standardmay permitsome specific ypes of discontinuities llover the workpieceor in specifiedareas.Inspections often appliedonly on a sam-pling basis for noncritical items. At the

oppositeextreme, tems are subjected o100%nspection, nd equirements re ex-iremelystringento thepointofdefining helimitations n eachsoecific rea.

cracks-rs

shown n

liquidpenetrantnspection re usuallyes-

tablishedor cach ndividual temor groupof itemsby the designer.n most cases,acceptanceand rejection standardsarebased n experience ith similar tems, he

Liquid Penetrant (Lev1el-I-level - II''

Documents

Transcript of Liquid Penetrant (Lev1el-I-level - II''