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UNIQUE TECHNOCR.ATS
SCHOOLOF NON.DESTRUCTIVE TESTING & WELDING

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TESTING LISUID PENETRANT

LEVEL.I/LEVEL-tr

S.H.DESHPANDE
ASNTLE\IEL_M

REGD, OFFICE: UMQUEIECHNOCRATS NO.9153, NO.47,P.O.BO)C ROADSIINKT{DAKATTE MACIADI MNGALORE-56009I PILNO.- 0t0 - 3489140 ,?1td6.59. FAX: 080- 34853?4'

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o _=/a!l_ o ONIOOE o o Liquid Penetrant lnspection is a non{estructivo method of revealing materials. of solidandnon-porous discontinuities thatareopento thesurfaces o Liquid PenetrantInspectiondepends mainly on the penetrantefectively a to form a overthe surface FLOWING of the test objec{, WEfnNG the surface to the that open are o rapidly intocavities SEEPING uniform coating, continuously to forman indication. getting BLOTTED OUTof thecavity surface andefiiciently a
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procoss can be as of the LiquidPenetrant lnspction A simplistic description follours: to forma PENETMNT) ls applied to the testsurface A tiquid, usually Red(called penetrant io provided for the surface. Adequate time is uniform layeroverthe (CLEANER) of cleaning A suitable method opento thesurface. seepintocavities penetrant the surface.Thenthe dye left the on excess is usedto remove onty on a to come is made out& forman indication intodiscontinuities thathasseeped of th indications The evaluation contrasting background. [calledDEVELOPER] lotof useful information about thetestsurface. so obtained canreveal to a wide and its applicability of the test is its simplicity The mainadvantage variety of situations. to only those defectsopen the of the testis its applicability Themainlimitation surface. EVOLUNON OFTHEPROCESS enteredthe was madeto flow on a iest surface,kerosene vv|renKerosene eitherflowedout or crevices open to the surfaceand the excessKerosene background provided a contrasting of wtrite wash application evaporated. The indication. The visual from the oponings made againstwhictr*re Kerosene with a by hitiingthe test surface couldbe increased, sensitivrty of the procees cracks of the onto out vibrations brought morekerosene hammer.Theresulting 'Oil method.lmprovements wascalled & \Mriting" thewhiteuiash.Thisprocss Inspection. development of Liquid Penetrant the of thismethod causgd

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PENETRANT TESNNG iIATERIALS Following arethecommon required for penetrant testing. materials 1. PENETRANTS/DYE 2. EMULSIFIER 3. SOLVENTCLEANER/REMOVER 4. DEVELOPER Depending on thedlaraeteristics of theabove materials choserr, a widevariety of penetrant testscanbe defined, wtrich aresuited for different setof circumstances. PENETRANTS Therearetno basictypesof penetrantspenetrants FLUORESCENT penetrants. VISIBLE penetrants A thirdcategory of penetrant called'DUAL SENSITIVITY" are also penetrants These available. are suitedfor use, both with visible& fluorescent methods. The aboveclassification is basedon how the oenetrant are seen indications during Inspection. Another classification of pnetrants can be madebasedon the method usedfor penetrant excess removal. Theyare WATER WASHABLE Penetrants POST EMULSIFIABLE LIPOPHILIC Penetrants POST HYDROPHILIC EMULSIFIABLE Penetrants SOLVENT REMOVABLE Penetrants psntrant penetrants greenin colour FLUORESCENT utilisss lhatareusually and (shine) fluoresce brillianfy under Ultraviolet light(black light). penehants The sensitivity of fluorescent on its ability depends to formindications that apparas smell sourcesof light in an othenrvise darkened area. The penetrant these sensitivity of methodsare easily alteredby the natureof fluorescing additives added to the penetrants. VISIBLEPFNETMNTutilisesa perietmnt that is usualtyred in colourand produces sharply visible redindications to thelightbackground in contrast of the
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altered areeasily light.Thesensitivity of thesepenetrants visible developer under of the dye. concentration & the nature by changing the dyre PEN ETRANT CHARECTERISTICS to makethem good thould have someciharacteristics All penetrant matrialE penetrants. * " * * * ' " * * " " ' * & unificrm consistency Chemical stability Goodv'iettability LorrViscosity brighhess Sufficient to containers & testmaterialg lnertness Chemical Sloirrdryingcharacteristics Easeof removal lndfensive Odour LowToxicity Resistance to UVlight& / or heat Low@st to possible contaminants Hightolerance point Highflash

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EMULSIFIERS penetrant andhence thatmake theexcess water\Nshable areliquids Emulsifiers products are extremely penetrant removal. These aid the processof excess penetrant parts. removal The surface useful whentesting of largeno. of intricate process ranuld less cr.rmbersome & complete. be made There aretvrotypes of emulsifiers
1. LIPOPH]LIC and 2. HYDROPHILIC

are essentially oil basedand work by diffusinginto LIPOPHILIC emulsifiers actionis fast penetrant it washable in water. The emulsification making excess the penetrant. Therefore, in with exc6$s as it is contac{ and continues as long is shouldbe quicklycompleted. The time for emulsification rinse operation rate,test emulsification its concentration, emulsifier, on the particular dependent piecesurface etc, andhencacannotbe a fixedvalue. condition TIME BY TO FIND EMUL$IFICATION IT IS, ALWAYS PREFERABLE EXPERIMENTATION, by water andgetcontaminated are usedas supplied LIPOPHILIC EMULSIFIERS & pefietrart 3 of 21 Page

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HYDROPHILIC EMULSIFIERS are essentially andaresupplied as waterbased concentrates. Theeeare dilutedin waterbeforeuse. 530016 concentration is usedbr dip applications 0.0$'5%concentration used for spray applications. is Hydrophilic emulsifiers ac{by detergent action i.e.,by displacement of pnetrant. Hydrophilic emulsifierc are slowactirrg& hence,norfrallyadequate emulsification pre+insing time iE available.Normally, with coar$ewateris done to reduce 'emulsification timeandpenehant contamination'. Penetrant manufacturers normally times specify emulsification for specific nominal types of emulsifiers andtheconcnfation in wttich theyaresupposed to be used, the emulsification Houpver,it uould be still advisable to determine time by experimentation as emulsifiercontamination can alter the emulsificatior, characteristics. SOLVENT CLEANER / REMOVERS penetrants, excess bur Solvent cleaners are chemicalg thatare usedto remove gurface penetrant action. Excess theyact by Direc* solvent is cjissolved by the free solventdeanerwhen appliedusing slightlymoistened lint cloth I cotton waste. Flooding the risk of the surfacewith excessive cleanerincreases penetrant from within the defectsalso getting dissolved. This will make indications disappear. Solvents areclassified into2 types
FLAM[,IABLE NON- FIAMI\,IABLE

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FREEOFHALOGENS HALOGEN CONTAINING

Halogenated but are not solvents havethe advantage of beingnon-flammable, presence would be harmful to in certain wfisre of halogens accepted applications the materials of testobject. DEVELOPERS The pwposeof the developer is to increase the visiblecontrastof visible penetrant indications the in normalvisiblepenetrant tostingand to increase penetrant brighhess in fluorescsnt testing. of fluoreseent indications process. A good developer Developer is is a oitical part of the inspec{ion requir6d suchas, to havemany characteristics, " it mustbecapable sf providing a contrast background penetrant in colourcontrast testing.
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it mustnot pmduce its ovwr fluorescence to theoperator.

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penetrant ftoma defect. it musthavea goodblotting action. it mustbe easyto rmove afler inspedion

all ihese characteristics Generally, are presentis varyingdegreesin various developers. Hence,lt is possibleto get differentsensitivity using different developers. There are4 tlrpes of developers cgmmercially available. 1. 2. 3. 4. 1. DryPouder Water Soluble suspendible Water Non-aqueoussolventsuspendible DRYPOWDER penetrant These aremorewidely usedin fluorescent testing.Theyarenot generally penetrant good us6dwithvisible testing as theydo not produce colourcontrast. Dry developers ehoutdbe light & tlnffy and non-hygroscopic for good usage.Theyshould clingto thesurface of thetestobject as a thinuniform coating.They are normally driedby heating to removerroisture. This restores theirability to dustuniformly clumping andavoids / iumping. Handling of drypouders is to be donewithcaras it cancausedryskin& problems.Prolonged respiration exposure to dry powder application may require useof glove, respirators & particle filtration equipment. Dry povlders can be applied by dipping, clouding the.surface in a dusty atmosphere or by fog chambers.

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WATERSOLUELEDEVELOPER exceptwater can be used with all types of penetrants These developers washable penetrants, Slight excess developer applicationcan cause defect penetrantto be washed away in the case of water washable

ponerants.

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\ /hich concentrate, Water-soluble developers are available as dry powder as a in water. On application, recrystallises the pov\der can be digsolved Kg/Lis the A12 - O.24 as the waterevapqrates. unibrmdeposit Usually, checked witha hydrometer. urhich n be conveniently bathconcentration, of ri/ater-soluble developers are Advantages i) ii) 1ii) Theydo not require any bathagitation. is not prior to developerapplioation Dryng of components necessary, and Postcleaning is veryeasyaswater washing is adequate.

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WATER DEVELOPERS SUSPENDIBLE penetrants. can be usedwithbothvisible & fluorescent Thesedevelopers as dry po'ader concentrate. Usualbathconcentrations Theyare supplied with a can be checked are 0.O4 0.fZ lQlL. Particleconcentration drying can be applied before hydrometer. Watersuspendible developers can application also DMrq of thecomponent afterdeveloper compsnents. help/ aidpenetrant bleedoutsfromdefects/crevices. conoslon inhibitors, dispersing agentsand weitingagentsare Normatly, performance. improve to their addedin developers
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- AQUEOUS SOLVENT, SUSPENDIBLE DEVELOPERS NON penetrants provide the best wheR Thesedevelgperc, usedwithfluorescent visible & are commonly used for both sensitivig. These develo'pers in a penehant prooess. They containparticles suspended fluorescant particles the volatile to of solvents with suitable dispersants keep mixlure liquids the highest sensitivity, as the volatile fromsettling.Theyproduce penetrant out of to enter & help bleed the crevices, dilute tend the penetrant itsvolume. by increasing

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SELECETK'N METHODS: OFPENETRANT penetrant Having it is nowimportant undorstood materials, to be able the various pnetrant to selectan appropriate testingmethod for a givenapplication. weight to be teeted, required 1. Thesize,shape, dvork pieces, no.of pieces facilities, surface of the testpiecas sensitivity, available condition etc.,are penetrant allfadorcwtlicfiinffuence theseledion method. of a proper 2, Cost,sensitMty d$ired, naturoof dfects beingsoughtand oiticalityof testingalsoinfiuences the seleciion method. of a penetrant The fotlowing for penotrant methods, cfiart gives us variougoptionsavailable basedon various inputingredients. PENETRANT VISIBLE FLOURESCENT DEVELOPER DRYPOWDER HYDROPHILIC SOLUBLE HALOGENATED WATER SOLVENT WATERWASHABLE WATER HALOGEN-FREE SUSPENDIBLE SOLVENT POST-EMULSIFIABLE NON.AQEOUS
EMULSIFIER

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CLEANER

WATER

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SCLVENT SUSPENDIBLE SOLVENT REMOVABLE

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Various combinations of ponetant materials yields various penetrant test methods, on the combination and,depending chosen, sensitivity achievable may vary. Because and the possibility of of the difficulties in quantiffing sensitivity differentsensitiviti$within a partio.rlar it has been the practiceto combination, speclfy a test methodcomblnafon and insist on a written procodurefor performingth6 tcat yvhile it is notnece$aryto individually descfibe eombinations, it iray the various bs pertinent to leamfeurspecific advantages & limitations of different methods. 1. primarily are utilised Mshle pene$ants lnspection whereas br localised penefants fluorescer* lendthemselves / largescale easllyto mechanised inspeciion. Highestsensitivities are achievable in post - emulsifiable fluorescent penetrant (with ircpoction hydrophilic emulsifiers).
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3, Solvent removable fluorescent penetrant method is ideal for spot inepction orwhereu/ater csnnot be conveniently used.Whenadequate care ia taken,this methodis as snsitive as the post - emulsified fluqfscentpenetrant method. Water washablefluorescentpenetrantmethodsare the fastest. Over is the most ueshing cause in thismethod. frequent of lossof sensitivity visible penetrant Solventremovable methodsare most versatileand portable. This methodcan give good sensitivity when adequatecare is takenin penebent removal. Wateru/aEhable visiblepenetrant are fastest,but provideleast methods sengitivity. They are very usefulwfien shallow& wide defectsare not significant. penetrantmethodsoffer higher sensiiivities than visible Fluorescent pntrant methods.

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PENETRANT TESTING EQUIPMENT Theequipment usedin Penetrant Inspection fromsprays, aerosol cansto varies cornputer controlled oomplex automated, systemg.Houover,eventhe automated linesare basically material handling systerns for coneclhandling of components providing timesof penetrant application, duell time,penetrant drainout, accurato drying. excegs penotrantremoval,washing,drying, developerapplication, lnspedionetc. EQUIPMENT PC}RTABLE penetranl is caniedout in the field in betvrreen various Mosttrequently, inspection processing This helps stages to identify developed defec.ts dueto the processing. in etiminatiqrof these defscts bfore furthsr processing/sorting out defective fromfurtherprocassing. componeqts Portabiligis a very importrant criterionin field inspection. Various penetrant chemicals in spraycansor aerosol cansfor easyportability. E','en are available portable to be packedinto compact Ultraviolet lampsI blacklampsare designed kits.

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penetrantremoverand developer, all in spray cans with Pre-cleaner, Penetrant, paper peneirant kit. Blacklightis adequate lintfree doih / to\ryels for?n a standard an additionaltool for fluorescentpenetranttesting. PENETRANT INSPECTION STATIONARY consistsof a The type of equipmentmost frequentlyused in fixed installation series of modular tanks designedspecificallyfor a particularpurpose. The are variousstations 1. 2. 3. 4. 5. Gleaning station Penetrantstation Drain/ dwellstation station Emulsifier Pre& postwashstation

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6. 7.
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Drying station Developer station

Inspection stiaiion

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Usually,a drain / dvuellstation is positionednext to each dip tank to provide flexibility of time. CLEANING STATION Pre-cleaningof uork pieces prior to penetrant inspectionis very imporiant because conlaminants i) may preventlhe penetrantfrom enteringthe llaq properties ii) mayalterthe physical of a penetrant, or, iii) mayinterfere with properexcessperEtrantcleaning. Precleaningis nonnally achieved chemically, mechanically or by usingsolvents. cleaningincludesalkalineor acid deaning, pickling,chemicaletching, Chemical moltensalt bathcleaning etc. Mechanical cleaning includes tumbling, wet blasting, wire brushing, high pressure steamcleaning, highpressure watercleaning etc. Solvent cleaning methods includes vapor degreasing,Ultrasoniccleaning in solvents, solventspraying / wipingetc.

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method is thatthe in selection of the cJeaning factorto be considered Onemajor , defects without leaving allcn to remain opento thesurface method should processing.ln orderto achieve the residues, wtrichinterbrewith srbsequent to be may be required morethan one of the abovemethods aboveobjective, usedfor pre-cleaning. methodschangevery widely,design of the pre-cleaning Sincepre-cleaning station mayalsovaryverywidely. PENETRANT STANON stiation is to providea coatingof of a penetrant The principal requirement to avoid penetrant whennot required] and havefacilityto coverthe penetrantl penetrant Drain drain out. to the excess evaporation & contamination and collect periodic provided for cleaning. plugsare normally to help drainthe contents spraying usingair by dipping, of the perntrantmay be accomplished Coating 'expendable" guns or usingelectrostatic technique is also spray guns. An frequently employed where no effort is made to collectthe drain out when permil. economies of operation steel, but may are made using galvanized Normallypenetrant containers gteel, whenwaterbasepenetrants especially somelimes be made usingstainless arestored. EUULSIFIER STATION e,omponents to help tanks are used for dippingpenetrant-coated Emulsifier pgnetrcmt (asin the caseof lipophilic emulsifiers) or spray remove excess surface stationswith coarse spray to removeexcess penetrant(as in hydrophilic by experimentation for emulsifiers). timesare normally established Emulsitication eachnatureof components. PRE& POST RINSING STATIONS precedes Pre-rinsing normally hydrophilic emulsification and is accomplished by since coarse watersprayusinghandheldsprayguns. The water& penetrant, tanks,reclaiming theydo not mix,can be allotr,rd to separate out in settling the penetrnt. by Post rinsingnormally succeeds and is accomplished emulsifier application guns. Washtrough scrubbing with coarsewatersprayusinghandhelp spray splash should be suitable to turnthe component to cleanall surfaces.Normally,
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shieldspreventthe conlamination of neighboring penetrant, emulsifier / developer tanks. Rinsestations are also eguipped one Wth set of Ultraviolet lightso that the progressof removalof fluorescentpenetrantcan be assessed. Since lot of lvaterwill be in contactwith the tank material,stainlesssteel is the prefened tank material,from conosion resistancepoint of view. DRYING STATION Re-cifculating hot air dryers are the most popular for drying of components. Electricelements, steamand hot gas are the variousheat sources. Eitherbatch type or conveyor type dryerscouldbe designed to suitthe component to be dried. DEVELOPER STANON Develqperstation is locatedafter lhe drier station wtren dry developersare useo. \t1/|en dipping is used, the excoss po,rder is shakon off before ailowing development.\A/tren large test articlesare to be locallydeveloped,a scoop is used for throwingthe pouder over the surfaces. Dry developerscan also be appliedin fog chambers or usingelectrostatic splay guns. Suitabledust control& ventilation anangements have to be made to see that no respiratjondifficulties ariss. When wet developers are used, the developer station should be located immediately beforethe drier. Therewill be a provisionto store the components after dippingin developerto allow drain bacJ< of developer. In case of water suspendible developers,it is ncessaryto stir the developer eitirerusing paddlesor pumpsto keep the developerparticlesfrom setfling. In cageof water-soluble developers, no suchseparate arangementis required. INSPECTION STATION It is a !rcrk tablewlreretest piecescan be thoroughly inspected underaF,propriate lightirg after developing. In case of visible penetrantinspection,it has to be illuminated with white light of adequate intensig, and in case of fluorescent penetrant test, it has to be illuminated with blacklight and provided with a hoodto blockwhite lightftom inspecdion area. Good air-circulation has to be providedin thisareato lirnitdiscomftture due to heat. The abovedesoiption describesthe variouszuFunits of a mechanised svstem and the specific systemwill consistof variouscombination of the aboveto suit the pafticular processrequirements. Page 1 1o f 2 1

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o oNtooE PROCESSING VARIABLES FORTESTING o o penetrant Having discussed the various possible variables, combinations & the eguipment to cany out the test, it is irnportant required to learnsomeof the a procssing impoilant variables, wfrich affedtest& testresults. o SOLVENT REMOVABLE iIETHOD o 1. A typical of processing sequence is givenbelow o
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Penstrant pouring, can be appliedby brushing, Bwabbing, dipping or by spraying All methods are acceptable. It is goodpradiceto allortr the penetrant to drainafterthe entiresurfaceis covered withpenetrant ratherthankeepit dipped. priorto penetrant Heatirgcomponents testing is not recommended dueto possible volatiliaation. Ihrell timedepends on the viecosity& surface tension of the penetrant & its contad angle with the inspe<iionsurftace. The longest dvr,elltime acceptable is the time it takes for the penetrantto dry on the surface. lf the penetrant u,ereto dry, pretrarilshouldbe ra.applied boforefurther processing. Optimumdlvell times have to bo establishedfor each penetrant. Formostp.rposes, 10mins. To 30 mins. would be optimum.

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6.

in thepenetrant as it will dissolve neverbe usedin excess should Solvent the to apply disappear. lt is necessary the defeclsmakingindications the solvent. with moistened material ftee tint a clean, using solvent with visible penetrant are not recommended developers Dry porarder low of Eensitivity" dueto reasons combination removable soivenl

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ItIETHOD WASHABLE WATER 1. is givenbelow of processing Atypicalsequence

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is a very low censitivity methodwith visiblepenelrants Wder washable method. Water washablemethodwith fluorescentpenetrantis quite popular. as for dtlElltimearethesame of penetrant in determination considerations method. removal solvent

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a -va!l(|1{to(IE o 4. is the majorproblm in waterwashable method. Optimum Overwashing o under conditions are bestestablished by observing the specimen rinsing blacklightuntilthefluorescent background is removed satisfactorily. o o 5. is normally donearound 30 psi pressure Rinsing of waterwhichis @ 10air is mixed with not 40" C. When waterfor spraying, air pressure should o 25 psi. exceed a aqueous developers are used,dryingis required 6. l/Vhen after developer is employed, application.tMren dry povrder / nonagueousdeveloper a
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be pior to devetoper dryingetrculd application. rinsing timesmaybe 1f2min.to 2 min. Nominal

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- EMULSIFIABLE ilETHOD POST 1. A typical sequence is irdicatedbelowfor both lipophilic & of processing emulsifi hydrophilic er application.

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in determination of penetsant d\ Ell timearethesameas for Considerations solvent removable method. penetrant remove of to partly to minimise contamination excess ' Pre-rinsing emulsifier is @mmon in emulsifier application. of emulsifier to afl surfacesto be inspectedis application $irnultaneous very important. brushingof while spraying& dippingare acceptable, emulsifier is banned. Thisis veryimportant especially uhen usinglipophilic emulsifier. Emulsification timeshould be determined by experimentation. Considerations explained for \^rater vrashable method' regarding 'developer cyde' applyto post-emulsifiable method application' & 'dryrng also. as Developing adequate, butshould be strictly timeof 10 mins.is normally specified in specifications, if any.

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INSPECTION 1. First step in the inspection tests is to ensurethat the of penetrant processing folloived & conditions in the procedure are adequately specified the resufts of processing are satisfactory. Availability of properlighting is a very important factorin the inspection stage. a) Sufficientwhite light should be presnt for visible penetrant inspedion.Lightintensity in specifications. is manytimesspecified Typical 500LUX/ 50 Footcandles. value for Sufficient darknesa & blacklight intensity shouldbe available FLOURESCENT PENETMNT INSPECNON. Typical values: 1@0-1500 Dw/cm2 btack light intensity at inspection $nface. 20 LUX(2 footcandles) max.for darkness.

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EVALUATION are indications underproperconditions \,8 seewhenwEinspedthe surface VWtat (except for badqground) . ln penetranttesting, the penstrant seen on the as canthenb termed INDICATIONS surface is theindication. inspciion INDICATIONS FALSE penetrant test. in fluorescent fltrorescen@ :1. Excessive background Examples / developer cause:Insuffcient cleaning Possible withPenetrant. contamination 2. Fingermarks hands. lt is very cause: Penetrant on operatofs Possible penetrant on inspection important to avoid contamination & adequate table, developer penetrant deaningto avoid FALSE ]NDICATIONS. INDICATIONS IRRELEVENT known by somefeature of designof the component Theyareindications caused to oxist. joints,scaleon rolledplatesurface. parts,boltedI riveted : Press-fit Examples forging. Roughsurface / on a casting ' RELEVENT INDICATIONS TRUE are TRUEINDICATIONS. lndications wtrichare not FHSE / NON-RELEVANT pre-specified a indications. TRUEINDICATIONS above sizeareRELEVANT INDICATIONS canb of tvrro t)/ps. RELEVANT ROUNDED INDICATIONS INDICATIONS LINEAR criteriafor Theseare normallydefinedin speciftcations.Also, the accepiance irdications relevant aregivenin SPECIFICATIONS.

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SIZE& is basedon |NOICATION / reiection to notethatacceptance It is important cycle reguiredto get of processing Une con'trol noi on Ff-qWSEE. Thereforb, cannotbe over-emphasized' interprtation conec;t POSTLEANING may be rquired to ascertainthat penetrant Post-cleaning After Ins9ec-tion, #t int"rf"r" wiih su6sequentprocessing. Most specifications ;;&;b-d" arEgivenin NDTprocedures' postctewrirrg requiramonts requirethat MATERIALS OF PENETRANT ASSURANGE QUAUTY that the regultsof the test are true to to ensure is Assttance Fu-tpo""of.OU"lity -trs teet method and have not deteriorateddr-reto faul$ th"'pot*ti"t of rawmaterials. of penetrant or deterioration irpfirent"tion of procedures & is controlledby rigoroustraining,qualification of procedures lmplementation of peisonnel employed,establishirg lwitten proceduresstating ""hin*tion re+rtification of personnel' vafiableito Oeusedandperiodic various of. cunent raw materialsare ctreckedby comparison of Penetrant Deterioration by a referencestandardin the p.tro*"n"" against awptable performance BLOCK of a REFERENCE iesting in are specifled of samples of comparison Varioustest blocksand mthods the mostpopularof wttichis the I specifications, standards [I ELOCK ALUMINIU CRACKED X WA THK SIZE 2" WDE X 1TLONG T ALUMIN]MUM MATL. 2024 SKETCH

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in waterprcduces to approx' 650: Fi19 queno\od Wlenheated Sucha block, width & depirr' This ig usefullor high cracr pattems;Ifiil" uncontrolled r proaucewider cracks' which are proceduree.Rt--had;;o-d0 seneitivity procedures' usefulfor loivsensitivity can materials ra\M / any tulo ponetrant of any tvo test methods The performance bYGompanson' be assessed COI'IPARISON VEFUFICATION, PROPERTY PHYSICAL the penetrartctremicalis verifiedby a $ome knom physicalproperty^of such testsare materials. o c[n-tril quality& penetrant procedure, standardisgd CONTENTTEST WATER MENISCUSTEST BLOCKTEST CERAII,IIC

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GRAVITYTEST SPECIFIC

TEsr FADE ir-uonescencE

TEST WASMBILITY WATER

Thesetestsaredescribedinstandards &be tec t r n i cout a|pubtications.Thesanr caried to JnJJri d! io||"rto utren trese testsare required OFRESULTS RECORDING

rqcgo permanent anv leave not does Ju9.ffo';,ilT,1t;"1,:ffi""tjJ; test This recordof indicati
iir*rL-r" lo have perman-ent / in - service inveitigations ,"v n r"fiyu drd or, i" t"iture requirements
etc. inspection ,1. PHOTOGRAPHY rcord' can createa permanent & WHITE, coLouR Photography BI-ASK of observation' iritantineous records Jn provioe pnotograPis Polaroid 2. DEVELOPERS FILITI PLASTIC Specia|@velopershavingp|asticconstitrerrtareavai|ab|e'wtricttfixthe can be peeledoff & storedwith lGse developers penstrflt inOications'identification. ProPer
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STRIPPABLE LACQUERS Threeto six layers of lacquer can be sprayed on the developed surfaces whose record is desired to be kept.Afterdrying, thesecanbe lifted direcfly or using transparent cellophane tapesto forma permanent record.

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TYPES OFDISCONTINUITIES In order to be ableto evaluate indications, it is necessary to havean ideaof the variousstagesof processing that a materialundergoes and the natureof discontinuities thatare relevant to thosematerials and the procssing involved. An inspector performing judgement thetestshould be ableto makea of the type of indications to expec{ whenlooking at thecomponent. DISCONTINUTIES canbe divided intothreebasiccategories. INHERENT PROCESSING SERVICE INHERENT discontinuities are those discontinuities present in the original produc{ion of metal / alloydueto thenature of production. Processing discontinuities are thusediscontinuities that are formeddue to the natureof procsssing matefals undergo- casting,uelding,forging,forming operations likebending, rolling & extrusion, machining, heattreatment, [latingetc. servicing discontinuities arediscontinuities thatareformed whenmaterials are in servica cDnosion, fatigue, erosion etc. DISCONTINUITIES ARENOTALWAYS DEFECTS, THEYBECOME DEFECTS ONLYI/V}IEN THEYARE IDENTIFIED AS RELEVANT & ARE KNOWN TO BE LARGER IN SIZETHANWHATIS CONSIDERED ACCEPTABLE FORGIVEN APPLICATION.

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OHIOOE
TRANING & CERTIHCANON ln order to help the industryin anivingat a uniformlevel of knoWedge & understanding of the test method, Americansocietyfor Nondestruclive testing hasbrought praclice outa documnt titledSNT-TC-1A wfiichis a recommended for Training & Certificstion. The ebovedo@ment is to bo usd as a GUIDELINE BY EMPLOYERS in establishing PROCEDURE & CERTIFICATION a Vi/RITTEN FORTRAINING OF N.D.T. PERSONNEL. ASNThasidentified of qualifications 3 levels - I LEVEL - II LEVEL LEVEL_ III . SPECIFIC; PRACTI'CALS GENERAL, SPECIFiC, PRACTICALS GENERAL, METFIOD, BASIC, SPECIFIC

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- | is the lo'nst LEVEL levelof qualification & is meant for personnel to perform per prccedures. testsandevaluate testsas written NODETAILED GENERALLY, KNOWLEDGE STANDARDS & SPECIFICATION AREEXPECTED. OF CODES, It is expecfed that fie personis trainedenoughto work with a pre-approved procodure provided to him. - ll is thelevelof qualification, - I , knowledge LEVEL wherein addition to LEVEL to set up & calibrate equipment,interpret & evalute test rosultsin accordance with codes,standards prepare & specifications, & reporttest w'itten procedures resultsis necsssary. - lll ie the highest LEVEL levelof qualification in eachmethod and requires an abilityto estrbtishteclrnique, selecl appropriate N.D,T,method,and train & qualifyNDTLevel- I & Level- ll personnel. in additionto Level- | / Level- ll knotflledge& tmdions, he should also have broad based back ground in processing Engirnering, & material Tecfrnology to be ableto assistin establishing acceptance criteria none existl. lwhers AS.N.T. presently condudsthe BASIC& METHODEXAMINATIONS in 12 DIFFERENT NDT methoG & leavesthe $PECIFICH(AMII{ATION to the - ll training, - I & LEVEL employer.LEVEL & certification etmination are left to - lll as detailed be contludedby LEVEL in theuritten procedure of the employer. Students arc a&ieedto studytho SNT-TC-1A dodment published by ASNT. Page20 of 21

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AS PERASMESEC.V STANDARDS LIQUIDPENETRANT

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1 ARTICLE 6 ARTICLE 24 . ART]CLE sE-165 sE-1209 sE- 1219 sE- 1220 sE- 129 sD-516 sD - e08 $D- 1s52

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GENEMLREQUIREMENTS EXAMINATION PENETRANT LIQUID TEST METHODFOR LIQUIDPENETRANT STANDARD EXAMINATION FOR LIQUIDPENETMNT TEST METHOD STANDARD EXAT\4INATION STANDARD TEST METHOD FOR FLUORESCENT PENETRANT EMMINATION USING THE WATER PROCESS. WASHABLE STANDARD TEST METHOD FOR FLUORESCENT USING THE SOLVENT PENETRANTEXAMINATION PROCESS. REMOVABLE TESTMETHODFORVISIBLEPENETMNT STANDARD USING THE SOLVENT REMOVABLE EXAMINATION PROCESS. STANDARDTEST METHOD FOR SULPHUR IN PRODUCTS PETROLEUM ION IN TEST METHODFOR SULPHATE STANDARD WATER. IN NEW& FORCHLORINE TESTMETHOD STANDARD PETROLEUM PRODUCTS. USED STANDARD TEST METHOD FOR SULPHUR IN PETROLEUM PRODUCTS (HIGH TEMPERATURE METHOD).

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so that they couldrefer the abovestandards to understard are advised Students during their careB. effciently thesstandards of theirunderstanding will enhance standards by otheragencies Studyof similar thesubjedandis recommended.

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Discontinuiry

Table6.1 VisualInspectionAcceptanceCriteria(see 6.9)

Statically Cyclically 'l'ubular Loadcd Loaded Nontubular NontubularConnections ConnectionsConnections AII Loads)

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(l) Crack ofsizc or localion. crackshallbe (2) $tld/Brsc-l\tctrl l'usi0n Pcld lnctal laycrs of$ eldnletalandbctwccD bctween adjaccnt Thorough shallexist firsion andbase mctal. (3) Crater CrossSection rveldsizc,exccpt for thc cndsof All cratenshatlbe filledto providcthespecified lcngth. of theireffectivc intcrmittent fillet weldr outsidc
(4) Wrlrl I'rolilo$ witl 5.24. Wcld prolilcsshallbc in conlbrnrnncc

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(5) Tlmeof lnspection $ clds aftcrthsconrllctcd bcgir inrrncdiatcll of wclds in all stccls nray Visual inspcction for ASfM A 514,A 5| 7, attd critcriir to ambicnt tcmpcrnturcAcccptancc havccoolcd pcrli)nlrud notlcss on visual inltpcction shall bc bascd and| 00 W stccls A ?09Cradc100 *eld. ofthe after thrn48 hours ((r) Undcrsizcd Wfltls -l txrntirtal wcldrniy bc lcss tlc spccilicd thrrn hcsizcofa fillctwcldin anyconlinuous (U): by thc fotlowingamounts size(L) withoutcorrection U. L, fromL. in Inrtnl allowable dccrclsc nomiualrvcld sizc. in. [mm] spccificd

< 3/r6 [s]

_ l/4 [6] > 5/16 [8]

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< l/l6[?] < l/32 [2.s] s l / 8l 3 l

lhc undcrsizc In all cascs. Dortionofthc t!cld shallod cxcccd l0')i' of thc $'cLl lcugth. On wcb-to-flangewclds on girdcrs, undcrmn shall bc prohibitcd at thc cnds for a lcngth cqual to twicc thc width of rhc

(7) Undcrcut l/32 in.Il mm], (A) l.'or shall notcxcccd lcss thanI in.[25mm] lhick.undcrcut mntcrial litr q1 l/l{r in. mrnl with tlrc fi,lk'winll cxccnrion: l2 UUsfggllEl]-lllgscd cqurllo or mml. liorrnatcri:rl lcngth accumulatcd 1p 2 in. [50mm] in ony l2 in. 1300

grcatcr than I in. thick, undc.cut shall not excced l/ I6 in. [2 mml for any lcngth of wcld. (B) tn primtry membcrs, undcrculshallbc no morc ihan 0.01 in. [0.25mml dccp whcn shall any dcsignkradingcondition tJndcrcul to tcnsilcstrcss un<Jcr thc wcld is transvcrsc l{)r nll olbcr c:rsus. tltrtr l/12 in. ll rrrrn bc no rrrorc

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(8) I'orosity slrcss tensile to thedircction of computed (A) CJPgroovc velds in buttjointstransverse wcldsandfor fillet *clds, the For all othcrgroove shallhaveno visiblepipingporosity, shallnot cxcccd in diamctcr sumofthe visiblepipingporosityl/32 in, I I mmJor greater 3/8in.[l0mmlinanylinearinchofweldandshallnotexcecd3/4in.[20mm]inanyl2in. ofweld. [300mfn]
(B) The frequencyofpiping porosity in fillct welds shall not cxcecd onc in cach 4 irr 3/32 in. [2 5 tnrtt]. Ll00 mffl of weld lengthand lhe maximumdiamctcrshallnot exceed Exceptiofl: for filler wclds connectingstiffenersto wcb, thc sum of thc diamctersof piping porosityshallnot exceed 3/8 in. [10 mm] in any lincar inch of weld and shallnoi

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cxcccd 3/4 in. [20 mml i$ any l 2 in. [3o0mml lengthof wcld(,l c(ttlpllludtcllsilcsttc\s k] thc d;rcctioll (C) CJI' groovcwcl(lsin buttj()intstransvcrsc of piping porosily l;or all othcrgroovcwclds,thc frcqucncy shallhavcno piping porosity. onc in 4 in. 100 mml of lcngthand the nlaximumdiamctcrshallno( shallnot exceed cxcccd3/32 in. [2.5 mm].
CcncrrlNolc: An ''X" indicates t y l c l a s h i d c d a r c ai D d i c . t c sn o n ' n P p l i c r b i l i t y . tpplicrbilityfor thc connccrior

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po.Box No. erss, Masadi Road,:,,j:111-i:"J No.47, : 3486659 Fax lili1il";llt^lll : 091- B0- 348 5374

TECHHOCRfiTS ONIOOE
@yahoo.com E-mail: weldaids

snc. vrtr Drv.l ^Errfi.4clsrnoM ASME

E.3 - - EVALUATION OTINDICATIONS imperfection.Only indicationswith ofa mechanical L indicationis the evidence relevant graterthan l/16 in' shallbe considered majordimensions i lin.u, indi.ution is onehavinga lengthgraterthan threetimesthe width. ". t.erounceaindicationisoneofcircularorellipticalshapewithlengthequaltoor lessthant},reetimesthe width' c.Anyquestionableordoubtfulindicationsshallbereexaminedtodetermine whetheror not theYarerelevant. t.4 ACCDPTANCE STAI{DARDS Th"**".pt-""standardsshallapp|yunlessothermorerestrictivestandafdsare within this Division' for specificmaterialsor applications specified shallbe free of All srfaces to be examined linear indication a. Relevant indicationsgreaterttnn 3/16 in rounded b. Retevant by 1/16in' or indicationsin a line separated c. fou. or *o.e t"tevarttrounderl= to edge) lesdedge that maybe largerthanthe imperfection olan imperfection d. An indication tlte sizeofthe indicationis the basisfor acceptance it; however, causes evaluation 'XTEICTAS FNOM ASME SEC. IX QW - 195LIQUID PENETARNT EXAMINATION weld in QW-214for corrosion-resistance examination dW-fSS.f Thi liquidpenetrant acceptance 6 The of sestionV Article metaloverlayshallmeetthe requirements met. shall be of QW-195.2 standards Criteria Acceptance QW-f 95.2Liquid Penetrant TelPinolory QW- 195.2.1 than 1/16 - indioations greatef with majordimensions indications a. Relevant in.(l.6mm) - anindicationhavinga lengthgreaterthanthreetimeswidth b. Linear indications - an indicationof circutaror elliptical shape with the length indicaUons c. Rounded timesthe width equalto or lessthan thLree Standards. QW f95,2.2Acceptance shaltbejudged techniques by liquid penetrant perfo-t uncetestsexamined n-rocedo"atrO ofthe limits in excess anyindicarion exhibits whentheexamination unacceptable below specified linearindications d. Relevant greater than3/16in.(4'8mm) indications rounded e. Relevant by l/16 in-(l.6mm) in a line separated indications rounded f. Fouror morerclevant or less(edgeto edge)

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ARTICLE 1
T-ll0 T-120 T- 130 T-140' T-150 T- 160 T- 170 T- 180 T-190
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Scope..........,. Cenera|,....,,.....,, Equiplnlt. Rquirements Procedure Calibration Eraminations and lnsDections Evaluation. Records /Documenlation

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Mandatory Appendix AppendixI Glossary of Termsfor Nondestrucrive Er(amination I-1l0 Scope...,....,..... I- 120 General Requirements I-|]0 Requirenrents .

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T-110 SCOPE

ARTICLE 1 GENERAL REQUIREMENTS

Afiicle of SubsectionA or as specified in orher Code Sections.2

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(c,l Unless otherwise specified by the refurencing Code Section or other referencingdocuments,this Section of the Code contains requirements and methods for nondestructiveexaminationwhich are Code reouirenlcnts to thc exlen! they are specifically referencei and required by other Code Sections.These nondesrructiye exilmination methods are intendcd to detect surface and intemal discontinuities in materials, welds, a-nd fabricateri pans and components. They include radioeraphic examination,ultrasonicexamination,liquid penctrant examination, magneticparticle examination,ddy current examination, visual exanrinaticn, leak testing, .urd acousticenrission examination. (D) For general terms such as Inspectiou,FIaw, DiscoDIi uitl, Evaluation, etc., refer to Mandatory Appendix L

T-130

EQUIPMENT

It is the responsibilityof thc.Manut'flcturer, fabricator, or installer to ensurethat the exxnrinrtion cquipmcnt being used conforms to the requirenrentsof this Code SectioD.

T-140

RBQUIREMENTS

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't'-120
GENERAL

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(d) Subsection A desqibes the methods of nondestructive examination to be used if referencedby other Code Sections. (bj SubsectionB lists Standards coveringnondestructive examination methods which have been accepted as standards, Tbesestandards are intendedto be infonnative only and are nonmandatory unless specifically refcrenced in whole or in part in Subsection A or as irldiciited in other Code Sections, 'of {c,} Refcrcncero a paragraph any Anicle in Subsec, lion A of this Scction or in tlrc referencinir Code Scction includcs rll of the applicabterules in rhe paragraph.' In every case, reference to a paragraph includesall the subparagraphs and subdir.isions under tl)rt paragraplr. (ri) Rcference to a Standardcontaincd in Subsection 13 is nrandatoryonly to the extent lpecified in an
I l'or er;rnrptc, refcrcncc td T-270 includcs ull rh. nrlus (onri|i|lcd i D 1 ' ' : 7 t t l r r o u g l iT , 2 7 ? . 3 .

(rr) Nondestructive ExanrinationPcrsourtel shall bc qualified in accordancewith tbe requirenrenrscf the referencing Code Section. (b/ For those Code Sections rhar direcrly refercnce lhis Article for the qualification of NDE. persontel, the qualification shall be ir accordance wifi one of rhe folldwing docunrents: (1) SNT-TC-1A,3 Personnel and CerQualificarion tification in NondestructiveTesting; or (2) ANSVASNT Cp-189,3 ASNT Standard for Qualification and Cedficatiofl of Nondes(nictiveTesting Persounel; or (3) ACCP,3 ASNT Central Cenification program. (c) When the referencing Code Section does nor specify qualifications or does nor reference dircctly Article I of this Section, qualiiication may sirrrply involve denronstratjon in routinc manulacturing operations to show that the personnclperforning the nonderFor example, T-213 rquircs tha( Inrigc Qurliry l dicntors bc manufaclured ind identificd in :tccoftl:rncewith the rcquirerncrls or i h e m a t i v e s a l l o \ | e d i r S E - 7 . 1 7o r 5 E - ! 0 2 5 , r n d A o i ) e l r d i c c s . ns . p n r o p r i l l t cf o r t h e s r y l c o f I Q t r o b c u s e d .t h e s c . ' r " i r i c o n t y r , r , r r s o f e i t h c r S E - 7 4 7 o r S E - 1 0 2 5t h n r a r c n r i r n d r r o l Ji n A n i c l e 2 . rSNT-TC'lA (1996 Edirio'r. wirh t99S i\ddcnitunr). I'crsonncl QurlificJlion and Ccriificnlion irr Nondtsrr*rire ,c],Jifl!:" ANSI/ A S N T C P - 1 8 9 ( 1 9 9 5 F d i r i o n , . ' A S N T s L : i t r l . , , Lr tt r r ) J . r t i r r : , u i o n and Ccrlificriion of NordcslrrKlivc Tcstin-! Pcfsonnctr" irnd ,\CCll 'ASN'l' lllevisio|l 3 (Nolcrulrr 199])1, C c r ) r | t r lC c i l j c r t i ( ) n l , r t ) h ) t h c A n | c r i c : r rS o c i c t yf o r N ( n r d l r l r L r c r i v t cc s l i r u . 8r:rDa publishcd l T t l A r l i n g r ( ( l n ' r r . t ' . O . I l . ' \ , l r i j l r i . a . ' 1 , , , , , 1 ' , ,,.r t ' ; , , . t r : : s . r t i t i .

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T-140

ARTTCI-EI _ CENERAL REQUIMMENTS

'

'r-170

structive examinttions are competent to do so in accordance witlr the Manufacturer'! establishedprocedures. fr?l Thc cenificare holder shall ensure that NDE personnel are qualilied and cenified ii accordance with thi$ 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 until recinification. Recertification or new cerdncation shrll be ir accordancewith the edition of SNT-TC-IA. Cp189, or ACCP specified in footnote 3. (l) Linited certification of nondestructiveexaminatiol pcrsonnel who do not perform all of the operations of !\ no|destmctive method that consistsof more thnn onc operation, or who perform nondestructive examinations of limited scope, may be based on fewer hours of training and experiencethan recommended in SNT'IC-lA. CP-189, or ACCP. Any limitationsor reshictions placed upon a penon's certificadon shall be describedin the wntten practiceand on the certification. (g) Tlrc SNT-TC-IA documentis a guide to esrablish practices for taining, qualification, and certification of Nl)E. personnel as required by the referencing Code Secrion,

Code, it shall be the responsibility of the Maoufacturer, fabricator, or installer to estdblishnondestructivcexamination procedurcsand personnelceni{ication procedures confomring to the referencing Code requirements. (cJ When required by the referencing Code.Section, all nondestructive examilations perfonned under rhis Code Seciiofl shall be done to a written procedure. This procedureshall be demonstraterl to the satisfaction of the Inspeclor.The procedureor method shall comply with the applicable requirements of this Secrion for the panicular examination method. Where so required, written procedures shall be made availableto tbe Inspector on request, At least onc copy of each proccdurc shall be readily available to the Manufacturer,s Nondesauctive Exantnation Personnel for their reference and use,

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T-160

CALIBRATION

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PROCEDURE

(a) The Manufacturer, fabricator, or insraller shall assurethat all equipment ctlibrations required by Subsection A and/or Subsection B are pcrfrrrnred. (D) When sperial procedures are developed fsee T150(a)1,the Manufacturer, fabricator, or installcr sltall specify what calibration is necessary,rvhen calibration is required.

examinationmethodsincluded f4, Tbe nondestructive in LhisSection are applicableto most geometricconngurations and materials encounteredin fabrication under nonnal conditions. However, special configurations and materials may require modified nrcthodsand techniques, in which case the l,{anufactuer shall develop special procedures which are equivalent or superior to the n]ethods and tecbniquesdescribedin this Code Section, and which are capableof producing interpretable examination results under the specia.l conditions-Such special procedures nray be modifications or combinadonsof nrethods described or referencedin this Code Section. and shlll be proved by demonstration to be capable of detecting discontinuitiesunder the specialcondirions, and such demonstratedcapabilities shall be equivalent to thc capabilities of the methods described in this Code Seclion when used under rnore generalconditions, Depending on the quality assuranceor quality control system requirements of the referencing Code Section, thcse spccial proccdures shall be submitted to rhe Inspcck)r for acceptancewhere required, and shall be adopted as part of the Manufacturer's quality cortrol Pro-qrilm. (/r.J Whcn ln cxanrination to the requiremcnts of this Scclionol the Codc is requircdby otherSections of the

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.T.170

EXAMINATIONS INSPECTIONS

AND

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{a) The Inspector concerned with the fabrication of the vessel of pressure part shcll, h,J,ve the duiy of verifying to his satisfaction that all exrminations required by the referencingCode Sectionhave been made to the requirementsof this Section and the referencing Code Section. He shall have the righr ro wirness any of theseexaminationsto the extent statedin the referencing Code Section. Throughout this Sccrior of the Code, the word Inspetlor means the Au pri:ed Inspector who has been qualified as required in Lh various referencing Code Sections. {0.) The special distincdon establishedin the various Code Sections between inspectiou tod e.ranination anrJ the personnel performing them is also adopted in this Code Section. In other words, (lle term rirr?drttorr applies to the functions perfonned by the Autlnrized lnspector, b.ut the term exanination applies to those quality control functions performed bv personnel cntployed by the Manufacturer. One areir o[ occasionill dcyiiltionfronl thesedistinctions exisrs.In thc ASTM Sla,ldilrdMethods and Recornrtren<led Practicesincomo-

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T- 170

2001sEcTIoN V

T.190

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rated in &is Section of the Code by reference or by reproduction in Subsection B, the words inspection or Inspector, which frequently occur iq the text or drles of the referencedASTM documents,may actually describe what the Code calls exatnination or exauiner. This situation exists becauseASTM has no occasion to be concemed with the distinctions which the Code makes between iaspecliol arrdexaminatiott,sinceASTM activ_ ities and documents do not involve the Authoized It$pector descibed in the Code Secdons. However. no xttempl has been made to edit the ASTM documents to conform with Code usagei this should cause no difficulty if the users of this Section rcogdze that the terms inspection, testing, artd examination in the ASTM documentsreferencedin SubsecticnB do not describe dulies of the Authorized Code Inspector but rather

describe the things to be done by the Manufacturer,s examina t ion personnel,

T-180

EVALUATION

The acceptance shndards for these methods shall be as stated iR the referencing Code Section.

T-190

RECORDS/DOCUMENTATION

Records/Documentationshlli bc in accordancewith the referencingCode Scction and rhe applicablerequirements of SubsectionA and/or B of this Code Section: The Manufacturer, fabricator, or installer shall be responsible for all required Rcco.ds/Documentation.

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ARTICLE 1 MANDATORY APPENDIX

indication - the response or evidence frorrr a nondestructive examination that requires interpretation1() detenniDe rclevance inspeition - the observation of any operation pert-rr0 scoPE formed on materials and/or components to determine its acceptability in accordancewith given criteria This MandatoryAppendixis usedfor the purpose li,tlited certificatiotr- an accreditationof an individuof establishing standard tems and definitionof terrns qualification to perform sonle but not all of the al's conmon to all methods usedin Noldestructiye Exami_ operations within a given nondesFuctive nation, examination mcthod or (echniquc that consistsof ooc or m,)rc than one operation, or to perforn no:ldestructive examina_ tions within a limitcd scopc of responsibility I-120 GENERAL REQUIREMENTS metlnd - thc following is a list of nondesfrnctile (c) The StandardTerminologyfor Nondestructive examination methodsand respective abbreviations used Exarninarions (ASTM E 1316)has been adoptedby within the scope of Section V: the Commiftee as SE-1316. RT - Radiography (rl SE-1316Section A provides the definition UT - Ultrasonics of ' ternls lisred in I-130(a). MT - Magnetic Particle (c) Paragraph I.130(b)provides PT - Liquid Penetrants a list of termsand delinitions,which are in additionto SE-1316and are VT - Visual Codc specific. LT - kak Testing ET - Electromagnetic(Eddy Cunenr) AE - Acoustic Emission no,tdestructive emminarion (NDE) - the developI-130 REQUIREMENTS ment and application of tech[ical nlethods to extmine (al The following SE-1316termsare used in conjuncmaterialsand/or componelltsin ways rhar do not inrpair tion with this Article: defect, disco thruiry*, evalu.ttion, future usefulnessand serviceability in order to detect, fel"^e indication, faw, law characterization, impetfecIocate, measure, interpret, and evaluate flaws I ior1,utterprctution, nonrekvant indication, relevant inoperation - aspecific phaseof a nerhod or technique ptocedure - an ordedy sequence of actions dgs-crib(D/ The foJlowing Code termsare usedin conjunction ing how a specific terhnique shall be applicd with this Anicle: sexsirivitl a measureof (hc lcvel of response erea of intcrcst - the specific po(ion of the object fronr a discontinuity by a nondestruclive exilnlilirtion thal is to be evaluated as denned by the referencing tecluique - z techniqucis a specilic rvay of utiliz_ing (lode Section a Fonicularnondestructive examiuation(NDE) method

APPENDIXI_GLOSSARYOF TERMS FOR NONDF,STRUCTIVE EXAMINATION

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T-600 T-610 't-620 T42l T-630 T-631 T-640 T-641 ^t_642 T-643 T-650 T_651 T-652 T-653 T-654 T,610
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ARTICLE 6
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T-6"12 T,6',73 T-6'74 T-6?5 T-676 T-680 T-690

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!-igure T-653.2

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Trble T-612

MinimumDwell Times ,. .. . ... -. .. .

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I{rndatory Appendix Appendix I I-6t0 t-620 Geieral Requirements . . . . . . . . . . . . . - , _, I,630

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ARTICLE 6 LIQTJID PENETRANT EXAMINATION

T-600 SCOPE
procedure shall includeat leastthe following information, as applicable: (aJ the materials, shapes,or sizes to be examined, and lhe xtent of the examination: (b) lype (numberor letter designation if available) of each penetralt, penetmnt remover, emulsifier, end developer; (cJ processing details for pre-examination cleaning and drying, including the cleaning materials used and minimum time allowedfor drying; (d) processing detailsfor applyingthe penctrant: tbe lenglh of time that the penetnnt will remain on the (dwell time),andthe tempemtqre surface of the surface peretrant and during the examination if ourside50'F (10'C) to 125'F (52'C) range; () processing penetrant detailsfor removingexcess from the surface, and for drying the surface before applyirg the developer; (/) processing detailsfor applying the developer, and lengthof developing time before interpretation; (8) processingdekils for post-examination cleanitg. T-621.2 Procedure Revision. A revised procedure may be required: (a) wbenevera changeor substitutionis madein the type or family group of penetrantmaterials (insluding develolnrs, emulsifiers,etc.) or in the processingtechniques; (b) whenevera changeor substitution is made in the type of precleaning materials or processes; (c) fq any change in part processing that can close surfmeopenings of discontinuities or leaveinterfering deposits, suchas tlte use of grit blast cleaningor acid treatrnents.

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The liquid penetant examinationmethodis an effective means for detecting discontinuities which are open to the surfaceof nonporousmetalsand other materials. Typical discontinuities detcrableby this method are cracks,seams, iaps, cold shuts,laminations, and pcrosity. In principle,a liquid penetrant is appliedto the surface to be examined andallowedlo enterdiscontinuities. Alt excess penetrant is then removed, the part is dried, and a developer is applied.The developerfunctions both as a blotter to absorb penetnnt that has been trappedin discontinuities, and as a contasting backgroundto enhance the visibilityof penetrant indicationsThe dyesin penehants are eithercolor contrast (visible underwhitelight) or fluorescent (visibleunderultraviolet light).

T.6T0

R-EF'ERENCINGDOCUMENTS

T-610.1 Wben specified by the referencing Code Section, the liquid peneEant examination techniques describedin this Article shall be ujed. The following SE Standardprovides details that may be considered in the specificprocedures used: (a) SE-165 StandardTest Method for Liquid Penelrant Examination T{10.2 The liquid penehantmerhoddescribedin tlis Anicle shall be used togetherwirh Article l, CeneralRequirements. T-610.3 Definitions of termsusedin this Article are in Mandatory Appendix I of rhis Article.

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T.630 T-620
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EQUIPMENT PenetrantMaterials

GENERAL ProcedureRequirements

T-6f

T-621

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f-621.1 Liquid penetrant examiration shall be performed in accordance with a written procedure. Each
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Tlnetermpenetrant mateials, as usedin this Anicle, is intended to include all penetrarts, emulsiflers, solveots or claning agents, developers, etc,,usedin the examina-

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ARTTCLE 6 _ LIQUID PENETRANT EXAMINATION "t-642

tion process. The descriptions of &e liquid penetrant classifications and materialtypesarc providedin SE165.

T.640
T-641

REQUIREMENNS

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Control of Contamitrants

(b) Whenexamining austenitic stainless steelor titanium, all materials shall be analyzed individuallyfor chlorineand fluorine contentas follows. (.1, An individuat sampte of the penetrant malerials with the exception of cleaners shall be prepared for analysisby heating 50 g of rhe material in a 150 mm nominaldiameter glass Petri dish at a temperature of 194"Fto 212'F (90"C to 100.C) for 60 min.
PRECAUnONT horide adequarevenritaiion to dissipateihe emir_ reo vaPor.

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The user of this Afticle shall obtaincertification of contaminant contentfor all liquid penetrant materials usedon nickel basealloys, au$eniticstairlesssteels, aod titanium. These certifications shall include the penetrant manufaciuiirs' batcb numb6rs and the test results obtainedin acbordance with (a) and O) below. These records shall be maintainedas required by the refcrencing Code Section. (o) When examiningnickel basealloys, all materials shall be analyzed individually for sulfur content as follows. (./) An individual sample of thepenetmnt materials rvithexception of cleaners shallbe prepared for analysis by herting 50 g of the material in a 150 mm nominal diarueter glassPefti dish at a temperature of 194"Fto 2l?oli (90oCto 100'C)for 60 riqin.
PI{ECAUTIOh$: Provide adequate vcnrilation ro dissipate the enril-

(2) If thercsidue is 0.0025 g or more,tbc procedure shown in (b)(l) above shall be repeated. The residue may be analyzdin accordance with SD-80g and the total shall not exceedl% by weight. Or, attemately, the residueshall be analyzed in accordancc with SE165, Annex 2 for chlorlneand SE-165,Annex 3 for fluorine, and the total chlorine plus fluorine content shall not exced1% by weight. (3) An individual sampleof the cleaner/remover materialsball be prepared for analysis by heating100 g of the material in a 150mm norninaldiametcr glass Petri dish at a temperarure of t94"F ro zlZ"F (90"C to 100'c) for 60 min.
PRECAUTION: Prcvideadequatc venrjlarjon ro dissipate the emitted vapor.

{?) Analysis of the residue shalt be as follows: If the residue is less than 0.0025 g, the material is accepteblc without funher analysis. If the residue is 0.0025 g or more, the procedureshown in (a)(l) above shilll bc rcpeatedand the rcsidueanalyzedin accordance n'itlr SD-129 or SD-1552. Alrernalely, the material may be decomposed in accordrncewith SD-lZ9 and alalyzed rn accordance with SF5l6 Method B. The iulphur content sllall not exceed l% of tIrc residue by weight. (-l) An individuat sampleof cleaner/removermaterirl shall be prepared for analysis by hea(ing t00 g of the naterial in a 150 mm nomilal diameter glass Perri dish at a Gmperatureof I94.F to 2t2.F (90'C to 100'C) for 60 min. PIII'CAUTION: ltovidc adequate venrilarion ro dissipare the
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(4) If the residueis 0.005 g or more, rhe procedure shown in (b)(3) above shall be repeated. The residue may be analyzed in accordancewith SD-808 and the 'total shall not exceed l% by weight Or, alternateiy, the residue shall ba analyzed in accordance with SE165, Annex 2 for chlorine and SE-165, Annex 3 for fluorine, and the total. chlodne plus fluorine content shall not exceed I% by weight. (c) As an altemative to (a) and (b) above, SE-165, Anaex .{4 may be used for dslelrninalion of anions by ion chromatography,which provides a single instrumental technique for rapid sequential meastrrement of conmofl anions such as chloride, fluoride, and s[lfate. T-642, Surface Preparation

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(4J Analysis of the residue shall be as follows: If rhc rcsidueis lessthan 0.005 g, the materialis acceptable rvitbout lurthcr analysis. If the residue is 0.005 g or rDore, the procedure shown in (a)(3) above shall be rei)eatedsnd the residue analyzcd in accordancewith SD- I2a or SD-I552. Atternarelytire marerialmay be decomposcd in accordancewith SD-129 and analyzed in accordance with SD-516 Method B. The sulphur corrLcnL shrll not exceed l% of the residueby weight. 123

(a) In general, satisfactory results may be obtained when the surface of the pan is in rhe as-welded, asrolled, as-cast,or as-forged condition. Surface Dreplration by grinding, machining, or otlrcr mcthods rnay be necessarywhere surface inegularities could rnask indications of unacceptablediscontinuities. (0, Prior to each liquid penetrant examination, rhe surface to be examined and all adjacent areas rvithin at least I in. (25 mm) shall bc dry and free of alj ditt, grease,lirt, scale,welding fiux, weld spatter,paint, oil, and other extraneous mrtler that could obscure

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2001SECTION V surfaceopeningsor otherwiseinterfere with the examination. rleaning agentswhich may be usedare Ic) Lyptcat detergents,organic solvents, descaling solutions, and paint removers.Degreasing and ultrasoniccleaning methodsmay also be used. (dl Cleaning solventsshall meet the req[iremeilts of T-641.-The cleaning methodemployedis an important part of the examination process,
NOTEI Condidodng of surfaccs grior lo cxami[ation rnay affecr tle resule Scr SgteS. eraex.l,i.

T-653.3 Techniques for Nonstandard Temperatures

T-653

T-653.1Ceneral.Wher it is not practical to conduct a liquid penebant examination within the temperature rangeof50'F to t25.F (10.C to 5Z"C),theexaminarion procedureat the proposedlower or higher temperature range requiresqualification. This shall requireihe use of a quenchcrackedaluminumblock, wiicfi in this as a liquid penekantcomparator r Article is designated block. T{53.? Liquid penetrant Comparator.The tiouid penetrant comparator blocksshallbe made of aluminum. ASTM B 2@, Type 2024,3/ziD. (10 mm) thick, anj should have approximateface dimensionsof 2 i'I.. x 3 in. (52 mm x 76 mm). At'$e centerof eachface. an areaapproximalely I in. (25 mm) in diameter shali be markedwith a 950"F (510"C) temperature,inCicating crayon or paint. The marked area shall be heatedwirh a blowtorch,a Bunsenburner,or sirnitardevice!o a temperature berween 950"F(510.C)and975.F(524"C). The specimenshall then be immediately quenchedin cold water, which produces a networkof fine cracks on each face. The block shallthenbe dried by heatingto approxima@ly300'F (149.C). Afrer cooling, the block shalt be cut in half. One-half of the specimenshall be designated block 'A' and the orher block ..B" for identificarion in subsequent processing. FigureT-653.2 .,A" rllusEasthe comparator.blocks and .,8.,, As ar altemate to 6u[ing the blcck in half to make blocks "A" and "B," separateblocks 2 in. x 3 in. (52 mm 76 mm) canbe madeusing the heatingand quenching 1 te;hnique as describedabove.Two comparatorblocks 'with closely matched crack pattems may be used-The bloclcsshall be marked.A" and .,8." T.6533 Comparator Apptication (a)_If.it is desired to qualify a liquid penetrant eXaminadonprOOedure at a aemperalure of less than 50"F (10"C), rhe proposed procedure sha.llbe apptied to block "B" after the block and all materials itave been cooled and held at the proposedexamination tempen[ureuntil the comparisbn is completed. A stan_ dardprocedure whichhaspreviously bec; dembnstrated as suitablefor use shall be appliedto block.,A', in the 50'F ro 125"F(10.C ro 52.C) temperature range. The indications of cracks shalt be comparedbetwe-en blocks"A" and *8.' If the indications obtainedunder the proposed conditions on block .,8" are essentiallv the sameas obtained on block -A,' duringexamination al50'F ro 125'F(10'C to 52.C),theproposed procedure shall be considered qualifiedfor use-

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T-643

Drylng Aftr preparation

Afrcr cleaning, drying of the surlaccslo be examined shall bc accomplishedby nornal evaporadonor wilh forced hot or cold ah. A minimum period of time shall be establishedto ensured|at the cleaningsolution has evaporatedprior !o application of the penehant.

T.650 T-651

PROCEDURE/TECIINIQUE Technique

Ejther a color contlasr(visible) pne&ant or a fluorescent penetrantshall be usedwith one of the following threepenetrant Pmcesses: ' (a.) water wasbable (b) post+mulsifying (c) solvent removable The visible and fluorescent peletrants usedin combiyjth these tfuee penetant processes resulr in ".u,i:." slx lrqurd penetrant bchniques,

T-652

Techniques ior Standarrt Temperafures

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As a standard techniquq the remperatureof the fen-etrantand the surface of the palt to be processed shallnor be below 50"F (10"C)noi aboveI25;F (52.C) (hroughour aheexamination period. Ircal heatingoi cooling is permitted provided the pah temper=tu.e remains in rhe rangeof S0"F ro 125.F(10.C ; 52"C.) during the examination. Where it is not practicalt; complywith these temperature limitations, othertemperarures and timesmay be used,pmvidedthe procedures are qualifiedaslspecitied in T_653. . " \ ."' t24 l'.. i \\J

T-653.3

ARTICLE 6 _ LIQUID PENETRANT EXAMINATION

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then after processingat the standardtempi,rature. The indicationof cracks shall be comparedbetweenthe two photog:aphs. Ttre samecriteriafor qualificarion as T-653.3(a) shatl apply. (2) The identicalphotographic techniques shall Le usedjo Take the comparisonphotographs. T-654 Technique Restrictions

Fluorescent pefletrant exarnination shall iot follow color a contrastpenetrant xamiflation. Intermixingof penetrantmatedals from different families or different manufacturers is rlot pemitted. A retest with water wahable peDeuants may cause lossof marginalindica_ tions due to contamination.

T.670 T-671 FIG.I-653.2 LIQUID PENETRANT COMPARATOR (N0TE:Dirnensions given arefor guidance onlyandare notcritical.)

EKAMINATION Penetrant Apptication

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Tl|e penetrant may be appliedby any suitable means, suchas dipping,brushing, or spraying. If the penetrant is applicd by spraying usingcompressed-air-rypc appara_ tus, filters shall be placedot the upshear.n side near the air inlet to preclude coRtamination of the penetrant by oil, water,did, or sedinleltihat may havecollected in the lines. ''l-672 PenctrationTime

(1r)If the proposed temperature for thc examination is above125"F(52"C), block.B', shallbe heldar rhis tenrperatufe throughout theexamination. The indications of cracksshall be compared as described in T-653.3(a) while block "B" is at the proposed temperatute and block "A" is at rhe 50.F to 125.F (10"C ro 52"C) temPcraturc range. (c')A procedurequalified at a temperature lower than50'F (10'C) shallbequalified from rhatremperarure to 50'F {10"c). (d) To qtalify a procedurefor temperatures above 125'F (52'C), the upper and lower tempemture limits shallbe established and theprocedure qualifiedat thesc tcnlperatures, (e) As an alternate to therequirements of T-653.3(a) and T-653-3(b)when using color conhastpenetrants, it is permissible to use a singlecomparatot block for thc slandard nnd nonstandard bmperatures andto make thc comparison by- photography. When /,1) rhe singlecomparator block andphotographic techniqueis used,the processing details(as applicable)describedin T-653.3(a) and T-653.3(b) apply. The block shatl be thomughlycleaned between the two processing steps.Photographs shall be taken attcr processing at the nonstandard terirperature and
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Penetration time is critical.The mininrum penerr:rtion time sballbe as required in TableT-672 or as qualilieri by demonstration for specificapplications. T473 ExcessPenctrant Remoyal

After the specified penetration time haselapsed, any penetmnt remainingon the surfaceshdl be removed, taking care to minimize removal of penetrantfronl discontinuities. T-673.1Water-Washable Penctrants. Excess warerwashablepenetrantshall be removed with a water spray. The water pressure$hall not exceed50 Dsi (3a5kPa),and thc wrtcr tcmpraturc shallnot cxccc,l r l0'F (43"C). T-673.2 Poslemulsification Pr:nctrants (a) Upophilic Enulsifcation. Aftet therequiredpenetrant dwell tirne, the excess pen;truntshall bc surface emulsified by immcrsingor floodingthe paft wirl) thc emulsifi . Emulsilicationtimc is depeodent on thc type of emulsifierand surfacecondition.The ac(ui\l

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T -613.2
2001 SECTIONV T -676.2

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emulsification time shall be determined experimentally. After ernulsification, ahemixture shall be removedby immdning-in or.rinsing with water.The temperature and pressure of the water shall be as recommended by the manufacturer, (b) Hydrophilic Emulsifcation. After the required penetrant dwell time and prior to emulsification, the parts shall be prerinsedwith water spray using the process as for water-washable same penetrants. Prerinsing time shall not exceedI mir. After prcrinsing, the penetrant excess surface shallbe emulsified by immersing in or sprayingwith hydrophilicemulsifier.Bath concentration shallbe as recommended by the.rrra[ufa:turer.After emolsification, the mixtureshallbe removed by immersing in or rinsingwith water.The temperature and pressure of the wa6ershall be as recommended by the manufacturer.
NOTS: Additionalinformarion lnay be obrained from SE-165.

With color contrast penetrants, only a wet developer penetrants, shall be used,With fluorescent a wet or dry developer may be used. T-675.1Dry DevelopcrApplication.Dry developer shaU be applied only to a dry surface by a soft handpowderbulb,powdergun, or othermeans, brush, providedthe powderis dustedevenlyover the entire surfacebeing examined. T-675.2 Wct Developer Application. Prior ro applyingsuspension type wet developer to the surface, the developermust be thoroughlyagitatedto ensure adequate dispersion of suspended particles. (a) Aqueous Developer Application Aqueous developer may be appliedto either a wet or dry surface. It shall be appliedby dippidg, brushing spraying, or provideda thin coatingis obtained other means, cyer the entire surfacebeing examined. Drying time rnay be decreased by usingwarm air, providedthe surface temperature of the part is nof raised above 125'F. Blotting is not permitted. (b) Nonaqueous Develope r Applicatiol. Nonaqueous developer shall be appliedonly to a dry surface. It shaUbe appliedby spraying,except\1,here safetyor restrictedaccessprecludeit. Under such condirions, developer may be appliedby brushirg. Dryirg shall be by normal evaporation. T-675.3Developing time for final interpretation begirs immediately aftertheapplication of a dry develoger or as soon as a wet developercoating is dry. The minimumdeveloping time shallbe asrequired by Table T-6'12.

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SotventRemovable Penetrants. Excess solvcnt removable penetrants shallbe removed by wiping with a cloth or absorbent paper, the operation repeating until nrosttraces of penetrant havebeenremoved. The renaining tmces shall be removedby lightty wiping the surfacewith cloth or absorbent paper moistened with solverlt-To minimizeremovalof penetrant from discontinuities, care shall be takento avoidt}|e use of excesssolvent. Flushing the surface with solvent, follorvingthe applicationof th penetrantand prior to developing is prohibited.

'f.673.3

T-674

Drying After Excess Penetrant Removal

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T-676

Interpretation

(s2"c).

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(b) For the solvent removable the surfaces technique, may be dried by normalevaporation, blotting,wiping, or forced air.

T.676.1 Final Interpretation. Final interprecation shallbe madewithin ? to 60 min afterthe requirements of T-675.3are satisfied. If bleed-out doesnot alter the examination results,longer periods are permined.If the surface to be examined to preclude is largeenough completeexamination within the prescribed or established time, the examinationshall be perfomredin increments. T-676.2 CharacterizingIndic.ation(s). The type of discontinuities are difficult to evaluate if the penetrant diffuses excessively into the developer. If rhis condition occurs.close observation of the fonlation of indicalion(s) during application of thc developer may assist in characterizing and determiningthe ex(enr of rhe indication(s).

T-675

- Developing

The developer shall be appliedas soon as possible after penetrantremoval; the time interval shall not excced(hat estrblishedin the procedire.Insufficient coatingthicknessmay not draw the penetrant out of discontinuities; conversely, excessive coatingthickness nay nraskindications.
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ARTICLE 6 _ LIQUID PENETRANT EXAMTNATION

T-690.1

TABLE T{72 MINIMUM DWELT L IMES

Dwell Times (l)l (minutes) tNote
Material Aluminum,magnesium, steel,brass and bronie, titaniumand high_ temperature alloys Castings andtrlds
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Type ot Discontioutty
Coldshuts,porosity,lack of f!5ion, . cracys (all forl,6) Laps,cracks (all forrns) Lack of fusion porosity, cracks Cracks Cracks Cracks, poroslty

Penetrant Developer

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Carbide-tipped tools 'Plaslic Glass Ceramic NOTE: (1) Fo/ temperature rangefrom

Wroughtmaterials - extrusions, {orgingr,plate All forms All forms All forms sooF to 125"F 6O.C to 5z.C).

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T-676.3 Color Contrast penetrants. With a color col"trast penetrant,. the forms a reasonatrly -developer urulorn white coating. Surface discontinuitiesare indi-_ calcd by blecd-out of the penetrantwhich is nomally ri dcel) rcd coJor thrt stains &e developer. Indications with a light pink.color may indicate excessivecleaninglnadcquatecleaning may leave an excessive backgrouri rnrking interyretation difficult. A minimum lighiinten_ fc (500 Lx) is r"4uired to ensure;equjtc :ll :t:O $cnsltivity during the examinationand evaluation of indica(ions_ T-676.4 Fluorescer.t penetranls. With fluorescenr penetrants, the process is essentially the same as in T-676.3, with the exception that the examination is pcriomrcd. using an u_ltraviolet lighr, called black light. lr)e exanrination shall be performed as follows; (a) It shall be performed in a darkened area (DJ The examiner shall be in the darkened area lbr at lelsr I rnin prior to performing the examination to enrDjc lr,s eyes to adapt to d3rk viewing. If tlte examiner wcars glassesor ienses,they shall not be photosensitive, (cj The btack light shall be allowed to warm up for a minimunl of 5 min prior to use or measurement of rne rntensiryof the ulrravioletlight emitted. The black light intensity shall be measured wirh .(dJ a orack trghl meter.A minimum of 1000pWlcmr on the surfaceof the part being exanrined shall be required.

The black light intensity shall be measured at least once every 8 hr, and whencver the work station is changed. T-677 post.examination Cleaning

When post-examina[ioncleirning is required by the pmcedure, it should be conductedas soon as practical usrng a processthat does nor adversely affect ihc part. , T.680

EVALUATION

(a) All indications shall bc evaluated in terms of the acceptanceshndards of the rcferencing Code Section. (bJ Discontinuities at the surface will bc indi.Jated by bleed-out of penetranq however, Iocaljzed surface irregularities due to machining marks or other surface concitrons may produce faise indications, (cJ Broad areas of fluorescence or plgmentalion which could mask indications of discontiiuities are unacceptable, and such arcas shall be clcaned and reexamined.

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T-690

DOCUMENTA'i'ION/RECOITDS

T-690.1 Documentation/recordsshall be in accord_ ance with the referencing Code Section,

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ARTICLE 6
MANDATORY APPENDIX
APPENDIXI_GLOSSARYOF TERMS FOR LIQUID PENETRANT EXAMINATION I-610 SCOPE This Manda[ory Appendix is used for the purpose of establishingstandardterms and definition of terms which appear in Article 6, Liquid penetrant Exami_ nation.
I-630 RIQUIREMENTS

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1.620

GENERAL REQUIREMENTS

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(a) The StandardTerminologyfor Nondestructive Examinations (ASTM E 1316) has beer adopredbv the Cornmi(ee as SE-1316. fb) SE-1316SectionG providesthe definitionsof termslisted in I-630(a). (c) For general cerms, such as Ind.ication, Flaw. Discontinuiry, Evaluarion, etc.,refer to Anicle I, MandatoryAppendix 1. (d) PangraphI-630ft) providesa list of terms and definitions, which are in add.ition to SE-1316 and are Codesnecific-

(4] The following SE-1316terms are used in coniunction with this Article: black light; bleedour; bloiting; clean; cofitaminant; contrasfi developer; dcveloper, aqueous;develoi)cr,dry; devclopcr, nonaqueousi devel_ oping time; drying time; dwell time; emulsifler; family; fluoresce[ce; overemulsification: penetmnt; penehant comparator; peoetra;t fluoresceor; pene$anl, water washable; post-cleaning;post emulsification; precleaning; rinse; solvent ren]over. (b) Thc following Cr:detcnns are usedin conjuncrion with this Article: black light intensit! - a quantirative expressionof ultmviolet inadiance color contrastpenerralt - a bighly pcnerratingliquid incorporating a nonfluorescent dye, which produces indications of such intensity thlt rhcy ar. readily visible during examination under white light post emulsif.cationpenetant - a type of peneirant containing no emulsiner, but which requiresa separate emutsifying step to facilitate waler rinse removal of the surface penetrant solvent removablepenetrant - a typc of penerrant used where the excess penefiant is removed from the surfaceof the part by wiping using a nonaqueous liquid

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ARTICLE 24 LIQUID PENETRANT STANDARDS

SD-129 StaldardTest Methodfor Sulfur in petroleum products(Cenerat (ASTM D 129-95) Bomb Me$od)_..... ........._....... 44s

SD-516 Standard TesrMerhodfor Sulfate Ion in Warcr. . . . . . . . . . . (ASTM D 516-90)

....._

44t)

SD-608 Srandard Tesr Methodfor Chlorinein New and Used perrolcum (ASTM D 808.95) products (BombMethod). .........

.. .....

453

SD-1552 Standard Tesr Methodlbr Sulfur in pctroleumproducrs (High_ (ASTM D 1552,95) Temperature Merhod) ,..........

. . . ... ..

457 464

SE-I6J n |x a m i r a r i o S r a n d r rT de s tM e f t o df o r L i q u i dp e n e r r a E .n . ... . . . . _ . . . . . . . . . . . , . . . . (ASTM E 165-95)

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STANDARD TEST METHOD FOR SULFUR IN PETROLEUM PRODUCTS (GENERAL BOMB METHOD)
sD_129
(Identical with ASTM D 129_95) (fhis specification is available in SI Units only.)

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Scope

1.1 This test method covers the determination of sulfur in petroleum prnducts,including lubricating oils containing additives,additiveconcentrates, and lubricat_ ing greasesthat cannotbe bumed completely in a wick Iamp. The test method is applicable to any petroleum product sufficieotly low in volalility that it can be . weighed accurately in an open sample boat and con_ talnjng at Ieast 0.170sulfur.
elcmenG lhar givc residues, otlEr lhBn barium sulfite, which ari insoluble in dilute hydrochloaic acid and would inrerfcre in rbe precipjtalioD step, Thesc inteifaring clements includc iron, aluminum, calcrum, siiicon, and lead c,hich arc sometimes presenr in greases, Iube oil addirives, or addirive oitr. Other acid insotubte m;lcrists lhat inrcrfere are silic4 molybdcnum disulfide, asbestos,mic4 elc. Thc rest rnethod is not applicrblc to uscd oils conraining wcar mcrals, l'nd leid or silicares from contamiaation.Samplcs thni are cxcluijed cilrl bc anfrlyz-d by Tesr M.thod D 1552.

E 144 Practiccfor Safe Use of OxygenCombustion Bombs

3,

Summary ot Tcst N.{ethod

NOTEI - Thjsresr nerhod is norapplicable to samples contaiDing

3.1 Tlle sampleis oxidizedby cornbustion in a bomb containing oxygenunderpressure. The sull'ur, as sulfate in the bomb rvashings, is deterntineil grlvimetricirlJy as bariunl sulfiltc. 3.2 lYarning * Sticr adl.tererce to all. oJ the provisions prescribed herealer etrttres against explo_ sive rupture of the botnb, or a blor.out, providetl the bornb is of propcr design and con.rtructionttntl in goorl ,rechanicql co dition. It is desirable, h,.ty,e,ter, rhttt the boob be enclosed in a shield of stecl l)!.le dt leosl l3 nn thi&, or uJ iwtlent hrotct:tio,t hc providcl t . t i t t s l u J i t r s a tl ( t . ) n | i g , . t i ! , . \ .

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1.2 This snndqrd does not purport to address all (l the :;efelf cotcerni if any, as.rociated ti r its use. II is the responsibility oJ the user of this standard to establish appropriate satetyand health practices and delennine the applicahility of regulatory limitations pior to use. See 3.2 for specificprecautionarydircctions incorporated'in the test method.

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Apparatus tnd Nlateriats

2.

Referenced Documents

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2.7 ASTM Statdards: D | 193 Specification ffi Reagert Water D 1552Test Method-forSulfur in petroleumproducrs (lli gh-TemperatureMerhod) 445

4.1 Bonh, hitving l cilpacilyof not lcss rhan 300 nrl-, so conslruc(edthat it wilt not leak during the test and that quantit tive recovery of the liquids frorn lhe bomb miry be achieved readily. Thc inncr surlace of the bomb may be tnlde of stai,ricss steelor aty orher naterial thal will not be affectedby the combustiorr proceris or products, Materials uscd in thc bornbassem_ bly, such as thc head gasketand lcld,wire insuhtion, shall be resistant to helt ind chenicll action,and shall noi unclcrgoi[ry rcilction thir will alfccr the sulfdr contentof thc liquid in rhc ixrnrh.

SD-I29

2OOISECTION V 6. Proccdure

4.2 kutltlc Crrp,platinunr,24 nrnr in outsidediametcr at the bottom, 2? rnrn in oubidc diameterat the tbp, 12 rrnr in heiglrt ourside,and weighing l0 to ll g. 4.3 Firitg lyi?, pla(inum,No. 26 B & S gage,0.41 nnr (16 thou), 27 SWC, or equivatent, - Theswirch jn rheiSnirioo NOTE2r Caution circuit shall be of
a rypc which rernxins opcn, exc.pt whcn hcld in closcd posirion by

4.4 lgnitiort Cirrir, capable oi supplyingsufficient currenr ro jgnite the cotton wicking or nylon thread without olelting thc wire. The curent shall be drawn fronr a stcp-down transformer or from a suitable battery. 4.5 Cofton Wickitlgor NyLn SewingThread,white.

6.1 Preparation of Bornb and Sanple - Cut a piece of firing wire I00 mm in lcngth. Coil rhe middle section (about 20 mm) and attach the free ends to the terminals. Arrange the coil so that it will be above and to one side of the samplecup, Insert between two loops of the coil a wisp of cotton or nylon thread of such length that one erd will extend into the samplc cup. Placeabout 5 mL of Na2CO3 solution in the bonrb (Note 3) and rotate the bomb in such a manner that the interior surface is moistenedby the solution. Introduce into the sample cup the quantities of sample and white oil (Notes 5 and 6) specified in the following table, weighing the sampleto the nearest0.2 mg (when white oil is used, stt the mixture with a short lensth of qutrtz rod and allow the rod to remain in the sam-ple cup during the combustion). NOTE3 - Afterrepeated uscof ihebomb for sulfordelerminadonsa nlm may b noticed on lhe inn.a surface. This dullncss can be removd polishing by periodic of drc bornb.A satisfactorv $e(hod for doing rhisis to rolare ftc bomb in a larhe at abour 300 |Pm rnd pohsh tfic ioside surface wirhenerypotishing papcrs GrirN-o. pape., 2,, or cquivalent coated wirhr lighrmachine oil to pre\.cnr

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Rcagcn(s und Mctcrials

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-i.l Prrrrr_r, oJ Reagents* Reagent grade chemicals shillj bc used in ali tests.Unlessotherwiseindicated, it is intended tltilt {ll reagentsshrll conform to the spccilic1lriorls of the Conrmittec on AnalyticalReagents of the ,A.nterican CltcmicalSociety,where suchspecificiltior)sare available.Other gradcsmay be used,providcd it is llrst r.jccnaincd thiLt thc rc gent is of sullicienrly high purity ro pcrnrir jrs use without less_ e n l - t j L h cu c c u f i r c y of llte dctcr li lltion. 5.2 Purity uf lvdet - Unlcss otherwise indicated, refereltces tr: rvaier shall meao wtter as defined by T y p c I l o r I I I o 1 '. S p c c i f i c a t i o Dn 1 1 9 3 . 5.3 Buriunr Chloride Soltuiott (85 g/litre) - Dissotve 100 g of barium chloridedihydrare (BaCl2. 2H2O) in distilled rvatcr and dilute to I Iitrc5.1 Ilrontirv Weter (satur(jted). 5,5 Jlsrlnx:ltloric;1crr/ (sp gr t.l9) hydrochloricrcid (ttCl). Concentratcd

cutt;ng. rnd rhcn wilh a paste of grjr-frEe chfomic oxide and watcr. 'fhis.pr.cdure \rill rehove all bur very deep pirs and pul a hi:h polrih on the surlace. Bcfore rie bomb is used ir jhall be washcd wilh soap and warer ro remove oil or patte lfr from the pol;shing operniionNOTE 4: Caution - Do not use more ihan 1.0 g rotal of samplc and white oil or olhea low sulfur combusrible mate.ial or more ltar. 0.8 e if the lP 12 bonb is used.

Sulfur Content, % 5 or undcr

Weigbt of Sample, I 0.6 to 0.8 0-3to 0.4

Weighrof WhireOil,g 0.0 0.3 ro 0.,1

tj9TF 5 - Use of sampteweiehlsconrainingover 20 mg of chlorinemay causecorrosionof the bomb. To avoid this. it js recoormended that for samples cootaining over 2% chlorine,lhe samplewcight be basedon lhe chtorinccontentas given in rhe follo*inp rabie: Wcighrof Sample, I 0.4 0.2 0.1 0.05 wciShrof WhiteOil, g 0.4 0.6 0.7 0.7

5.6 O-n'qca,frec of combustiblcmllcrial and sulfur coDrpolrn{Js. aviljlablc lt tr prcssurc ol 4l kgf/cmz {40 rlrrr). 5.7 Sodint CarLtctrtQrc Solution (50 g/litre) _ Dis_ solve 135 g of sodium carbonate decflhTdrate (Na2CO1 l0ll-O) or irq equivalcnw r c i g h Li n d i s t i l l e dw a t e r and diiure ro I iitre. 5.8 ll4rire Oif, USP, or Liquitl par<ffir, Bp, or

Chlorine Conlenl, % 2to5 Over5 to l0 Ovcr l0 lo 20 Over20 lo 50

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NOTE 6 - tf rhe sampleis nor readitymiscjblewi$ whitc oil, some o$er low sulfur combustible dituent may be substituted. (he combinedwejghtof sampleand nonvolatile However, djluenl shallnot xcecd1.0g or mor. rhan 0.8 g if the Ip 12 bombis used, 6.2 .Addition of Oxygen - place the sample cuD in position and arrange the cotton wisp or nyion thread so that the end dips into the sample. Assemble the bomb and righten the cover securely. (Caution _ See

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. ' ARTICLE 24 _ LIQUID PENETRANT STANDARDS

sD,129

Note 7.) Admit oxygenslowly (to avoid blowing the oil from the cup) until a pressue is reachedas indicated in the following table: .;S:1, ;
Capaciti of Bomb.d' 300 ro 350 350 to 400 400 to 450 450 to 500

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MiniqutoGaBq . ,: MaximumGage Pressurei kgf/cml(attn) Prcssuic,^kgfl.in'z (atin) 39 (38) 4l (40) 36 (35) , 38 (37) 33(3?) . 3l (30) 28 (27) 30(29)..

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'1Thc minimurn prcssuresarc speaifred ptovide to sufncieDtorygen for complete combustioh and thc natimM prcssuhcs tcpletent a :afetj- requircnent. IOTE ?i Caulion - Do nor edd oxygetrot ignile lhe sampleif the bomb has beenjarred, dloppe4 o! rilied, 6.3 Combastion Immerse the bomb in a cold distilled-water bath. Connect the terminals to the open

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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. Releasethe pressureat a slow, uliform rate such that tbe operation requires not less than I min. Open the bomb and examine the contents. If traces of unbumd oil or sooty deposits are found, discard the determinationard thoroughly clean the bomb before again putting it in use (Nore 3). - Do not ro nea!fie bomb NOTE8: Caution untilar le3st 20 s
alier firing.

6.5 Detennination of Suvur - Evaporate the combined washings to 200 mL on a hot plate or. other souce of heat. Adjus( the heat to maintain siow boiling of the solution and add l0 rol- of rhe BaCl2 solution, eittrer in a fine steam or dropwise. Stir the solution during the addition and for ? min thcreafter. Cover the beaker wilh a nuted watch glass and continue boiling slowly until the solution has evaporatedto a volume approximately 75 mL as indicated by a mark on the beaker. Remove rhe beaker from the hot plare (or other sourcc of hcat) and allow it to cool for I hr before filtering. Filter the supcrnatantliguid through ari ashless,quantitati{e filter paper (No(e 9). Wash the precipihte with water, first by dccantationand then on the.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 igniring it, and finally ignite at a bright rcd hcar unril (hc residueis white in color. After ignition is complere,allow the crucible to cool at roont temperarure,and wcigh.
NOTE 9 * A wciglrcd porcelain lihcr cnrciblc (Sclxs type) ol 5 1o 9-pm porosily miy bc used in plrce of rhc lllrer paper. In rhis case ths prcipit:rte is w:rslled frec of chloridc xnd rhen (lricd to const&|lt weight at 500 r ?5'C. NOTE l0 - A sa(isfirctorymeilns of drying, ch ring, tDd igniiing lhe piper and precipititc is to pLacethe crucible coahinir,g the $er liher papcr in a cold elcckic mufflc furrace and ro tum on rhe currel|t. Drying, chaning. and ignition usulll] will (xcur al rhe desircd rate.

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6.4 Collection oJSufur Solution- Rjnserhe interior of the bomb, the oil cup, and the inner surfaceof the bomb cover with a fine jet of water, and collect the washings in a 600-mLbeaker havinga markto indicate 75 nrl-. Removeany precipitate in the bombby means of a rubberpoliceman. Washthe baseof the terminals until the washings are neutralto the indicatormethyl red. Add l0 mL of saturatedbromine water to the u,ashings ([he volumeof the washings in the beaker. is normally in excessof 300 mL.) Placethe sample cup in a 50-mL beaker. Add 5 mL of saturated bromine water, 2 mL of HCl, and enoughwaterjust to cover the cup. Heat the contents otthe beaker to just below its boiling point for 3 or 4 min and add to lhe beaker containingthe bomb washings. Wash the samplecup and thc 50-mL beakerthoroughly with water.Removc any prccipitate in the cup by meansof a rubber policeman.Add the washingsfrom ahecup and the -50-nrlbeaker, and the precipitate, if any, to the bomb washings in the 600-mL beaker.Do not nlter any of the washings, since iiltering would removeany sulfur as insoluble t)rescnt material.
447

6.6 Blank * Make a blank determinltionwhenever new reagents, white oil, or otherlow-sulfurcombustible materialarc 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 tlle sulfur conten'iof the sample as follows: Sulfur, weight percent = (P - B)13.'l3lW where: P= gramsr.rfBaSOaobtainedfrom sample, B = grams of BaSOaobrrincd fron) blank, ard l,Y: granrsof santplcUscd,

E,

Report

8.t Report the resulls of rhe test to tfre niirest 0.0lVo.

sD-129 9, Precision and llias

2OOISECTIONV
1.5to 2-0 2,0ro 5.0 0.t2 0,18 0.25 o.2:1

Ll Tl)c precisionof this (est is not known to havc beeo obtained in accordance with currently accepted guidelines (for exanrple in Comrnittee D-2 Research Report, "Manual on Determining precision Data for ASTM Methods on Petroleum products and Lubricants"). 9.7.1 Repeatability- The difference betweentwo tcst results, oblai ed by thc same o;:crator with the salnc apparatusunder constant operating conditions on identical tesr material, would in the long run, in the nomral and coftcct opeEtion of the test method,exceed the follorving values only in one case in twenty. 9.1.2 lleprotlucibility - Tl.)e difference between two singleand indcpendcnt resultsobtained by different operators workiog in different laboratorieson identical test ntaterialrvould, in the long run, in the normalard corrcct operation oI the tcst mcthod. exceedtlre l-ollowurg values only in one case in twenly:
SLr lfur, wci!hr % 0.1 lo o--5 0.5lo 1.0 1 . 0r o 1 . 5

NOTE I I - Thc pr.rision sho*r in the abovc table dosnot apply to samples containingover 2% clrlorine because an addedreslricrion on the amoDntof samplewhich can be ignired is imposed. NOTE 12 - This tesl methodh.s beencooprntivcly tcsrcdonly in fte rnngeof 0.1 to 5.0%sulfur. NOTE 13 - The followioSirfofiarion on rhe precision of this methodhas beendeveloped by thc lnstitule of Petroleum(London): (a) Resulls of duplicatc iestsshouldnot differ by nrorc lhan rhe followinSamount!: Rcpatability 0.016 r + 0,06 Reproducibilily 0.03?x + 0.13

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where r is tha meaoof dupli4ate test resulls. valocswere obtaincdin 1960tJy statislicrl fr, Theseprecision examinstion of interlaboratory tes,tresults-No limirs have been esbblishEdfor additivc conceftrates.

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9.? Bias - Results obtainedin one laboratory by TcstMethodD 129on NIST Srandard Reference Marerial Nos. 1620A,1621C,and 16628 were found ro be 0.05mass7ohigherthanthe accepted reference values. 10. Keywords 10.1bomb;sulfur

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Jicpeatability 0.04 0.06 0.08

Reproducib;lhy 0.05 0.09 0.15

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STANDARD TEST METHOD FOR SULFATE ION IN WATER

sD-516
(Identical with ASTM D 516-90)

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1.

Scope

3.

Terminology

1.1This turbidimetric thedetermitestmethod covers nation of sulfatein water in the rangefrom I to 40 rnC/L of sulfateion (SO+--). 1.2 This test methodwas used successfully with drinking, ground,and surfacewaters.It is the user's responsibility to ensure the validity of this testmethod for waters of untestedmatrics, 1.3 Former gravimetric and volume.trictest methods' have been discontinued. Refer to Appendix Xl for historicalinformation. 1.4 This standard does not purport to address the saJetyconcems, if any, associatedwith its use. h is the responsibililyof the userofthis standardto establish appropriate safety and health practices and determine tlrc applicability of regulatgA limitafibns prior to use.

3.1 Defnitiotts - For defiritions of tcrms used in this test mcthod,rcfcr to Tenninology D 1129.

4.

Summery of Tcst Mcthod

4.1 Sulfate ion is convertedto a brrium sulfate undercontrolled A solutionconsuspension conditions. taining glyccrin and sodium chloride is addedto stabilize and minimize interferences. The resulting the suspension specbophoturbidity is determinedby a nephelonreter, tometer, or photoelectric colorinreter and compared to a curve prcpared from standard sulfate solulions.

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Significance and Use

2.

Rcferenced Dosrmenls

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2.1 ASTM Stdndards: D 1066Practice for Sampling Steam D 1129Terminology Relating to Water D I 192Specification Water for Equipment for Sampling ilnd Steamin ClosedConduits D 1193Spdcification for Reagent Water fot D ?'1"17 Practice Determination of PrecisionandB ias D-19 on Water of Applicable Methods of Cbmmittee D 3370Practices for Sampling ConWaterfrom Clo$ed duits E 60 Practicefor Photometricand Speclrophotometric Analysis Metbods for the Chemical of Metals E 275 Practicefor Describingand MeasuringPerformance Visible,andNearInfrared Spcctroof Ultraviolet, photometers

5,1 The determinationof suliate is important because it has becn reportcd that when tbis ion is prescot in excessof about 250 mg/L in drinking water, it causes a cathaflic action (especiallyin children) in the presence of sodium and nragnesium,and gives a bxd taste to the water.

6,

Intcrfcrcnccs

6.1 Insoluble suspcndcdmatter in thc sample musl be removed. Dark colors that can bc compcnsatedfor in the procedure intcrfere with the neasurenent of suspended bxriuin sulfirte(BrSOa). as low as I mg/l- will inhibit 6.2 Polyphosphatcs barium sulfate precipitation causing a negative interferprescnt in low concentrations,deence. Phosphcnatcs pendingon tlre type of phosphonrte, will also causc a negativeintcrfcrencc. Silica in excessof 500 mg/L

sD-516

2001sEcTIoN v 8,3 Barium Chloritle - Crystalsof barium chloride (BaCl2. 2H20) screened to 20 to 30 mesh. To prepare .in the laboratory, spread crystals over a large watch glass, desiccate for 24 h, screen to removeany crystals thatarenot 20 to 30 mesh, andstorein a clean,dry jar. - Place30 mL of concen8.4 Conditioning Reagent tnted hydrochloric acid (HCl, sp gr Ll9),300 mL water,100ml- 957oethanol and reagent or isopropanol ?5 g sodiumchloride(NaCl) in a container. Add 50 mL glyceroiand mix. 8.5 SulfateSolution, Sandard (l mL = 0.100mg SOr--) Dissolve0.1479 g of anhydrous sodium sulfate(Na2SOa) in water, and dilute with water to I L in a volumetricflask

may prccipitate along with the barium sulfatg causing a positive interfcrence. Chloride in excess of 5000 ngn- \+)11caus a negative interference, Aluminum, polyrners, and large quantities of organic material prescot in the test sample may cause the barium sulfate to precipitate nonuniformly, In the presenceof organic matter cefiain bacteria may reduce sulfate to sulfide. To minjmize thc action of sulfate reducing bacteria, samplesshould be refrigented at 4"C when the presence of such bacteria is suspected. 6.3 Alihough other ions normally found in water do not appear to interfere, the formation of the barium sullate suspensionis very criticat. Determinationsthat arc in doubt mry be checkedby a gravimetric method in some clses, or by the procedu.esuggested in Note 2,

7.

Appalatus

9.

Sampling

7,1 Pluno leter * One of the following, which are given in order of preference. 7.1.1 Nephelorneter or turbidimererl 7.1,2 Spcctrophoto,neterfcrr usc at 420 nm n'ith liilrr l)rth ('t'4 to 5 cn)l wi$ a violet lilter having 7.1.3 Filter photometer a nraxinrum near420 nm and a light path of 4 to 5 cm. 7.2 Stopv, cl\ if the magnetic stjrrcr is not equipped witl'r arl accuratts timer. 7.1 Measuring .Spool,capicity 0.2 to 0.3 mL. 7.4 Iriltcr photornctcrs nnd photonrctric pructiccs prcscribcclin {his test nrethodshrll conform to Practice practiccssltnll conform to E 601 spcctr{)photon'rcter PracticcE 275.

9.1 Collectthe samplein accordance with Practice D 1066,Specification D 1192,and Practices D 3370, rs applicable.

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10. Calibration givenio SectionI l, using 10.1Follow theprocedure appropriate amountsof the standard sulfate solutior, prepared in accordance with 8.5andprepare a calibration curve showingsulfateion contentin milligrams per litre plottedagainst the corresponding photometer readings(Note l). Prepare standards by diluting wirh water 0.0, 2.0, 5.0, 10.0,15.0,20.0,30.0,and 40.0 nrl- of standrd sulfate solution to 100-mL volumes in volul])erric flasks. These solutions rvill havesulfateion concentrationsof 0.0, 2.0, 5.0, 10.0, 15.0, 20.0, 30.0, and 40.0 m/L (ppm),respectively.
NOTE I - A scparatc ,.ialibration curve must tle prepared for each pholoDrclcr and a ,)rw curye murt be prcprred jf il ,! neccsstry n) changc thc ccll, lamp, or frltcr, or if any orlrcr akeftrtionsofi||strunrcnt or reagenlsare made- Check rhe curve wirh each serics of tests by running two or morc solutions of known sulfate concenfadons,

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lleagcnts

8,1 Pttitr oJ-Retgetts- Reagenrgradechemicals shlill l)c uscd in illl tcsts.Unlcss othcfwisc itrdicatcd, rl is rIrtcIl(1.(l tltirt illl reagcnl$sl)lll co|llbrnl to thc specilic tions ol the CoDlmittee on AnalyricnlReagents ol (he Amcrican Chcmical Society.Otlrergradesnay irc used,y>roviclcd it is first {sccdaincdthat the reaBent is ol suliicicnrly high purity to pcrn)ir irs use without lJsjJr)iu! !:lc uccuracyof the delcrutlinxtio,l. 8.2 l'utir.t ,,I lvatcr - Unlcis otlrr:rrvisc indicated, referenccs to u,atershallbe undcrslood to tneanreirgent wlltcr conibnrlinlt to SpccijictriorlD 1193,Type III450

11.

Procedure

1l.I Filter the srn)ple if ir is turbid, and adjusr rlre tenrperalureto betwcen 15 and 30"C11.2 Pipet into a 250-mL beaker 100 mL or less of the cle!. sample containing between 0.5 and 4 mg of sulfate ion (Note 2). Dilute to 100 mL with water if required, and add 5.0 mL of conditioning reagcnt (Nore l).

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ARTICLE 24 -

I,IQIJID PENETRANT STANDARDS

sD.s16

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NOTE 2 - The sotubiliry of BaSO. i6 such that difficulry may be experienced in thc deteaohatio[ of sulfatc conccntrationsbclov about 5 mg/L (ppm), Thb can be overcomc by colccntratint lhe sample or by adding 5 dtr of dtrlrdard $tlfatc-solutiol O mL = 0.100 mg SOr--) to thc taEplc bcforE dilutiDg to 100 mI- This will add O-5 mg SO,tto thc ssmpL. which mu$ bc subFrctcdfrom the frnal result.

1 TABLE ( SO) (5/) ANDSINGLE.OPERATOR OVERALL MEAN AGAINST DEVIATIONS STANDARD INTERLABORATORY F CONCENTRAT IO R N WATER'4 FROMREAGENT OFSULFATE RECOVERY
(X), lrlean Concentratlon mg/L
20.4 mg/L Deviation, Standard
JI

11.3 Mix in the stining aPParatus. 11.4 while the solution is being stirred, add a measuredspoonful of BaCl2crystals (0.3 g) and begin timing immediatelY. speed. 11.5 Stir exactly 1.0 min at constant
NOT! 3 - The sii.ring shouldhc at a consbnt rale in all delcrmin!_ r;ons- The use of a magnctic atfulcr hi.s becn found satisfactoryfor this purposc.

Ss
0.1 0.4

1-0 2.5

r Thetestmethod was at the63.9 level is linear to 40 mg/L Tesling in 11.2. as described accomplished thro!ghdilution

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afrrthe stirringperiodhasended, 11.6 Immediately th'turbidity pour soludoninto the cell and measure the maximum Record at 30-s intervals for 4 min. readingobtainedin the 4-min Period 1I.7 If the samplecontainscolor or turbidity,run ll.6 ll.2 through blankusingthe procedure a sanrplc without thc additionof the bariumchloridc. Cilutethe sample are susPectcd, 11.,3 If interferences \r'ith an equal volume of water, and determinethe again.If the valueso determined sullatcconcentration interferences is one half that in the undilutedsample, to be absent. lu)aybe assumed

2 TABLE 5O 0) (L S I )A N DS I N G L E . O P E R A(T R OVERAL E A N A G A I N S T M EVIAIIONS DD STANDAR F INTERLAEORATORY CONCENTRAT IO R N GROUND, FROMDRINI(ING, RECOVERY OFSULFATE A[D SU R F AE CW A T E R N
( )'), MeanConcentration mq/L 6.9 24.2 h3.3
I

0eviltion,n)!/L Standnrd

s"
0.7 2.2 4.5 0.5 1.8 1.6

T h et e s t m e t h o di s l i n e a r t o 4 0 n l g l l , T e s l i n ga t l h e 6 9 . 9 l e l ' e l$ ' 4 5 in I1.2. h r o u q hd i l u t i o n a s d e s c r i b e d a c c o m p l i s h et d

12. Calculation lvith obtained readings l2.l Convertthe pholometer thc sampleto milligramsper litre sulfateion (SOl--) 10. in Section curvedescribed by uscof the calibration

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observations at each lcvcl for relgent water and for matrix wrter (drinking, ground, and suriaca water). 13.3 Recovcries of known amounts of sulfate from reagent water ancldrinking, ground, and surface watcrs are as shown in Table 3. 13,3.1A tabte fot estimatingthe bias of the test mcthod throuilh its ltpplic:tblc concentration range can be found in Trlrlc 4. 13.3,2 These collaborativetest data were obtaincd on reagentgrtdc water and niltural waters. For other matrices, thcse dala may not aPPIY

13. Precisionand Bias in this test 13.1 The precisionand bias datapresented of Practice D 2777-86. method meet the requirements precision of the 13.2 The overallandsingle-oPerator with range, varies its designated within test method; I for Table to tested actording quantity the being reagent water and Table 2 for drinking, ground, and surface waters. in the round participated 13.2.1Sevenlabontories robin at threelevelsin triplicate,makinga total of 2l

14.

Keyrvords

14.1 drinking watet; ground wateri sulflrtel surfuce water; turbidimctric

451

DtilIlcl.

( ' r . f u / t , r tr cn q r t e r a n d w i t s l c w l l c J . Srtr,rplo cs ontainin" lrur)r ft) to 100 rlg/L sulfatc rnli I,c iujllyzed. * , . , , . : S l r r r r ci . .r\ I r ' c c i I r r r , , . ,.rr l ) . rw c r , , l l l c d r.).; l I l ' l n\lu l l i , , , . l l r c rr r . r , , f l l o r : i l i , r r, r r , lo t l r c r insolublc X1.1.4 'l'his

a o sD-5r6 2OOISECTIONV a TABLE 3 D E T E R M I N A T IO OF N TABLE 4 a BIAS4 *,',"1Tir1ijtii#..,i,iif,y"ilff fltil.'.,^^, a .AmountAmount FoR rNrERLABonaro Added, Found, . _?r-v^r.s.r.0ll.!!0wN ii R.qc-oveni oesur_rnrE mglL FRo mg/L M FJ^r"Tly :LrlL^ o REAGENT WATER AND DRINKiNG-, GROUND, AND SURFACE WATER, o Mean Surface (,11, Recovery Sufate ng/L Adde4ng/L Reagent Water( Sr) a MatrixWater(.ta) 7.O 20.a o 63.9 7,o o ro'y1--al,;lllffil]fiffi iigu-iiiiril;E ,cconrptished -lil,ll:Ji,I"..'"''.l ll"'.to ;"*:::::J:'l-"-1r:IT:'toqo'?uT"f, accomplished tt rorsh aitution fhroush dit"tio"u. aiririO"O'ii'rijl is d!s;r,;;;:;,ri:;l o o o a API'ENDIX a (Nonmandatory Information) o t1. o It r.lgIArE!.oRDrscoNt,rNuArroN Xl.2 Volunetric: 0Ir l\.lttT[toDS a Xl.l.l This lest methodwrs X7.l (iruvine t ic: discontinucd _. in l9tig. Thc. test method nray be found tn the lggg Anttual t., This.lcrt o nretl)oJ Book u a s t l i s c o r r r i r r u c d of ASTM Standarcls, in I9gg. _ " I , Vcl l l_01. fll* t"rt rlr"rflJi r , l c r ( . \ f n t c t n o dn r i l y b c f o u r ] d| t n c l g g i A t t n u u l was onginally issuedin 1959 as a non-referee metho( BrtoL ol A,ll'I4 Stqnrktrrls, a Vol ll.t)1. .l.ltcIcsr ntctho.l lhc prirnrry nrcrhod in rhc t9S0 lj:,j l':1.1" 'l'csl ijsrr. L)l *,irs or.j-qin!li-y issucij il J93lJ. Mcthod D 5i6 o T l r i s r c s tn ) r , r i r , ) cL ol \ . c : "t i , . ( j J t c l n i n r r i o n X-1.2.2 This tesr . )t,,..,
Reagenw i ater

20.8 63.94 7,0

D r i n k i n g ,g r o u n d and strface waler

Statisticay Significant at 5% Level lBias :%8i"s (ar : 0.05) -0,4 _1.9v" 20.4 No 63.7A -a.2 -0.2"/" NO -a.4 _5.30/6 6.6 No

20.8 6.gn

-0.6 _1.7V" 24.2 63.34 -0.6 -0.i./" 6,9 -0.1 _1.8%

l{o l!o No

6.6 (0.5) 20.4 (1.0) 63.7 (2.5)

6.9 (0.7) 20.2 (2.2) 63.3 Q.5)

methodcoversthe dcterrnir:r{iorr .. of sulfate in industrial water. San)ples contai.ningi;o;; 5 to 1000 mg/L of sulfate m0y be anatyzed.

tc.sr nrcrhodwas (trs(ontinucd because , Ilrcrc u('t-cir)suflicicllL labornt()rics ilt(!:rcsted in paflici_ l)ating iD lDothcr coll boraljvc srul]t), to obtajn the prccision and bias rs rcquirect by pracrice 11":lt:yy D 1111.

X1.2.3 Sulfalc i$ titratcd in an alcoholic . sollttiorr ur:oer controlled acid conditions with a stan<iard bariu|lr chloridesolution using thorin as fie indicator. X7,2.4 This test method was discontinucd . bccausc there wcre insuflicient laborarories interestedh p*i"lpating in another collaborative study to oUtuln tf.," necessaryprecision and bias as required by practicc
111'1

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452

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STANDARD .TEST METHOD FOR CHLORINE IN NEW AND USED PETROLEUM PRODU.CTS(BOMB METHOD)

ffi
l. Scope

sD-808

fill,

(Identicat with ASTM D 808-95)

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of 1.1 This test method covers the determination includingnew chlorinein lubricatingoils and greases, containing addiand usedlubricatingoils and greases Its range of applicatives,and in additiveconcentrates. assumes bility is 0.1 to 507ochlorine.The procedure containing halogens otherthanchlorine that compounds will not be present. units arc masspercentand SI. 1.2 The preferred 1.3 This standud does not purport to address all c.,fthe safety concems, if any, associatedwith its useIt is tlrc responsibility of the user of this standard to establish appropriate sdfety and health practices and rlerennine the applicability of regulatory limitations
PrQr to u|e.

Safct! Slrict adherence lo all of lhc NOT l: (Ceution provisions prescribed herciniftcr 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 dsirable, however, tbat the bomb bc ncloscd in a shield of stel plate at lasi l3 mm (% in.) thick. or equivirlenl protcction he provided agsinst unforseeablcconlingeDcics.

4.

Significancc and Usc

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4.1 This test method nray be used to measure thc level of chlorine-contairing compoundsin petroleum products. This knowledge can bc used to Predict performance or handling chlracteris(ics of the product in questioIl.

5.

Apparatus

2,

Refcrenced Docurnents

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2.1 ASTM Standards: D 1193 Specificationfor ReagentWater D 4057 Practicefor Manual Sampling of Petroleumand Ircrrolcum Products

3.

Summary of Test Mefliod

5.1 Bonb, having a crrprcity of not lcss thrn 300 n]L, so constructed that;t will rot lerk during the test, recovcryof the liquids from the and that quantitative ''l'lre inner surfaceof bomb m y be readily ichicvcd. slcol or any otber the bonrb may be nradcof stainlcss materialtlrxt will nol bc offcctcd by thc cornbustion proccss or products. Mrt(:riirlsuscclin thc bontb assctnbly, such ls thc hcrd grsket:tnd lerd-wire insulation, lction, and shall to heatand c)rcmical shall be resistant not undergoany reactionthlt will affcct the chlorine Jontentof the liquid in the bomr.r. 24 nrnrin outsidcdian'rctcr 5.2 SanpleCap,platinum, at thc bottom,2? mm in outsidc dianretcrat the top, l 2 m m i n h e i g h to u t s i d c r , n d w c i g h i n g1 0 t o l l g . 5.3 Firing lVlre, phtinunr,No- 26 B & S gage 0.41 (16 thou),27 SWG or cqrrivrlcnt. 453

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3.1 The sample is oxidized by combustionin a bomb conraining oxygen under pressurc (Caution - See Note l). The chlorine compoundsthus liberatedare solution and the amount rbsorbed in a sodium carbonate of chlorine present-is determined gravimetrically by DreciDitationas silver chloride.

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sD.80lJ :OO; SECTION V

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TABLE I QUANTITIE OS FS A M P L A E N DW H I T E OIL

5-4 lgnitiott Clrrair, caprLblq of supplyingsufficicnt cuffent to ignite the nyJon thread or cotton wicking wrthout nlelliDg the wirc'I'he 5.4.1 switch in thc ignition circuit shall be ol a typc lhat rcntains open,exceprwhen hcld in closed position by 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,

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Chlorin Content, . % Weighr. g Weighrof Whire Oit, q of Sample, 2 and under 0.B 0.0 Above 2 to 5, incl 0.4 0.4 Above5 to lO, incl o,2 0-6 Above10 to 20, incl 0.r o.7 Above 20 to 50, incl 0.05 0.7

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6,

Rexgents and l\.Iatcrials

6.1 Puritl, of Reagent:;- Reagentgrade chemicals shall bc used in ail tests,Unlessotherwiseindicated, rt rs rntendedthat all rcagenCs shall conform to the specifications of the Comlnittec on AnalyticalReagelts of the American Chernical Socicty, *treie suctrsplln_ catio s are available. Otlrer grades may be used', provrdcd it is lirst asccrtained that the reagent is of sufficienrlyhigh purity to permit its use without less_ ening the accuracvof tbe detcmination. 6.2 PuriD. of Water - Unless otherwise indicated, rcferencesto tvafcr shali be understoodto mean reagent waler as dcfined by Type II or III of Specification D I193. 6.3 Nlrric Acil (l + I) - Mix equal volumes of conccnrratcd nitric acid (JjNO1.sp gr 1.42)and water. 6.4 Otlgru. ilcc olcornLru,rible marcrial rnd halogen compoulcls,avaihblc at a pressure of 4t tgf/cm, i40 atnros).(Wxr-ning - Scc Norc 2.)
NO'rE 2: l\,arning Orygen vigorously accelcratcscombuslion.

of the sampleused for the test is thoroughly representative of the whole sample.

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8.

Procedure

Preparation of Bomb and Sample _ Cut a piece ,8,1 of firing wire approximately t00 mm in lensth. Coil rhe middle section (abour 20 mm) and attach the free ends to the terminals. Arange the coil so that it will be above and to one side of the sampte cup. Insert into the coil a nylon thread, or wisp ofiotton, of such length that one end will extend into the sample cup. Place about 5 nrl- of Na2CO3 solution in ttre tonib and by means of a rubber policeman, wet the interior surface.of the bomb, including the head, as.thoroughly as possible.Introduce into the sample cup tl,e quantitles of sample and white oil (Notes 3 and 4) specif,ed in Table I (Caution - Note 5), weighing the sample to the nearest0.2 mg. (When white oil is used. stir tlre mixture with a shon length of quaftz rod and allow the rod to remain in the sample cup during the combustion.) 8.1.1 After repeateduse of the bomb for chlorine determination, a film may be noticed on the inner surface. This dullness can be removed by periodic polishing of the bomb. A satisfactorymethod for doing this is to rotare the bomb in a lathe at about 300 rpm and polish the inside with Grit No. 2/0 or equivallnt pepercoatcdwith a iight machineoil to prevcni cuuing, and then with a paste of grit_free chromic oxide and water. This procedure will remove all but yery deeo pits and put a high polish on the surface.Aefore usini the bomb wash it with soap and warer to remove oil or paste left from the polishing operation. Bombs with porous or pitted surfacesshould never be used becausc of the tendencyIo retain chtorine fronr sample to sample. 8.1.2 When the sample is not readily miscible with white oil, some other nonvolatile, chlorine-frce combustiblediluent may be employed in place of white

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6.3 Silter Nitrete So/utiot (50 g AgNO3/L) _ Dis_ solve 50 g of silver nitrare (AgNO3) in water and dilulc to I L. 6.6 Sodiun C(!rbonarcSolution (50 g Na2CO3/L)_ Dissolve.50g of anhydrous NarCO3. 5g.5 g of NarbO, H1O, or 135 g oi NaICO-I. i0 H2O i,r *ot"i aui dilurc ro I l-. 6.'1 llhirc Jil refined.

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Surrrplin! 7.1 'l'akc sln'tplcsin lccodllnce with the iostlgctions in Placticc D .1057. 7.? T|ke carc Ihirtthc srlDplcjs thoroughly rcprcsenta_ . trvc of the ntiltcrinl to bD rcstcdand lhat the poftion

7.

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ARTICLE 24 _ LIQUID PENETRANT STANDARDS

sD-808

TABLE 2 GAGE PRESSURE

Capacity of Bomb, mL
300 t0 350 350 to 400 400 to 450 450 to 500

Milimum Gage Maxinum Gage Ptesure,, kgf/cmz Presure,'kgflcrn2 (atn) - . (ah)

39 (38l 36 (35) 3I /.JO' 2a (21)

4r (40) 38 (37) 33 132) 30 129'

the interior of the bomb and the inner surface of the bomb cover with a rubber policeman. Wash the base of the terminals until the wastrings are neuaal to the indicator methyl red. (The yolume of the washings is nomally ir excess of 300 mL.) Take special care oot to lose any wash water. 8.5 Detennination of Chlorine - Acidify the solution by adding HNO3 (1 + l) drop by drop unril acid to methyl red. Add an cxccss of 2 mL of the HNO3 solution. Filter through a qualitative paper [if tbe solution is cloudy, thc prescnccof lead chtoride (PbCJ2) is indicatedand the.solurionshould be brousht to a boil before filteringl rnd collecr in a secondi00-mlbeaker. Heat the solution to about 60'C (140.F) and. while protecting the solution from strong light, add gradually,while stining. 5 nrL of AgNO3 solution. Heat to incipient boiiing and retain ar this temperature until the supernatant Iiquid bilcomcs clear. Tcst to ensurecomplc(eprccipilalionby xdding a few drops of the AgNO3 solution. If nrore precipitation takes place, repeat dre above steps which have inyolved heating, stirring. and adCirion of AgNO3, as often as necessary, until thc additionrl d.aps of AgNO3 produce no turbidity in the clcrr, sulernatrntliquid. Allow rhe beaker and contents to stand in a dark Dlace for at lcast an hour. Filter the prccipitrrte by slcrion on a weighed fritt'ed-glass filter cmciblc. Wash the precipitate with water containing2 nL of HNO3 (l + 1)lL, Dry the crucible and precipitate at ll0'C for I h- Cool in a desiccator,and weigh. E.6 Blank - Make a blank detennination with 0.7 to 0.8 g of white oil by following the normal procedure but omitting the sample (Notes 6 and 9). Repeat this blank wheoever new batches of reitgentsor white oil afe used. The blank rnust not exceed 0,03% chlorine basedupon the weight of the white oil.
NOTE 6 - llis procedure measureschlorine in lhe while oil and io th rcrgents used, as well as thar inkoduced from conramination.

" The minimumpressurcs are speclfied tQ providesufficient orygen for complete combustion, and the maximum pressuresrcpresent a safety requiretuent.

oil. However, the combinedweight of sampleand nonvolatilediluent shall not exceedI g. Somesolid additives are relativelyinsoluble, but may be satisfactorily bumed when coveredwith a layer of white oil.
NOTE 3 - The practice of running altedarely high ard low samptes in chlorine content shall bc aroidcd whenever possibla, It is difficulr to .inse lhe last traces of chlodne from thc walls of the bomb and Lhe tendency for residual chlorinc to carry over from sample to sampie has been observed io a number of laboratories. When a sample high in chlorine has precedcd one low in chlorine contcnt, lhe (est on the low-chlorinc sample shnlJ be repeated and one or both of the low values thus obtnincd caq be consideredsuspec( if 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 sarnple lnd whi(e oil or other chlorine-ftec comburtible matcrbl.

8.2 Addition of Oxygen- Place the samplecup in position andarrange thenylonlhread, or wispof cotton, so that the end dips into the sample.Assemblethe bonlb and tighten the cover secudy. Admit oxygen (Caution - See Note 8) slowly (to avoid blowing the oil from the cup) until a prcssure is reached as indicatedin Table 2.
NOTE 5: Caulion - Do not add oxyge[ o! ignilc rhe sampleif lhe bomb ha9 been jaficn, dropped,or tiltcd.

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8.3 Combustion- Immerse the bomb in a cold water bath. Connectthe terminals!o the openelectrical circuit. Close the circuit to ig[ite the sample. Remove the bomb from the bath after immersion for at least l0 min. Releasethe pressureat a slow, uniform rate such that the operation requires not less than 1 min. Open the bomb and examine {he contents. If tracesof unbumed oil or sooty depositsare found, discard the determination, and thoroughly cleanthe bomb before againputtingit in use(8.i.1). 8.4 Collection oJ Chlorine Solution - Rinse the interior of the bofnb, the samplecup, and the irner surfacedf the bomb cover with a fine jet of water, and collect the washings in a 60GmL beaker.Scrub

9.

Calculation

9.1 Calculatc the chlorinecontentof thc sampleas follows:

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

where: P= grams of AgCl obttrincdfrom the sample, 8= grams of AgCl obtained lrom the blank, :rnd W= gramsof sampleused-

2001 sEcTroN v
10. Precision and -llias

10.1 The precisionof this testmethodis not hiown to hilvc been obtailed in accordance witfi cunendv rcceprcd guidclincs (for crample, in CommitrceD_i ResearchReporr RR:D2-100?, Manual on Dererminins Precision Dltl lbr ASTM Methods prod_ on petroleum ucts and Lubricants). 10.2 The precision of this test method ts obtained. by statistical exanination of interlaboratorytest results is as follows: 10.2,1 Repeatability - The difference between successryetest results obtained by the same operator with rhc samcafnar tus underconstant opcrating condi_ tions on identictl test mate al would, in the long run, in the normal and conect operationof the test niethj cxceed the following r,alues only in onc casein twenty:
Chloripe,./c . 0-i ro I.9 2.0 lo 5.0 Abovc5.0 Repea(ability 0.0.1 0,t5 3% of amovDlpresent

two singleandindependeDt results obtained by differenr operatoru workingin differcntlaboratories on identical test material would, in the long rua, in tbe normal anrl correct operation of thetestmethod exceed the foltowing values only in one casein lwenty:
Chlorine, %

0.1ro 1.9 2,0to 5.0 Above5.0 lO.3 Bias:

Reproducibility 0.10 0.x0 5%of smouitpresent

103.1 Coope&tive data;ndicate tbat deviationsof test rcsultsfrom the true chlorineconfent_are.of the sameorder of magnitudeas the reproducibility. 10.3.2It is not practicable to specifythe bi4s of this test methodfor measuring chlorine because the responsible subcommittee, after diligent search,was unableto attract volunteers for an interlaboratorystudv. 1I. Keywor&

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10.2.2 Raproducibili4, -

The difterence between

11.1 bomb; chlorine

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STANDARDTEST METHOD FOR

SULFTIR IN PETROLEUM PRODUCTS

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(HIGH.TEMPERATUREMETHOD)
sD-1552
(IdeBticalwith ASTM D 1552-95)

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3.

Summary of Test Method

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1.1 This test methodcoven threeprocedures for the determination of total sulfur-in peffoleumproducts including lubricatlngoils containing additives, and in additiveconcentrates. This lest method is applicable to samplesboiling above l7?'C (350.F) and containing not less than 0.06 mass% sulfur. Two of the three procedures use iodate detectio.n: one employing an induction fumace for pyro$sis, the other a resistance fumace.The third procedueuse$ IR detectionfollowing pyrolysisin a resistance fumace. 1.2 Petroleumcoke codtainingup to 8 mass% sulfur can be analyzed. 1.3 This standard may involve hazardous,nnterials, operations, and equipment. This standard does not lrurpon n address all of thz safety concems, if any, associated with its use. It is the responsibility of the user of tltis standard to estoblish appropiate safety awl health practices and determinethe applicability of regulatory limitatioru pior to use.

3.1 lodate Detectiort.lyste,'r- The sample is burned in a sream of oxygen at a sufliciently high ternpcrrture to conven about 97% of the sulfur to sulfur dioxide. A standardiz-a(ion factor is employed to obtain accuritte results.Thc combustionproducts trc passcd into an absorber containing an acid solutionof potassium iodide and starch- indicator, A faint blue color is developed in the absorber solution by the ,ddilion of starrdard potassium iodate solution. As combustion proceeds, bleaching the blue colo( more iodate is added. The aDount of standardiodateconsumedduring the combustion is a measure of the sulfur content of the santple, - Tbe sanrple is weighed 3.2 IR Detectiort System into a special ceramic boat which is then placed into a combustion furnace ar l37l'C (2500'F) in an oxygen atmospherc,Most sulfur preseot is combusted to SO2 which is then mealured with an infrared detector after mois(ure and dus( are removed by traps. A microprocessor calculates dle mass percent sulfur fron the sample weight, the integrard detector signal, and a predetermined catibration factor. Both thc sxrlrplc iden(ifica(ion number and mass pe.cenl sulfur ate. then printed out. The calibration factor is detenrrincdusing standlrds approximating the marerial to be lnalyzed.

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2. Referenced Documents '

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2.1 ASiM Standards: D I 193Specification for Reagent Water D 1266 Test Method for SuIfur in PetroleumProducts (LampMethod) D 4057 Practicefor ManualSamplingof Petroleumand Petroleum Products
45'7

4.

Significancc and Use

4.1 This test methodprovidesa meansof monitoring the sulfur level of various petroleum products and additives. This knowledge can be used to predict pcrformaoce, handling, o. processing propenies. In some casesthe prcscnceof sulfur cornpoundsis bcncficial

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2OOISECTION V to rhe productand monitoringlhe depletionof sulfur can provide uselul inforntltion. In orher cases th: presenccof sulfur cornpoundsis detrimentalto the or use of the l)rodrrcl. Drn(c)5inS

I 0
Secondary heatet

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Interlercnccs

Vycor tube

5.1 For the iodatesystents, chlorinein concentations less thair I mass 96 does not interfcre. The IR systen can lolcriLte sonrervhat highcr concentrations. Nitrogen when present in excess of 0.1 ruass 7o may interfere with thc jodate sysrems;thc extent of such interference may bc dependent on the type of nitrogcncompound as wcll as trte combustionconditions.Nitrogen does nol inrerfere widr the IR system.The alkati and alkaline eanh netals, as rvell as zinc, phosphorus,and Iead, do not intcrrerewith ejther systenl.

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6.

Apparatus 6.1 Cotnbtrstiottand lodate L)durio srstetn

F I G .I

COMBUSTIO TU NB E

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6-1.1 Funtttces - Trvo ntljor rypes are available, (he p.intary differcncebeing the rnrnner in which the necessury higlt ternperutures ale ohtoined.These two types arc as follows: \ 6.1.1.1lnductionT)pc, which dcpencis upon the high-frcqucncy clectricalinductionmethodof heatilg. This asseltbly shall bc capableof a aining a temperature of at least l4g2"C (2'100"F) iD tho sample combustion zone, undcr lhe conditionssct /br(h in Sectionl0 and shall lrr: crlL:ippctl wirh rrrr irrili:ionirl induction coil locatcd al']ovc Ll)e corrbustionzonc, substantiitlly as showniu Fig. I. 6.1.1.2 Thc furnace rvork coil should have a mrriDun) outprt of 500 W; (he ntinimum input rating of thc I'urnlcc nlust bc 1000 W. With thc conect anronnt oi iran chips,weighcdto:!0.05 g, thc nraximum pla{e currc)nt *,ill bc betweenj50 and 450 mA.
N O T E l : l \ ' r r r n i | l g - - f t r i s r y p c o t n r n r r c c i s c r p a b l eo f i n f l i c r i n g hi-qh frcqu.ncy Lrums rJrd high-\'ottrge shocks. Ilt addirion ro otbei piccnutions. mrinr;rin all gurrds properly. prccxution - Disconnect lhc fum?cc fro the line whenevcr clectrical repa;s or ' n d i u s t m c n tri r c n r r d c . fower

NOTE: - Also suirablcfor use *irh ei{herrype of furnaeris i.r automalictirraror,specifically designedfor iodometry,This combjnes the funclions of absorptiolandtiration !o a predetermined eodpoint.

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6.1.3 Buret, st.lndard 25-mL or automatic types availablc from thc manufacturcrs of the sf,ccificcort)l stio$ units, are suitable (Note 2).

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6.2 Combustionand lR Detection.syrreri, comprised of auiomatic balance, oxygen 0ow contols, drying tubes, combustion fumace, infrared detectorand microprocessor.The fumace shall be capable of maintaining a nominal operating temperatureof I350.C (2460.F). 6.3 MiscellaneousApparalas - Specific combustion assembliesrequire additional equipment such as crucibles, combustion boats, crucible lids, boat pushers, separator disks, combustion tubes, sample insetters, oxygen flow indicator, and oxygen drying trains. The additional equipment required is dependenton the type of fumace used and is available from the mnnuf4q1x... of dre specinc combustion unit. To attain the lower sulfur concentration given in Section l, the ceramics used with the induction fumace rssembly shall be

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6.1.1,3Resistattct i..tpc,capabJe of naintaining a ternpcr:rtrrrc oi ar lcmL 1371"C (2500"F). 6-1.2 Absorher, as dcscribed in Test Method D 1266.

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ARTICLE 24 _ LIQUID PENETRANT STANDARDS

sD-1552

ignitedin a muffle fumaceat l37l.C (2500"F)for at least4hbeforeuse. 6.4 Sieve,60-mesh (250-mm).

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7.7t Potassiton lodare,StandardSolution(0.01248 M, I mL = 0.2 mg S) - Measure exacrly200 mL of KIO3 solution(0.06238M, 1 mL = I mg S) inro a l-L volumetric flaskanddilute to volumewith water. Thoroughlymix the solotion. 7.12 Ascaite, 8 to 20 mesh. 7.13 SpecialMatcrials for lruIuction"TypeFurrlc"s, 7.13.1Tin (20 to 30-mesh). 7.13.2lron-ChipAccelcrotorhavinga sulfur content of not more then 0.005 mass7o.

Reagents and Materials

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:-- Reagentgrade chemicals Z.t,ipur;ty of Reagenti shall be usedin all tests.Unlessotberwise indicated, it is intended that all reagentsshall conform to the specifications of the Committeeon Analyical Reagents of the American Chemical Society, wheresuchspecifications arc available.Other gradesmay be used, provided it is first ascertainedthat the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy of the determination. 7.2 Purity of Water - Unless otherwiseindicated, references to watershallbe understood to meanreagent water as definedby Type II or III of Specification D I193. 7.3 Ahtndnn (4120) or MagnesiunOride (ComAid). 7.4 Anhydrone (MagnesiumPerchlorate).
NOTE 3i Prccaulion - ln additiotr to olhe! prccaurioos,handle mngnesiumpercltoratc with carE.Avoid contacringit with acid and ' organic materials.Rcactio$ rdth fucl may bc violenl

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- Porassium 7.14Standard Santplc alunl [AlK(SOa)2

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7.15 Starch-Ioelide Solution Make a paste by adding 9 g of soluble starch ro 15 nrl. of water. Add this mixture, with stirring, to 500 mL of boiling watcr. Cool the mixlure, add 15 g of potassium iodide (Kt), and dilute to I L with watcr. 7.16 Sul/uricAcitl (rclltivc dcnsity J.84)trated sulfuric acid (l I?SOa). Concen-

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NOTE6: Wsrning- Pois.ir. Corrosive. S{roDg oxidizer.

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7.5 Hydrochloic Acid (3 + 197) - Dilute 30 mL of concentrated hydrochloric acid (HCl, relative density l.l9) to 2 L with waler.
NOTE4: Wsrning- Poison. Con6ivc. May befatalif swallowed. t-iquid and vaporcausc scvarc bult|s. 7.6 Oxygen (Extra Dry) - The oxygen shall be at least 99.5ol pure and show no detectable sulfur by blxnk determination. NOTE5: Warnlng- OxygFn vigoaously accclerates combustion. 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) - Dissolve 2.225 g of porassium iodate (KIO3) that has been alried at about 180"C to constant weight, in water and dilute to I L. Thoroughly mix the solution. '1.10 Potassium lodate, Standard Solution (A.fi6238 M, I mL = 0.1 mg S) - Measure exactty 100 mL of KIO3 solution (0.06238 M, I mL = I mg S) into r l-L volunretric flask, and dilute to volume with water. Tlroroughly mix the solution. 459

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7.17 Vqnadiunt Pentoxide, anhydrous, powdered

. 8.

Sampling

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8.1 Take samplesin accordancewith the instructions in Practice D 4057.

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9.

Preparation of Apparatus

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9.1 Induction-TypeFurnace - Assemblethe apparatus accordingtc the instructionsfurnished by the manufacturcr. Purify the oxygen by passing it rhrough (.1) H2SOa(relative density 1.84), (2J Ascarite, and./J) magnesium perchlorate [MS(ClOq):] or phosphorus pentoxide (P2O5)(Precaution - sce Note 3). Connect a rotameterbctweenthe purifying train and the fumace. Insert a small glass-woolplug in thc upper end of the glasstubing connec(ing Lhc furnacc wjlh the absorber to catch oxides of tin. Connect rhe exit end of the combustiontube to the absorbcr with glass tubing, position usingguni nrbbcrtubing to nrlkc connections, the absorber so xs to ntakethis dclivcry line as shortas

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Absorbet

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F I G .2 S C H E M A T I C I L L U S T R A T I OO NF INDUCTION.TYP FE URNACE

FIG. 3 S C H E M A TT IC L L U S T R A T IO OF N RESISTANCE.TYPE FURNAC E

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SAIIPLE W E I ' H TF O R RESISTANC ERNACE FU TAB L E1 SAlv'IPLE WEIGHTFOR INDUCTION FURNACE

!Veiqht of Sample S]llflr Content,'/o to Be Taken,mg
0to2 2 I a 4 41o10 over 10

Nornrality ol StandarC KI03Solution for Titration 0 , 0 0 53 28 0.006238 0.01248 (Note 7)

Normalityof Sl,andard Weightof Sampte K[03Solution for Sulfur Content/ 7o to Be Taken,mg Titration 0to2 2lo5 5tol0 overl0 100 to 200 100 to 200 100 to 200 (Note7) 0.006238 0_01248 0.06238 (N o t e 7)

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90r 50 to 90 50t0 90 12.1.1

drops of the appropdatestandarclKIO3 solution (Table 2) to producea faint blue color. Adjust tbe buret to zero. possible. Figure2 illustrares schelrliltically theassembled lpprralus. Adjusr.he oxygcn fiow to I r 0.05 Umin. Add 65 nrl- oi HCI (3 + 197) and 2 mL of srarchiodidc solutionto thc absorbcr. Add a sufocient amounl ot the npproprirle srandardKIO3 solurion (Table l) to produce a frint blue color. This color will serve as the cnd poilt{ lbf the titration.Adj[st the buretto zero. Turn on thc lurnacelllamentswitch and allow at least I min wrrnr-up belbrc runningsamplcs (Precautionscc No(e 3). 9.2 Resistouce-'I yte Il.rt.tcc - Asselnblcthe apparatus {rccording to the instructions furnished by the manutlc(ufcr. Purily thc oxygen by p;rssing ir througb (^l) ll25Oa (rclarive dcnsiry 1.84). (2) Ascarite,and (J) Mg(CIO{): or P?Os(Precaution - seeNote 3). Connecr a rotan]ctcr bctweeI the puriiying train and the fumace. Figure3 illustrates schernatically the assembled apparatus. Turn on thc cuoent itnd ildjust ihe furnace control to nrlintirin it constlLnt tcntperature, oi l3l6 + t4"C (2400 l 25"F). Adjust rhe oxygen llow rate to Z a 0.1 L/min. AJd 65 ml- ol- FlCl (3 t I97) .rnd 2 nrl ol sturch-iodicle solution to thc rbsorbct.Add a few 460 " ,.3 Resistance-Ttpe Fumace-IR Detectioa - Assemble and adjust apparatus according to manufacturer's ins[ructions.Initialize microprocessor, check power supplies, set oxygen pressure and flows and set furnacc temperatureto l37l'C (2500"F). 9.3.I Condition a fresh anhydrone scrubber with four coal samples. 93,2 Calibrate the automatic balance according to manufacturer's instructions.

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10.

Standardization

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10.1 For lodate Methods: 10.7.1 Determination of Al.un Factor: 10,1.1.1 Becausethese rapid combustion mcthods involve the reversiblereaction 2SO2 + 02 = lger, it is not possible to evolve all the sulfur as SO?. Thc equilibrium of the reaction is temperature depcntlent and, in an oxygen atmosphere above l3i6"C, about 9'7o/o of the sulfur is prescn[ as SO2, To assure that the furnaceis in proper adjustnlentand that its operation

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

sD-1552
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prod_uces acceptablyhigh temperaturc, potassiumalum is eriiployedfor standardizing the apparatus. Depending on thd type of combustiorr.equipment used,proceed as descfibed in Sectionsl0 tb 13 to determine the alum factor. Use tS mg weighirdto *0.1 mg of potassium alum for this determination Usethe samematerials in thedetermination of tbealumandsundardiz:atior factors rs for the unknownsamples. For example, V2O5has a definiteeffect and shouldbe includedif used for unknowns as recommended in the procedure with the rcsisrxnce-type fumace(Note l0). 10.1.1.2C^lculate the alum factor as follows: Alumfictor(/F) = (glxWal[tm(V"- V) x ctl (t)

Strandardization factor(F,) = (S, * W")I[OO(L -V)xCt

wnetp: ' 'S,= mass percent sulfur in standddization sample used, I/, = milligrams of standardizationsample used, Vr= millilitres of. standardKIO3 solution usedin the blank determination. %= millilitres of standardKIO3 sclution used in determining the standardizationfactor, and C= sulfur equivalent of the standardKIO3 solution used in determining the standardization factor, mg/mL. 10.13 Quality Control - Piun a suitable analytical quality control sample several times daily. When tbe observed value lies bctween acceptable limits on a quality control chart, proceed r,vith sample dcterminahons.

where: S^= masspercent sulfurin potassium alum used, = milligrams IV,e of potassium alum used, y.,= millilitres of srandarrd KlO3 solutionuscd in determining thealumfactor, y, = millilitresof standard KIO3solution used in the blankdetermination, ard Cr= sulfurequivalent of theshndardKIO3solution usedin determiningthe alum factor, mg/ml. 10.1.1.3 The alumfactorshouldbe in the ranse from 1.02 to 1.08.If valuessmallerthan 1.02 aie obsewed, confirm independently the sulfur contentof the alum and the sulfur equivalent of the KIO3 solution beforerepeatingthe alum factordetermination. If values larger than 1.08 are observd make adjustments in the equipment in accordance with the manufacturer's recommendation ald repeatlhe alum factor determination. 10.1.2Determinationof Standardization Factor: 10.1.2.1 Because effects such assample volatility can also affect the daaive rccovcry as SO2 of the sulfur originally presentin the samplq it is necessary to determin a standardization factor. koceed as descdbedin Sections10 to 13, using an oil sampleof similar tpe to the unkrown sample and of accurately known sulfur cgntent. 10.1.2,2For IR detection, determine and load the microprocessor with the calibration faclor for the particulart)Te of sampleto b analyzed(ubricating oil, petroleum coke,residual fuel) as recommended by tbe maflufacturer. 10.1.2.3Calirilate the standardization factor as lbiiows:
461

ll.

Preparation of Coke

11.1 It is assumed tbat a representative samplc has been received for analysis. U.2 Crind and sieve the sample receivcd so as to pass a 60-mesh (250-mm) sieve, 113 Dry the sieved material to constant weirht ar 105 to I lO'C.

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12.

Procedure With Inducrion-Type Furnace

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- Add a 3.2 ro 4.8-mm ,l2.l Sanple Preparation (7r to Zr-in.) layer of alundum or magnesium oxide to a sample crucible. Make a depression in the bed with the end of a stiring rod. Weigh the crucible tq 0.1 mg. Weigh into the depressionthe pnoper amourt of sampleaccording to Table I (l2.l.l) (Note 7). Cover the sample with a separator disk (Note 8. place on th separator disk the predeterm;nedamount of iron chips necessary to obtain the required temperature (6.1.1.2).This is usually between 1.2 and 2.0 g, but should be held constant with 10.05 g. Sprinkle about 0.1 g of tin on the iron. Cover the crucible with a li<t and place on the fumaca pedestal 12.1.1 Under no conditions shall an organic sanrple larger than 100 mg be bumed in'an induction-type fumace,
nr' soludon, may be found .norc .o vedenr t6r ssmrtcs c.,nr.]iflifls

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NOTE7 - Moreconceoliled KIO] solulions, such asthe0.06233

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sD-t552
2001 SECTIONV

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r ,'rc $ullur. llle samplc sitr in,l KtOl concentrarion .rfixn .10% sr,c,utdbc chojcn so rhnr not more thrn 25 mL of tilr3nl is oceded. NOTE 8 Thc lJs of lhe sepaFror disk j! oprional.

14. Procedure With ResistanceFurnaceIR Detection 14,1 Allow the system to warm up and the furnace to reach operating temperature. of the sampteis assured, -14.2 After homogeneity selectthe samplesize as follows: for liquid samples, take up to-0.13 g for analysisand for solia samples, ta.ke up to 0.4 g for analysis.In eachcase,masspeicenr sulfur times weight of samplemust be less than or equalto four in the caseof the SC32instrumen!and two in, the caseof the SCl32 instrument. For other rnstruments,,. consultthe manufacturer's instructions. 14.3 Determine and storethe systemblank value. f4.4 Weigh the samples into combustion boatsand record the net weights.It. is possibleto weish and store seveftl weights in the microprocessor before beginninga seriesof bums. f4.4,1 Filt thecombustion boatto one-third capac_ ity with evenlyspreadMgO powder. 14.4.2Form a slight trenchin the MgO powder .. with a scoop.

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72.2 Cotnbustiortand Tiffatiotr _ Tum on the plate cunent switch. After about.l min for warm_up, iaise the-pedestaland lc,ck into position. The plate cunent will fluctuate for a few secondsand should gradually nse to a nlaximum value. Add the approprif,testandard KIO3 solurion (Table l) to the absorber io maintain rl)c blue color. Should thc absorber solution become conlpletelycolorlcss,discardrhe delermination. Make KlOq 1al6li1i611* as the m(e of evolutionof SO3 dinrin_ ishes such thar, when combusrion is compleied, the jntensiryol.rhe blue color is thc same as the initial intcnsily.Combus(ionis completcwhen this color renrains for at least I min and the plate current has dropped cor)siderably, Record the volume of KIO3 solution required to titrate the SO2 evolved. 12.3ljltuk Derernirrnlion _ Make a blank detemtina_ tion lvlrcnevcr a new supplyof crucibles, materials, or relLgcn(s is uscd, I.bllow tl.leprecedinEl proccdure, but 0fitt the siluplc.

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Proccdur.eWith lksistltncc-.fypeFurnace

13.1Srlrryr/c /'reltert i()tt -,Wcigh into a colnbustion boal lhc pfopcr a|tou|t ol-slinple uccordingto Tab]e 2. Add 100 t -5 mg of vanrdiunrpentoxide and com_ p)ctclv covcr lhe rnixturc rvirlt Alunclurn. 13.2 Coutbustionand Titntrion __ place thc boat in the co()l lr(Jfti()!) ol' the conlhustiontube, ncar the cntrancc. Ib pnrcccclwith thq conlbLrstion, push thc Lroitt corlLirinilur the slLnrple progrcssively into tle honer z-onc ol lltc con)bustiontubc using thc equiplnent provitlcd by tlrc nranuiacrurcrs. l.he bort should be advarceci as ftrjridlyas possjble consistcnt with the rate ol.evolulionol SO2.Add rhe rppropriatc standard KIO3 solulion('fill)lc 2) to thc rlrsorl)crto nraintlin tltc blue cok[. Shouirltltc absortrcr sol!tiot) bccorr]c conlplctcly cotorlcss, diicrrd the dctcnnination. Mrke KIO] additioxs as rhc r,lle ol cvolLrtion ol SO3 rlinrinishe^s such tlrlt, wh(:,t cor1lbrrslion is conrplctcrl, lllc irrlcnsityof tht bluc' color is tltc snn:c lrs thc inititl iltcnsity. Conrbustion is conlplcte when this colol rcmainsfor at lcrst I min. Record the vclume oI KIO3 solution rcquiredto rirriite thc S02 evolvcd. 13.3lllanii [)ctcnnirratroa- Make a blank determinalion whenever a new supply of colrbustion boats, rtlatcrials. or rcrsents is uscd.lro]low tlre abovepro(:e_ dnre, but ontit thc sanlple_ 462

14.4.3Placethe combustion boat on rhe balance and weigh an appropriate amountof the saolplcinto the trenchin the MgO powder.Enter the wcfuht. 14.4.4 Remove the combustionboat from rhe balanceand add MgO powder until the co bustion boat is filled to two-thirdscapacity.
NOTII9.- lf nrcccprilblc rcpeitrbiliLy is cncounrcrL. fJ nr pilnie lj .xr sjutu'rcs,conbusrron pronroter such as V?Or or lhu LtiCO prorlu.t LoDt-Aut can ba subsrirutedfor the MgO. NOTE l0 - CautioD - \/.2O5 cnn causedererjorlrion of rhc iurflr. ( cerarnlcs sO use rl uith c e_

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14.5 Initiate oxygen florv and load boat into fumacc. I4.6_ Wlrcn lhc anulysisis cotDplclc. rcild th(, rcsull rrom the microprocessor. 14.7 Remove the expended combustion bo:il frool (lrc firrnace. l4.E Make repeaced runs until two results difl.er by less dtan the repeatability of the method.

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15. Calculation 15.7 Calcukttion tor lodate Detuction - Calculatc the sulfur content of the sample as follows:

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ARTICI-E 24 _ LIQUID PENSTRANT Sf,ANDARDS ''Sulfur, mass % = llf0 (V - V) x F" x Qll|l (3)

sD-15s2

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

V= standard KIO3 solution, ml. used in the analysis, -: ! i: , = Vr standard KIO: solution,mL, usedin the blank determinatiorL I factor(see10.1.2), 4= standardization C= sulfurequivalent of the standard KIO3solution usedir the analysis, mgn . nd I4: milligrams of sarnple usedin the analysis. 15.2 Calculationlor IR Detection: 15.2.1Reportall rcsultsusing the rnicroprocessor. 15.2.2 Report the averageof two results.

ing valuesin only one casein twenty:

Sulfur,Mals, % Range O.0to 0.5 0.5 10 1.0 l.0lo2-0 2,0 to 3.0 3.0 to 4,0 . 4.0 to 5,0 Reproducibilily Iodate 0.08 0.1I 0.1'7 0.26 0.40 0.s4 IR" 0.13 0.21 0.?'l 0.38 0,44 0.49

L7.2 For Petroleurn Cokes by lodate and lR Methods - 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 the following values in only one case in twenty: r = 0.05X where X is the average of the two Lsst rcsults. 17.2.2 Reproducibilir) - The difference between two single and independentresultsobtained by different operatorsworking in different laboratorieson identical test material could, in thc long run, in the normal and correct operation of tbe test method, exceedthe follorving values in only one case in twenty: R = 0.22X where X is the average of the two (cst results.

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16. Rcpod 16.1 In the rangehom 0.05 to 5.00 mass% sulfur, rcpon to the nearest0.01 mals %. In the range from 5 to 30 mass % sulfur,reportto thenearest 0.1 mass%.

17.

Precision and Bias

l7.l For Petroleufl Prodacts by lodnte and IR Methods - The precision of this test method as deternined by statistical examination of interlaboratoryresults 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, exceedthe following valuesin only one caseir twenty:
Sulfur,Mass,% Raogc 0,0 ro 0.5 0.5 ro 1.0 1.0ro 2.0 2.0 ro 3.0 3.0 ro 4.0 4.0 lo 5.0 Rcpahbility Iodate IRll

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0.05 0.07 0.I0 0.16 0.22 0.24

0.04 0.0? 0.09 0.12 0.r3 0.16

17,3 Bias - The bias of the procedurc in this test method is being deternrined.

18,

Keywords

17.1.2Reproducibility- The difference between two singleandindependent resllB obtained by different

18.1 furnace; high tcmperature; induction fumace; iodate titration; IR detection; petroleum; resistance: sulfur; tiration

463

STANDARDTEST METHOD FOR LIQUID PENETRANTEXAMINATION

sE-r65
(ldentical with ASTM Specification E 165-95)

(ilt,

Scope

1.1 Tl)is t(.srnrerhod coversprocedures for penetrant cxlLn:ination of rlirterials. Thcy are nondestructive testing rncthodsfor detecting discontinuities that are open to thc surlacc such as cracks,seanrs, laps, cold shuts, lantinations, through lcaks, or lack of fusion and are hpplicable to in-process, linal, tnd mtintenance examinalion.'I'hcycan bc c[f'ectiyely uscd in the examination of nonPc'rous, nrctallicmaterials, both fenous and nonlerrous. ilnd of nonmctallicnaterials such as glazed ol ltlly (lcnsiliedcciamics,ccrtlirr nonporous plastics, xno 3russ. 'l'his 1.2 lcst rclhod tlso providcs I rcfercnce: 1.2.1 tly which a liquid pencrrantcxanrination proccss rccon'lrcn(lcd or requifedby individualorganizirtionsclr br: r'cvicwcdto iLsccnitilt its lpplicability ilnd corDI)lctcrcss, 1.2.2i.br use in rhe prepxration of process specificltions dcaliDgwith the liLluidpcnetrantexamination of niaierirls rnd parts. Agreenent by thc user and thc supplier regnrdingspecifictechniquesis strongly reconrntcncled. 1.2-3 Frx usc in lhe orglnization of the facilities ilnd pcrsonncl conccrncd with the liquid peneirant examinai to n . 1.3 fllis lcsl Dlctho(ldocs not irxlicrtc or suggcst c{itcriit lor cvaltrationcl thc inclicatio|ls obtrined. It should be point(.dout, howevcr,rhlt after indications have beenproducecl, they nlust be iDterpreted or classified lrnd then cvrluated,For this purposc there must bc.a scpilrirtecodc or specilicationor a specific asrccnrent to definethe type,size,lociltion, anddirection of indiciltions considered acccptablc, and thoseconsidcrcd unucccptable464

1.4 The values stated in inch-pound units are to be rcgarded as the standard-'Sl uniis are provided for information only. 1.5 This standard does not purport to address all of the safety concems, if any, associdled v'ith its use. It is the responsibilitf of the user of this standard lo establish tppropriate safety and health pructices ttnd deternite the applicability of regulatory litnitations prior to use. For specilic hazard statements, see Nores 5, 12, and 20.

2.

IleferencedDocuments

2.1 ASTM Standards: D 129 Test Method for Sulfur in Pctroleum Producrs (Ceneral Bomb Method) D 516 Test Method for SulfateIon in Water D 808 Test Method for Chlorine in New and Used Petroleum Products(Bomb Mcthod) D I193 Specificationfor ReagentWater D 1552 Test Method for Sulfur in Petroleum Products (High-Temperature Method) D 432'1Test Method for Anions in Warer in Chemically Suppressed Ion Chromatography E 433 RuferencePhotographsfor Liquid PenetranrInspection E 543 Practice for Evaluating Agencies that perfo l NondestructiveTesting E 1208 Test Method for FluorescentLiquid Penetrant ExaminationUsing the Lipophilic Post-Emulsification Process E 1209 Test Method for FluorescentLiquid Penetrant Examination Using the Water-Washable Process E 1210 Test Method for FluorescentLiquid Penetrant Examination Using the Hydrophilic Post-Emulsincation Process

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E l2l9 Test Method for FluorcscentLiquid penetrant process ExaminationUsing the Solvent-Removable E 1220Test Method for Visible P.e4etanf,Exami4ation Using the Solvent-Removable Process ,, ., E 1316Terminolo.gy fof NQndpstru.pdve;Examinations , E 1418Test Merhodfor VisiblePenbtrant Examination Using the Water-Washable Eocess 2.2 ASNT Docutneu: R""ommenoeopral,i"" Svi-fb-f e fo, irlondestructive Testing Personnel Qualncatiotr and Certification 2.3 Military Standard: MIL.STD-410Nondestructive Testingpersonnel eualificationandCertification 2.4 APHA Standard: 429 Method for the Examination of Water and Wastewater 3. Terminologr TABLE I CLASSIFICATTON OF PENETRANT EXAMINATION TYPES A N DM E T H O D S
TypeI - Fliorescent Penetrant Exaninatiot
(seeTe5tMethodE 1209) MethodA - Water-washable MethodB - Post-emulsifiable, (seeTest MethodE tipophitic r208) (seeTest MethodE tZ19) l\4ethod C - Solventremovable (seeTest Method MethodD - Post+mulJifiable, hydrophilic E t21.0) (seeTest MethodE t4l8) MethodA - Water-washable (seeTestt ethodE MethodC - Solventremovable 1220)

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3.I1fhe definitions relating to liquid penetrant examinarioni!which appearin TerminologyE i316, shau appty...tb the termsusedin this standani. 4. Summary of Test Method

Each of the various metbods has been designed for specific uses such as critical service items, volume of parts, portability or localized areasof examinarion.The method selectedwill dependaccordinglyon the servicc requirements. 6. Classification of Pcnetrntions and Mcthods

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4.1 A liquid penetrant which may be a visible or a lluorescent materialis appliedevenlyover the surface being examined and allowedto enteropendiscontinuities. After a suitable dwell time, the excess surface penetmntis removed. A developer is appliedto draw the entrapped penetrantout of the discontinuity and stain the developer.The iest surfaceis then examined to determine the prcsenced abserce of indications.
NOTE l: - Thc developcrrDry bc omittcd by rgrernentbet*eeo purchaserand supplier. NOTE 2: Cauaion - FluoEsccnt pcnclrant qxaoinalion shall not follow a visible penerrant cxaminationuds*s thc Focdurc bss been qunlificd in accordrncewith.l0:, becauscvi3ibL dvcs mav cause deterioration or quenchingof Auorcsclt dyar.

6.1 Liquid penetrantexaminttion mcthods and types are classified as shown in Tablc I 6.2 Fluoresccnt pcnetrunl (xaninariolr utilizes pcnetrants that fluoresce brilliantly when excited by btack light (see 8.9,1.2). The sensitivity of fluorescentpenetrants depends on their ability to be retainei ir the various size discontinuities durirg processing,then to bleed out into the developercoating and produce indications that will fluoresce. Fluorescent indications arc many times brighter than their surroundings when viewed under black light illuminarion. 6.3 Visible penetrant exaninalion uses a penetrant that can be seen in visible light. The penetrant is usually red, so that the indications produce a definite conhast with the white background of the developer. The visible penetrantprocessdoes irot require the use of black light. However, visible penerant indications mustbe viewedunderadequate white light (see8.9.2.1). 7. Types of Materials

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4.2 Processing pafameters, such as surfaceprccleaning. penehationtime and excesspenetrantremoval methods,arc determinetiby the specificmaterialsused, the nature of the part under examination(that is, size, shape, surface condition, alloy| andtypeof discontinurties expected.

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Significance and Use 5.1 Liquid penetrant examination methodsindicate the presence, locati6riand, to a limitd extent. the nature and magnitude of the detected discontinuities.

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7.\ Liquitl penetrantexaninatiott nrateriob (secNotcs 3,4, and 5) consist of fluorescenl. and visibleDenetrants. emulsificrs (oil-brse anrl watcr-base; fast and stow acting), solvent removers and developers.A family of liquid penetrant examinationmaterials consistsof the applicablc pcnetrantand cmulsifer clr rcDro!,er'as rec-

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2OOISECTION V

(D

i,?lf_],,-,, X,il#.i;r

:ii'i:11"1":1"ii"J::1",i::i:::lf ff :;,"$#::: :j,[;*l:?i,""Hr;:1ru, : .:1j,":1,i forsrcciar requ,rcmenrs

ror surrur. haroscn

:;r,:i,::j d"l{;:ril:r*il1hry"*il,#,',#f,ff
"fi ;:l"fr ,'r;;;,;",:,il{#t;""fl""'"'}#:ff JlHT',];fl ,ilx
7.2 penetaus:

n.ffiff"flt',H
:

: d*ftil{i,,qfif"" :'",f

"*,]f"."

,;i ;J:,"",:I[,ffarion

:i:,'ll,Tffi :lJ:"T,l'", ,T,,"i1,.::,::1,1,r.,il*"ff ",:"ff*"."*," does noroccur, ffi Tr#*$JJf*ff resutring

in

Jiff ;Il;f; i'# i, fl :;".ilt"l# * Jtil i:i :l jT#:H,..,i1T; .""" *",.._*,,"ni1,J #,"1,*;,:;T,1il: "Ii9 ffT:,: J,: : :; m,,n:I,;*:l I r h e,u,ra". q r,e" ;:,,','T,:"1,,' l r ;:,l "
ll:":il:'r:.;":.,";

*:";t**#*#*t,T:lr I ';:1"",;?*# i tfi :l' [flTf"..",i#i?il-,1

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

i;;a;;#n1p*,in :

:l;:l,j.*:; l:'x

rvirsncL r rrr r t r)l discontinuilicl il llx

**.";;:;lli$:::fii:: "::,*;,,lti"_ ,:g,llL:l :j;T:

: -*lit*t[*:'**T, **t I:i;,;ll; ::ll,,J"li:x*1,,ti*:i!:*i:iTil:li

,i;1,:,i;:l;:,1;;..:tffi.:: iii ,,, !,q,ff rirnc.'.;;,;. ll-,.]i'i" I :.illillryff
fi';;:werr

: ln i#".I';:tr,r#*Ji,-.rp j: ;ffiil:J; t ;iiJi";l"L',l,ll? ji"J:Tl"j;:l', .

:I ;il.;li:jf ",I"",r.,"":,il"1,ff1

*n#*#*;*,rt : run$*ffiffi *;llij:;l,y;,:x1,":"t'ff:l[{j*'$*f $l#if i",*r,""""*,*":i?"::#:,

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7.3 E,tut.tiliert;
rrr rrusron crtrrblishcs lhe entulsificr lime Theyarc cirtrcr st,'rr.. .,' ng on rhcir viscosity "..,.*ii"-.,'u"o"lirL'rtion

a ;li"#-jfi.,fi e,iquids ::x* *Ii:ft;::::::xib *'r'r:}"ffi ,'",'.ii'"!r;iliL 1i *r'i.r, ,"1*r;; ,",,' t';""i'J,.Ti:lill::llij ali",""nr* ,.0,",' I :ll,,ll': Ll'J';; i;'J:lgr*"n '"-"*iirr,"
,i",'ni,i iX;rt"--*is rypc ordvetoncr isinrendcd forappr,calion

,,,oJ;,1.i"1,Jr"T.".:J#, as f^;:,;::i:.rs,suppried

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ASTSE ?a- L]auIDIEYIIIff

STANDARDS

sE-16s

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7.5.4 Liquid Film.Diveloperc are solutionsor 8.4 Removal of SurfaceContaminants: colloidal suspensions of resins/polymer in a suitable ,will-form'a-lranSparent .or-.,,.--*-.&4.1 carrier. These developers Freckaning - ."thesuccess of any penelrant examination procedurcis gre.ay dependertupon the translucentcoating on the surface of the part. Certain . types of film developerrnay-be stripped from the p-art -. surroundingsurfaceand discontinuitybeing free cf aay ..'contamilant (solid or liqu0 that might interfere with and retained for record purposes(see 8,8.5). 8. -.',Procedure .-.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 section of 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 defined by the contractingparties."Clean" is intended to mean lhat the surface must 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 penetrantfrom entering discontinuities(see Anne,( or Cleaning of Parts and Materials). NOTEll: Caulionproccsscs suchxs Residues from clcaning

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processing guirtelinesapply LtlThe following generat 2,3, and 4) and visible to bolh fluorescent lseefigs. (see penetmnl examination Fig. l). methods 8.2 TemperalureLimits - The teriperature ol the penetant materials and the surface of the part to be processed shouldbe between 50 and 100'F (10 and 38'C). Where it is not practicalto comply with these temperaturelimitations,.qualify the procedurc as describedin 10.2at lhe temperature of intended use and as agreetl to by the contracting panies. 8.3 SurfaceConlitioning Pior to PenetrantExaminarlo,, - Satisfactory resuls usually may be obtained in as-cast, or ason surfaces the as-welded, as-rolled, (or conditions in ihe densified forged for ceramics penetrants lesseasily conditions). Sensitive aregenerally rinsedaway and are therefore less suitablefor rough Whenonly loosesurface arepresent, surl'aces. residuals these may be removedby wiping with clean lintprecleaning free clo(hs.However, of metalsto remove processing residuals suchas oil, graphire, scale, insulating materials, coatings, and so forth, shouldbe done using cleaningsolvents, or chemical vapordegreasing removingproccsses. Surface by grinding, conditioning nachining,polishing or etchingshaltfollow shot,sand, grit or vapor blastingto rcmoyethe peened skin and when penetrantentrapmentin surface irregularities discontinumight maskthe indications of unaccptable iries or otherwiseinterfercwith the effectivenesi of the examination. For metals, unless otherwise specified, exists that etchingshall be performed when evidence previouscleaning, surface teatmentsor serviceusage the have produceda surfacecondition that degrades effectiveness of penetrantexamination.(See Annex Al.1.1.8for precerrtions.)
NOTE 8 - wlen agncd betlregn purchasef atd supplier, grit cl3nin8 ctchingmay bc sn acccptable blasringwirhoutsubscqucnt NOTE 9: Coution - Sand or sbot blastingmay porsibly close discontinuilies and extreme care shouldbe lsed with Erindingand machining operarionsto avoid rnaskirg disconlinuili.s. NOTE 10 - For strucluralot elefionic ccraflrcs, sudaceprcparatiod by giinding, sand blasting and crclitrg for pcnetrantcxamination is not recommended because of thc polentialfor damage.

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skong alkalics, picklin8 solulions aod chromaies, in padicrlat, mny adversely t.act tvith the penetrant and reduce its sensitivity and prfonnancc.

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8.4.2 Dryiry after Cleaning - It is essentialthat the surface of parts be tboroughly dry after cleaning, since any liquid residue will hinder the entance of by warming the penetmnt.Drying may be accomplished the parts in drying ovens, with infrarcd lamps, forced hot air, or exposureto ambienttemperature. 8.5 PenetrantApplication - After the part has been cleaned,dried, and is within the speciiied temperature range, the penetrant is applied to the surface to be examined so that the entire part or area under examination is conpletely covered with peoctrant. 8.5.1 Modes of Applicstion - There are various modes of effective application of penetrant such as dipping, brushing, flooding, or spraying. Small parts are quite often placed in suitable baskets ard dipped into a tank of penetrant. On larger parts, and those with complex geonetrics, penetrantcan be applied effectively by brushing or spraying. Both conventional and electrostatic spray guns are effective means of applying liquid penetrants to the part surfaces. Electrostatic spray application can eliminatc cxcess Iiquid build-up of penetraoton the part, nrinimi:e overspray, and minimize the amount of penetrilntentcring hollowcored passageswhich might serve as penetrantreservoirs, causingseverebleedoutproblemsduring examination. Aerosol sprays are conveniently porlable and suitablefor local aDDlication.

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467

sr,r-165

?00tsEcTloNv
[tlcoMlNc PAnls

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PsElLElta (See 8.4)

i:fi";:; P I IT TRA ' E (See 8.5)

I I

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REMOVI

(See 8.6)

0EvEtoP (See 8.8)

(See8.7)

(See 8.7)

IHSPECT

(SeeB.9l

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P0 5 T C ! t N (See8.10 and A 1. 2 "

O U T G O I NP G AATS

F I G .]

FLUORESCE N TDV I S I E L E A N PENETRAN TS P E C T I O IN GN ENERA LR O C E S S IP P NR GO C E D U R E S FLOWSHEET

NOIL l2 Caurion - Not all prnerr,rnr n l i , r c f l x t \ a r c s u i r a b l ef o r (rc.-1r.rr . .T .r' nftrtrc.lon\. so rcsts \houtJ he conctucrcd prior \OTlr t . 1 : r \ , , r r ) i [ - W i r h s p r . i yr p l l i c . ( i o n ( . i r i s r m l l o n a n rr h l r r c D l , l , , L o. T h i s i s S.nc|:| y .,cronrptislcd rhrcu -!h r , . 1 c . t I d ! \ r i n L , J \ t r , : r ) h r \ 1 r ' r: r n d c r i t r . , u $ r systern

1J.5.2 l)tttt'truat Dwall Tinc _ Aftcr applicatiotl, :rllou cxcr]lispcnclrant to drain ll.otrr the pAn (C fe 458

should be laken to preventpools of penebrnt from tonnrng.on thc part),whilc rllowing for properpenetranr owe/r tlme (see TabJe 2). The teng(h of time the penctrrnt must rernainon the pan to allow prooer penelration slrouldbc irs recomntcnrled by thc pcnetranr manufacturer.Table 2, howevel provides a iuide for selection of pcletri|nt dwell times for a varietv of materials.lbrms, :lnd types of discontinuiry. Unlcsr

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

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ARTICLE 24 -

UQUID PENETRANTSTANDARDS

sE-165

PBECLE4TI (s68...1)

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Psrn tubp6r
DFY (5 8.1.2, PA{ETnA|.T {s4o e.5) FIIJALRINSE (s8-6.11

o.y

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Sp.rt
ORY {sd 8.7) OEVEIOP (S E.8)

gry

oEvgtoP {sr.8}

D8Y (Se8.7,

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

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' L O W S H E EF TO R PENETRAN ET X A M I N A T TU OS NI N G pR'cEss *ASHABLE (rdsr METH'D IHE WAIERe rzosFdR ;'iu';;$;ii AND rEsr METH.D 1220 E F.RvlsrBLE LIGHT)
t . 1

F I G '2 ' ' G E N E * o L PROCEDURE

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i
off manually, by the useof ilutornatuc or sentr_automatic water-spmy equipmentor by immersion, For immersion are completelyimmcrsed in thc wxrcr :lnslng,_pans oatn wttn arr or mcchrnicrltsitition. Accuntulr(ion of Yater rn pockeh or rcccsscs of th; surflrcc nrust bc avoided, thc finul rilsc stcp is not cflectivc, us .lf evrdenced by e\cessive resiLlual surfacepcnelrrni tftcr rinsing, dry (see 8.7) and recleanthc part, rhen reapply the penetrant for rhc prescribccldwell tine. (a) The temperiltureof the rvater should be rclativc)y constant and should be maintilined within the range o-f 50 to 100'F (10 ro 38"C). {a),lnra1-y-s3 waler pressurc should nor bc grentcr -, rhan 40 psi (280 kpa).

othcrwise specified, the dwell time shall not exceed the, maximum recommendedby the manufacturer. spccifir appticarions in strucrurat ceramics )^911-lo , dcrccung ,F:, -:".c L'u,cxampte. paning I'|'csin sID{asr n.alcrial), therequirEd peneFanl dwel dmeshould bc determin;d exprimentally sndntay bc roDScr lhanlharsho*nio Taulc.l aDJ 8.6 Penetrant Removal 8.6.7 Warer t$ashaite: ,8.6.f.1 Removal o! Excesspenetrants _ Afrer . rnc required oenetration time, the excess penetrant on (nc ,surlace being exarnhed must be removed with water"iusually a washingtbperation. It can be washed 469

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sri-t65
2001 SECTIONV

I I

8.t.2

Scr: 8.5 E.5.1 8.5.2

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1.. 8.8.3 0.0.1 8.8.t

Sc(: 8.6.2 8.6_2.1 86.2.2 5c! 8.6.?.3 .6.2.'l 0.6.?.5

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6.7.2

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ria
S...8.9-1 0.9.t.t

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0_9.r.2
8.9.1.3 8.9.1,21 Stlecial R.qui..nEatt 9.1

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9.2
Ptoc.dt,. Requirc.u4|l l0.i 't0.2

8.2(VitiblcJ

S..: .9-2 ,9.2-r

Sc.: 810

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the surface with a clcan, absorbentmaterial dampened rvith.w.rteruntil the excesssurflce penetrant ts renovcd, as dcterminedby examinatienunder black light for fluorescert methodsand white light for visible mithods. 8.6.2 Lipophitic Enulsificarion: 8.6.2.1 Application of Enulsifter _ Aller thc required penetrationtime, the excess penetrant oD lhe part rnust be emulsified by immersing or flooding

F I G .3 T Y P E2 _ P O S T E I \ l U L S I F I A BP LE ROCEDUR E N TD ) B - 2( V I S I B L E ) A -S 2 ( F L U O R E S C EA N
fc) Rinsetinre shouldnocexcced 120 s unless other_ wise spcci,iedby palt of material specification.
out of disconiinujties. with fluorelenf n c n . t r r n l F c ' h o d s p e n n n n r b e r i n s i n e o p m t i o r )u n d e r b t a c k l i q h r s o I n r I r r c n i r h c d r t e r m i n c d w h e n t b e s u d : r c ep c n d m n r has bcen . d e q u n t c l yr c m o v e d .

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_ Avoidoverwashi Ercessive washing s. can )-9.1u-]:.. 9"11,":' causepcnclranL to hc washed

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1J.6.1.2 Renoval by Wipiug _In speciatapplica_ . trons,pcnetrantrentoval may be performedby wiping 470

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,ARTICLE 24 -

LIQUID PENETRANTSTANDARDS

sE-165

P.rl. Incornlng

PNECLEAI'I

(ss 6.1.1) Modnlcal oaY tS 8.4.2) PENETAAr{' APPLICATIOII (S0.8.5) PEht Strlpp. oeiwgent

D(f ^pgly Solvn(Flroasclnl

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NE OVE ICESs PENETR NT (S6 8.0.4) DBY {s6 8.7)

Solvnt WIp4ll

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Dry
No.l3quoout Wol or LJquld Flln Ovfo!r

OEVELOP (So 8.8)

oaY (s8e8.7) EXAMINE nuor6sc0nt (f'6o 8.9.1) Vlslble (So 6.9.2) ltlr!r|l POSTCLEAI{ (56 8.10 and Ann6x on Posl Cloartng)

Dry

ory
Vapor Og.e.36 SolvntSoax Oulqoint P.tL Ulrasonk Cl3n

gENERAL. FIG.4 SOLVENT.REMOVABLE PENETRANT EXAMINATION PROCEDURE FLOWSHEET (TESTMETHOD E I2I9 FORFLUORESCENT AND TESTMETHOD ! I22OFOR VISIBLELIGHT)

the parts with the requiredemulsifier(the emulsifier combines with the excess sutfacepenetrant and makes thc mixture-removable with wter rinsing).After application of the emulsifier,the pars are drained in a mannerthat preventsthe em sifier from pooling on the part(s). 8.6,2.2 Emulsifcation Dwell Timebeginsas soon astheemulsifier hasbeen applied. The length of timethat theemulsifier is allowed on apartandin contact to remain with thepenetrant is dependent on the typeof emulsifier employed and the surface condition(smooth or rough).
411

Nominal emulsificationtime should be as recommended by the manufaciurcr. The acrualenrulsificationtime must be determincdexpcrimentallyfor each specili tpplication. The surfacefinish(roughness) ofthe pan is a significant factorin theselection ofand in theetnulsification time of an emulsifier.Conracttime sbould be kept to the least' possible time consistentwith an rcceptablebackground andshould notexceed themaximumtimespccified for the part or material. 8.6.23 Post Rursirrg- Effectivc post rinsing of the emulsified penetrant from the sulflsg 6xr 6.

sE-165

2001sEcTIoN v TABLE 2 RECOMMENDED MINIMUM DWELL TIMES

Material Form castings and welds

Type of Discontinuity
porositt lack of fusion, coldshuts, cracks(all formg) lapt cratks (all forns) porositt cracks lack of fusion, cfacks crack3 porosity cracks/

(minutes) DwellTimes/
Penetrantt Developef' 10

Aluminum, nragne5ium/ steel, bra5s andbronze, titaoium andhightemperature alloys

wroughtmaterials- extrusion!, lorgingt plaie Carb;de-tipped tools Plastic Glass Ceramic ^ For temperature rangefrom all forms all forms all forms

10

l0 10 10 10 10

50 to 100'F (10 to 38.C) for fluorcscent penetrants and50 to L25.F (10 to 52"C) for visiblepenetrant. \.4arimun pcnerrrnl dwelltime:n accordance with 0.5.2: t Development time beginsas soonas wet developer qf part5(recommended coatinghasdried on surface mlnlmum).Maxlnum oevetopment t.rre in ac<ordance w;rh8.8,6.

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accomplishcd using either manual, semi-automated, or automated water immersion or spray equipment or conrbinations thereof8.6.2.4lnucrsiou - For inrmcrsion postrinsing, prrts are cotnpletely inmersed in the water bath with arr or n)cchanicl gitation.Thc tinle and tempcrature should bc kept constant. fd) The nlaxintunl dip-rinsetimc should not exceed 120 s unless orllerwisespeciliedby pan or material specification. (b) The tempertture of Lhcwrrcr should be relatively coJrstant and should be maindined within the rangeof 50 to 100"F (1Crro 38'C). Cndion: A touch-uprinse xr3), bc nccessary aiier imntcrsiotr. 8.6.2.5,Sirro-rPo.il /tir-rirg - Effective post rinsing folio\ring emulsificatiolr can also be accomplished by eithcr manual or aLtouatic water spray rinsing of lltc I)1trts rs tbllervs: Control rinsc wirtcr fl) tcllpcriL{urc tvithin tlrc rangc o f 5 0 t o 1 0 0 " 1( .10 to 38"C). (b) Spray rin-se water pressur.c should be in accord_ ilrce \\,ith llanufaclurcIs' rccotnmcldations. (cJ Tlic rnnxintuiD sprayrinsc tirDcshouldnot cxcccrl 120 s unlcss olherlvisespecilicdby part or mate.ials specificaiion. 8.6.1.6nnrre Elft'ttiwncss- If rhc emulsification and final rinsc step is not effcctive, as evidenced by excessivc rcsiduaisurface penetnntaftcr cmulsificalion and rinsing, dry (scc 8.7) and reclean the part and rcapply the peflerrllrlr for tha prescribcd dwell time. 472

8.63 Hydrop hil ic Emul sif catio n : 8.6.3.1Prerinsing - Directly after the required penetrationtime, it is recommendedthat the parts be prerinsed with water prior to emulsification (8.6.3-3). This step allows for the removal of excess surface pcnetrant from the pads prior to emulsilication so as to minimize the degree of penetrant contaminatiol in the hydrophilic emulsifier bath, thereby extending its life. In addition,prerinsingof penetrated pafls minimizes fossible oily penetrantpollurion in the final rinse stcp of this prccess.This is accomplishedby collecting thc prerinsingsin a holding tank, separatingthe penetrant from water. 8.6.3.2Prerinsing Controls - Effective prerinsing is accomplishedby either maoual or automaaed waler sprav rinsing of the pans as follows: (aJ Water should be free of contaminantsthat could clog spray nozzles or leave a residue on parts, (b] Colltrol wttcr tcnrpcnrturc within 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 time should be tlre lcast Dossiblc tirnc ( onrinill!, 60 s rnaximunr)to providc a consislcnt residue of penetranton parts. lvash time is to be as spccified by the part or matedal specification. (e.)Remove water trapped in cavities using liltcrcd shop air ar a nominal prelsure 25 psi (175 kpa) or a suction deyice to remeve water from pooled areas. 8,6.3.3 Application of Enulsifier * After thc required pcnetration time and following the prerinsc,

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ARTICLE24 _ LIQUID PENETRANT STANDARDS the residualsurfacepeneh t on pan(s) mustbe emulsified by immersing the paft(s)in a hydrophilic emulsifier bath (8.6.3.4) or by spralng theipar(s) ?with the emulsifier (8.6.3.5) thereby rcnderingthe iemaining residual surface penetrantwater-washable in the final rinse station(8.6.3.6). 8.63.4 Immersion-For immersion application, parts are complQtelyimmersedin the emulsifier 5ath. The hydrophilic emulsifiershould be gently agitated thrcughoutthe contactcycle. la) Batb concntrationshould be as recommended by the manufacftrer. Most hydrophilicemulsifiers are used within the rangeof 2n to 33% in water. Nominal use concentrationfor imrnersion applicationsis 207o. (D) Bath temperatures should be rnaintainedbetween 50 and 100'F (10 to 38'C). (c) Immersioncontacttime should be kept to the minimumtimeconsistent background wilh an acceptable and should not exceed120 s or the maximumtime stipulated by the part or materialspeaificatiol. (d) Emulsifier drain time beginsimmediatelyafter parts have been withdrawn from the emulsifier tank and continuesuntil the parts are wsshedin the final dnse station(8.6.3.6). This drain time shouldbe kept to a minimum to avoid over emulsification and should noLexceed 90 s, - For sprayapplica8.6,3.5SprayApplication tion foltowing the prerinse step, psrts are emulsified by the spray applicationof an emulsifier.All part surfacesshould be evenly and uniformly sprayedto effectively emulsifo the residualpenetant on part surfaces to render it water-washable, (4J The concentration of the emulsifier for spray application shouldbe in accordance with the manufacrecommendations, turer's but shouldnot exceeA 5%. /r) Temperaturc to be maintained at 50 to 100"F (10 to 38'C). (c) The spray pressureshould be 25 psi (175 kPa) max for air and 40 psi (280 lPa) max for water. (d) Contact time should be kept to the rninimum consistent with an acceptablebackgroundand should Dot exceed-120 s or the malimum time stipulatedby rhe part or ma@rialspecification. 8.63.6 Posr-Riruing of Hydrophilic Emulsified Parrs - Effective post-rinsingof emulsified penetrant from the surface can ba accomplished using either manual,semi-aubmdted,or automated water immersion or spray equipment or combinations thercof.
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- Pansare to E,6.3.7 Immersiott Post.Rinsing be completely immersed in the water bath with air or mechanicalagitation. be relatively of the watershould . (a) The temperature constan! and shouldbe maintained within the rangeof 50 to 100'F(10 to 38'C). (b) The maximum dip rinsetime shouldnot exceed 120 s unlessorherwise specified by part or material specification. Cautiont A touch-up rinsemaybe necessary after immersion. - Followingemulsi8.6.3.8 SprayPost-Rlzsirg panscan be post-rinsed 0cation by watersprayrinsing as follows: (a) Controlrinsewatertempcrature within thc rungc of 50 to 100'F(10 to 38'C). (6) Sprayrinse waterprcssure shouldbe in accordancewith manufacturer's instructions, (c) The maximum sprayrinsetime should not exceed part 120 s unlessotherwise by or specifled mate als specification. 8.6.3.9 if tle emulsification nndfinal rinsesteps are not effecdye,as evidenced by exccssive residual after emulsification surfacepenetrant and rinsing, dry (see8.7) andrcclean the penetrant the pan andreapply for the presdibeddwell time. 8.6.4SolventRernovable Penetran!s : 8.6.4,1Removal of Excess Penetratt- Aftcr penetrant is the requiredpenetration time, the excess insofaras possible, removed by usingwipersof a dry, clean, lint-free material and repeatingtlre opemtion until mosttraces of penetrant havebeenremoved. Then usinga lint-freematerial with solvent lightly moistened remover theremaining aregentlywiped to avoid traces removirgpenetrant from discontinuities. Avoid the use of excess solvent.If the wiping step is not effectivc, by dimculty in removing the excess as evidenced penetrant, dry (he pa( (see8-7),and reapplythe penetralt for the prescribed dwel[ time. Flusbing the surface with solventfollowingthe application of the penetrant and prior to developing is prohibited. E!7 Drying - Drying the surfaceof the part(s)is prior to applyingdry or nonaqueous necessary develor followingthe-application opers of the aqueous developer.Drying time will vary with the size, nature,and numberof pans underxaminalion. 8J.l Drying Modes - Pans can be dried by using a hot-air recirculating oven, a hot or cold air prfticublast,or by exposure to ambient temperflaure, penetrant larly when the excess was removed surface

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the pans in a prepareddeveloperbath. Immerse parts only long emugh to coat all of the part surfaceswith the developer(se Note 18). Then remove parts from lhe developerbath and allow to drain. Drain all excess developerfrom recesses and trappedsectionsto elimipoolingof developer, nate whichcanobscure discontinuiues. Dry the pads in accordance with 8.7. The dried developercoating appearsas a translucent or white coating on lhe part,
NOTE l8r Cttlion - Atomiz6d sprayingi9 aor recommended since a spooy film may result NOIE 19: Cg| ion'If parts arc lcft in thc bath too lon8, indicationemry lcach out.

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with a solvenr. Dryingis bestdonein a thermostatically controlledrecirculating hot-airdryer.lncal heating of cooling is pernritted providedthe temperature of tha 'part in the range rcmains of 50 to 100'F(10 to 38"C) for lluorescent methodsand in the range of 50 to 125"F(10 to 52"C) for visiblemethods otherwise unless agreedby the contracting parties.
NOTE 16: Cautlon t 60"F (?l"c). Drying ovcn temperalur should oot exceed

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 of developers such as dusting, immersing, flooding or spraying. The sizc, configuration, surface condition, nunrber of parts to be processed,and so fonh, will influence(he choice of developerapplication. 8,8.2 Dry Powder Developer- Dry powderdevelopers should be applied inrmediately after drying in such a nranner as to ensure complete part coverage. Parts can be inrmcrsed in a containcr of dry developer or in a fiuid bcd of dry developer. They can also be dusted widr rhe powder devcloper ihrough a hand powdcr bulb or a conventional or elecbostaticpowder gun, It is conrnron and cffcctive to apply dry powder in an encloseddusl chamber.which createsan effcctive and controlleddust cloud. Other meanssuited to the size and gcornctry of thc spccinrcnmay bc used, providcd the polr'dcr is dustcdcvcnly ovcr ths enttte iur(ace being eraurincd. Excesspowder may bc removcd by shakinr or tapping the part, or by blowing with low-pressure (5 to l0 psi) (34 to 70 kPa) dry, clean, coruprcssed air.
N O 1 l i : l 7 : ( l o l i o , r - - I - l r cr i r $ r r c : r l n i o r c n \ i r y\ h o u k l h i : c s r u h t i s h c d c x p c r i n r r D ( t l l yl l r e l c h a p t l i c a r i o r ) -

834 NonaqueousWet Developers- After the excess penetranthas beenlemoved and the surfacehas been dried, apply developer by spraying in such a manner as to ensure complete part coverage with a thin, evenfilm of developer. Theset)rpesof developer carrier evaporate very rapidly at norma.lmom temperature anddo not, therefore,requirethe useof a dryer (se Note 20). Dipping or floodingpafis with-nonaqueous developers is prohibited, sincetheymayflushor dissolve the penetrant from within the discontinuities because of the solventactionof thesetypesof developers.
NOTE 20: Warning - Tfie vapors f(om $e evaporaling, volatile solvent dcvcloper carricr may be hazardous.Roper venlilarion should be prcvided in all cases. but especially when rhe surface (o be elamined is insidc a closed volume. such 9s a process drum or a small sto|age taok.

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83.5 Liquid Film Developers- App)y by spraying as recommendcdby the manufacturcr. Spray parts in such a manner as to ensurc complete part covcrage of the area being examined with a thin, evcn film of developer. 8,8.6 Developing Time - The length of time the developeris to rernain on the part prior to cxamination slrould bc not less lan l0 rlin. Dcveloping tinrc beginsimmediately after the application of dry powder developerand as soon as the wet (aqueousand nonaqueous) developercoatirrgis dry (that is, the solvent carrier has evaporatedto dryness). The maximum perrnitrcd developing times are 2 h for aqueous developers an,J I h for nonaqueousdevelopcrs. 8.9 Examination - Perform examination of parts afrcr the applicable development time as specified in 8.8.6 to allow for bleedout of penetrantfrom disconrinuities into the developer coating. It is good practice ro observe the bleedout while applying the developer as an aid in interpreting and evaluating indications,

8.li,3 /rTrrcors Det'elcpers- Aqueous developers should bc lppliccl to the pirt inrnrcdiately after thc exccss penetrlnt has been relnoved and prior to drying. Aqueous developels should be preparedand maintained witll the ntanufacturer's il accordance instructions and applied in such a nlanrcr as to ensurecomplete, even, p3fl covcragc.C:rutionshouldbe excrcised when using !n aqueous developer with \rater-washablepcnetrants to avoid possiblc stripping of indications.Aqueous developcrsnay bc appliedby spraying(seeNote I?), florving, or ir)lltrcrsing thc parl-It is commonto immersc

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,: ] AITTICLE STANDARDS 24 _ UQIND PENETRANT 8.9.1 Fluorescent LiShi Emmination: 8.9.1.1 VisibleArtbient Light Level - Exffine fluorescentpenetraiitindicationsunder black light in a darkenedarca"Visible ambientlight should not exceed 2 ft candles(20 Lx). The measurement shouldbe made with a suitablephoographic-type visibte light meter on the surfcebeing examined.. Btack light Izvel Control - Black lighr inrensity,minimumof 1000 pWcmz, shouldbe measured on the surface being examine4 with a suitable shallbe black light meter.The black light wavelength in the ralge of 320 ro 380 nm. The intensity should be checked weekly to ensurethe requircd output Reflectors and filters shouldbe checkeddaily for cleanliness and integrity. Crackedor broken ultraviolet (lw) Defective immediately, frltersshouldbe replaced bulbs, which radiate UV energy, must be replaced before further use. Since a drop in line voltage can cause inconsistdecreased black light outputwith consequent transformershould ent perfor.mance, a constant-voltage be usedwhen thereis evidence of voltagefluctuation.
Caution; Certain high-inlensity blact light may emil DnacceplabJe rmounts of visible light, which will cause fluorcacentindicationslo disappear. Care shouldbe takento usc only bulbs cenifiei by lhe ' purposes. Jupplicrto b suitnblefor suchexamination NoTE 2l - The recoruncnded minimumlight intensityin 8.9,1,? is intended for general usag.- Foi critical eraminations, hiSher intensitylevels may bc ftquircd,

- Keepthe examination area ESj Howekeeping of htefering including fluorescent free debris, objects. at all times. Practicegood housekeeping &9A Evaluation - Unless olherwise ageed, it is normalpracticto interpretand evaluatethe discontinuity based on the sizeof the indiiation (seeRefercnced Phoaographs E 433). in &10 Post Ckaning - Postcleaning is necessary thosecases wherercsidualpenetant or developercoutd processing interferewith subsequent or with service requircments. It is particularly imponantwhereresidual penehant examinalion' materialsmight combinewith in service conosion. A suitable to produce otherfactors technique, such as a simple water rilse, wate$pray, solrntsoak,or ultramachine wash,vapordegreasing, (seeAnnex on Post be soniccleaningmay employed It is rxommended thatif developer rcmoval Cleaning). necessary, should caricd out as proroptly as is it be possibleafter examination so that it does not "fix" pan. on the
- Devclopers pdotto vapor should NOTE be .emoved 23:Crution thEdeveloper on pans. Vapor degrcssing canbake degreasing.

'8.9.12

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Special Rcquirements 9.1 lmpuities:

8.9.1.3 Black Light Warm-Up - Allow the black light to wann up for a minimumof 10 min prior of the intensity of the ro its use or measurEment ulrraviolet light emitted. E.9.1,4 Visual Adaptation - The examiner should be in the darkened area for at least I min parls.Longertimesmay be neaessary beforeexamining under some circumstances.
NOTE 22: Crution c)iamination. Photochromic lensEs shall not be worn dudng

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9.1,1 When using penetrantmaterialson austenitic stainless steels, titani[m, nickel-base or other hightempeHture alloys, the need to restdct impurities such as sulfur, halogensand alkali metalsmust be considered. Theseimpurities may causeembrittlementor corrosion, particularly at elevatedtemperatures. Any such evaluation should also include consideration of the form in which the impurities arc presnt.Son)epentrantmaterials contain significant amoun(s of these impurities in the form of volatile organic solvents. These normally eyaporatequickly 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 Because volatile solvents leave the surface quickly without reaction under normal examination procedures,penetmnt materials are normally subjected to an evaporation procedure to rcmove the sclvents before the materials are axalyzed for impuritis. Thc residuefrom this procedureis then cnalyzed in accordance with Test Method D 129, Test Metbod D 1552, or Test Method D 129 decompositionfollowed by Test Method D 516, Method B (Turbidirnetric Method) for sulfur. The rcsidue nray also be analyzed by Test

8.9.2 Visible Light Examiwtion: 8.9.2.1 Visible Light lzvel - Visible peretrant indications can be examinedin either natural.oraftificial light. Adequate illumination is required to ensure no A minimum of the examination. loss in the sensitivitylight intensity at the examination site of 100 fc (1000 Lx) is recommended.

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be qualified/cenified in accord&ce wiii a writtenprocedurc conformingto the applicableedition of recommended Practice SNT-TC-IA or MIL-STD-4I0. 10.2 ProcedureQualifuation - Qualifrcationof procedures using times or conditionsdiffering from thosespecifiedor for new materialsmay be performed by any of several methodsard should be agreed by the contractingparties. A test piece containing one or more discontinuities of the smallestrelevant size is used. The test piece may contain real or simulated discontinuities, providingit displaysthe characteristics of the discontiluities encountered in product examination. 103 l./ondestrucrive TestingAgency eualification If a nondestructive testing agency as describedin Practice E 543 is usedto performthe examination, the agencyshall neet the requircmentsof practice E 543. 10.4 Requalifcationmay be required when a change or substitution is madein the type of penetant materials or in the procedure Gee 10.2). 11. Keywords l1.l fluorescenr liquid penetrant testing;hydrophitic emulsification; lipophilicemulsification; Iiquidpenetranr testing; nondestructive testing;solventremovable; visible liquid penetrant lesting;water-washable methods

MethodD 808or AnnexA2 on Methods for Measuring Total ChlorineContent in Combustible Liquid Penetrant Materials(for halogens otherthan fluorine)andAnnex A3 on Method for Measuring Total Ruorine Content in Combustible (for fluo. Liquid Penetration Matedals rine).An altemative procedure, Arnex A4 on Determination of Anions by Ion Chromatography, provides a single instrumental techniquefor rapid sequential measurement of commollanionssuchas chloride, fluoride, and sulfate. Alkali metals in the residueare determined by flamephotometry or atomicabsorption spectrophotometry.
NOTE 24t - Some cuncni staodardsindicatc 6ri impurity levels of sulfur and hrlogenscxceeding 1% of any onc subpect clamcnt may be considcred xcessive. Howevcr,this high a level may bc lnacaeltable for somcapplications, so the actualrnaximum acccpioble jmpurirylevel must be decideibetwen suppticr ard useroo a csse by casebasis. 9.?, Evaluated-Temperature Exdrni.ndtion Where penefant examination is performed on pans that must be rnaintained at elevated temperatureduring examination,

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special materials and processingtechniquesmay be required. Such examination requircsqualification rn accordance with I 0.2.Manufacturer's recommendations should be observed. 10. Qualincation and Rcqualification 10.7 Persotnl Quulifcatiott- When requiredby user/supplier agrcement, all examinxtion pe.sonncl shall

ANNEXES (MandatoryInfornadon)
A1. Cleaning of Parts and Materials ,A'1,1 Choicc of Cleaning Mcthod A.1,1.1The choice of a suitablecleaningmethod is based on such factoni as: (1) type of contaminant lo bc rcmovcdsinceno onc rr:cthod rcmoycs all contrminants equally weli; (2) effcct of rhe cleaningmerhod od the pafts; (J) praclicality of rhe cleaning method ior the part (for example, a large pan cannot be put into a small degreasel or ultrasoniccleaner); and (4) spccilic clcaning rcquirenrcnrs of rhe purchrser. Thc firllowing cleaning methodsare recommended: F.1.1.1.1Detergc t Clearl?lg- Detergcntcleaners are nonflarumable water-soluble compounds con_ taining specially selectedsurfactantsfor wetting, penetraling, emulsifying, and saponifying various types of 476 soils, such as greaseand oily films, cutting and machining fluids, and unpigmenteddrawing compounds, etc. Detergent cleanels may be alkaline, neutral, or acidic in nature, but must be noncorrosive to the item beinq inspected. The cleaning propenies of derergenr solurioni facilitatecomplcteremovalof soils and contamination from the surface and void areas, thus preparing them io absorb the peneirant.Cleaning time should average l0 to 15 min at t70 to 200.F (77 to 93"C) with moderate agitation, using concentrations (generally 6 to 8 ozlgat or 45 to 60 kglm3) recommended by thc manufacturerof tbe cleaning compound. Ll.l.l.2 SolventCleaning -There are a variety oi solvent clcaners that can be effectivclv utilized ro dissolve such soilsas grease and oily fitms, waxeslnd sealants,paints, and in general, organic matter. Thesc

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ARIICLE 24 _ LIQUID PENETRANT STANDARDS solvenrs should be residue.free, especially *t"n ur.a as a hand-wipe solvent or as a dip.tank degreasing riolvent. Solvent cleanersare not recommeided for th; removal of rust and scale, welding,flux and spatter, and in gencral, inorganic soils. Cautiou Somecleaninp solvcnts are flammable and can be toxic. Observe a rnanufacturers' instructions and precautionarynotes. A1.1.1.3 Vapor Degreasing - Vapor degreasing is a prefened method of removing oil o. gr"r""l type soils from the surfacc of parls and from open discontinuiries. k will not remove inorganic-type soils (dirt, corrosion, salts,etc.)"and may not removeresinous soils (plastic coatings, vamish, paint, etc.). Becauseof the short contact time, degreasingmay not completely clean out deep discontinuities and a subseouent solvent soak is recommended. Al.l.l,4 Alkaline Cleaning: (a) Alkaline cleaners are nonflammable water solutions containing specially selected detergentsfor wetting, penetrating, emulsifflng, and saponifying various types of soils. Hot alkaline solutions are also used for rust removal and descaling to remove oxide scale which can mask surfacediscontinuities.Alkaline cleaner compounds must be used in accordance with the manufaclrrrers' recommendltions. Caution: partscleaned by the alkalineclenningprocess must be rinsedcompletely free of cleaner and thoroughly dried by heat pdor to the penetrnnt inspcction process lpart temperatureat thc lime ofpenetrant aFplica(ionshall rot exceed 125.F (52"C)1. (rJ Steam cleaning is a modification of the hottank alkaline cleaning method, which can be used for preparation of large, unwieldy parts. It will remove inorganic soils and many organic soils from the surface of prns, but may not reach to the bottom of deep discontinuities, and a subsequent solventsoak is rccommended. L1.1.7.5 Ultrasonic Clcaning - This method adds ultrasonic agitation to solvent or detergentcleaning to improve cleaning efficiency and decreasecleaning time. It should be used with water and detergent if thc soil to be removed is inorganic (rust, dirt" salts, conosion products, etc.), and. wirh organic solvent if the soil to be removed is organic (grease and oily films, etc.). After ultrasonic cleaning, pans should be heated to rcmove the cleaning fluid, then cooled to at least 125"F (52"C), before application of penetrant. l{1.1.1,6 Paint Removal - Paint filrns can be effectively removed by bond release soivent paint rernover or disintegrating-type hot-tnnk alkaline paiDt

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strippgrs. In most cases,the paint film must be completely removed to expose &e surface of the metal. Solvenrtype paint removerscan be of the high_viscosity thickened type for spray or brush applicaiion or can be of low viscosity twolayer t)?e for dip-tank application. 80th types of solvent paint removersare gen-raliy used at ambient temperalures, as received, Hohtank alkaline sfippers are water-soluble powder compounds genenlfy used at 8 ro 16 ozJgal (60 ro lZ0 kg/ml of water at 180 ro 200.F (82 to 93.C). After paint removal, the pans must be thoroughly rinsed to renrove all contamination from the void openings and then thor_ ougbly dried. Al.l.l.7 Mechanical Cleaning and SurfaceCon_ ditioning - Metal-removing processessuch as tiling, buffing, scraping,mechanicaltnilling, drilling, reaming, grinding,liquid honing, saniling,Iathe cutring, tumbie or vibratorydebuning,and abrasive blasting,including abrasivessuch as giass beads, sand, aluminum oxide, ligno-cellulosepellets, metallic shot, etc., are often used to rcmove such soils as carbon, rust and scale, and foundry adhering sands,as well as to debun or prorluce a desired cosmelic effect on the parl!.Thet processe: may decrease the ffictiveness of the pc,letront exanli ation by smearing or peening over metal surfaces and flling discontinuities open to the surface, especlall1. for soft meralssuch as aluminum, titaniwn, magnesiun, dnd beryllium allo!. 41.1.7.EAcid Etching - Inhibited acid solurions (pickling solutions) are routinely used for descaling part surfaces.Descaling is necessaryto remove oxide scale, which can mask surface discontinuitiesand orevent penefant from entering. Acid solutions/etch;nts arc also used routinely to renrove smearedmetal that peensover surfacediscontinuities.Such etchantsshould be uscd in acconlancewith thc manufacturers'rccommendations.Caution:
NOTE Al - Etched must bc rinscdcomDletelv Fns and malerial$ free of etchank, rlc surfacc neutralized snd lhoroughly dri;d bi heat prior to application of pnetrana, Acids'and chromates can adverselyaffad thc nuorcscence of fluorcsccnt matcrials. :{OTE A2 - Whneverlhrc is a possibiliry of hyd.ogenembritllemcnt as a resDlt of acid solution/etching,the pan should be baked at a suitable lcmperaturc for an ap?rcpriare time to remove rhe hydrogcn before furthcr proccssing.After baking, rhe part sball be cool.d lo a lempcrsture below 125"F (52.C) bcforo apptyjns penetrants-

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41.1.1.9 Air Firing of Ceramics - Heating of a ceramic pan in a clean, oxidizing atmosphereis an effective way of removing moisture or light organic soil or both- The maximum temperature that will not

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the bomb is of properdesignand constuctionand in good mechanical condition. It is desirable, however, that the bomb be enclosedin a shield of steel plate at least 72in. (12.7 mm) thick, or equivalentprotection be provided against unforeseeable conlingencies. A23 Apparatus AJ.3.l Bonb, having a capacity of rot less than 300 nL, so conslructedthat it will not leak during tbe '!est,and that quantitative recovery of the liquids from the bomb may be readily achieved. The inner surfaceof the bomb may be made of stainless steel or any other naterial that will not be affected by the combustionplocessor products.Materials used in the bombassembly, suchas the headgasketand leadwire insulation, shallbe resistant to hcatandchen)ical action, and shall not undergo any reaction that will affect the chlorine contentof the liquid in the bomb. 4.2.3.2 SanpleClp, plntinum,24 mm in outside diameter at the bottom,27 n)m in outsidediameter at the top, 12 mm in height outsideand weighing l0 to ll g, opaque fusedsilica, wide-fonn with an outside diameter of 29 nrn at the top, a height of lg mm, anda 5-mL c-apacity (Note l), or nickel(Kawin capsule form), top diameter of 28 mltr, 15 mm in height,and 5-mL capacity.
NOTE A2.l - Fused silica crucibles arc mLlcb more economic:rl and longer-bstilg than platinum. After each use, they should be scrubbcd out with 6ne, wer emcry cloth, heated to dull red heal o\r a bum., soaLed in bot wa(fi for I h, then dried alld stored in a desiccator before reuse.

cause degradation of the properties of the ceramic should be used, A1.2 Post Cleaning 41.2.7 Removal of Developer Dry powder developer can be effectively removed with an air blowoff (free of oil) or it can be removed with water rinsing. Wet developer coatings can be removed effertively by waler rinsing or water rinsing with detergent either by band or with a mechanical assist (scrub brushing, washing machine, etc.). The soluble developercoatings simply dissolve off of the p.art with a water rirse.. At.2.2 Residualpenetranrmay be removedthrough solvenr action. Vapor degreasing (10 min minimum), solvent soaking (15 min minimum), and ultrasonic solveot cleaning (3 min mininrum) techniquesare recommended. In some cases, it is desirable to vapor degrease,then follow with a solvent soak. The actual tinre required in thc vapor degreaserand solvent soak will dcpend on the nature of the part and should be determjnedexpcrimentally.

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42.

Methods for Measuring Total Chlorine Content in Combustible Liquid penetrant Materials

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A2.l Scope and Application .1.2.1.1These methods covcr the detemrinationof chlorine in combustibleliquid penetrantmaterials, liquid or solid. lts range of applicability is 0.001 to 5% using . either of the aliernative titimehic procedures. The proceduresassume that bromine or iodine will nor be prescnt- If these elements are present, they will be detected and reponed as chlorine. The full amount of these elementswilt nbt be reported.Chromateinterferes with the procedures, causing low or nonexistentend poinls. The method is appticable only to materialsthat are totally comb,lsrible. A2.2 Summary of Mthods 42.2.1 Tlte sample is oxidized by combustion in a bomb containing oxygen under pressure(Caution, see 42-2.1.1). The chlorine compounds thus liberated are absorbed in a sodium carbonate solutiofi and the anount of chloride present is determinedtitrimetrically eilher against_silvernitrate with the end point detecred potiometrically (Method A) or coulomefiically with the end point detecredby cuEent flox, increase(Metbod B). 42.2.1.1 Satety - Sbict adherenceto all of the provisions prescribed hereinafter ensures against explosive rupture of the bomb, or a blow-out, provided 478

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42.33 Firing lVire, platinum,approximately No, 268&Sgage. 42.34 lgtition Circuir (Note A2.2), capableof supplyingsuf{icient currntto ignire the nylo,r thread or cottonwicking without melting the wireNOTE A2.2rCsution- The swi[chiD rhe ignilion cir<uitshaitbe of s type thar rcnrninsopeo, cxcept when h;ld in closcd posirion by drc opcmror.

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42.3.5Nylon Sewing Thread,or Co on Wickhs, whiteA2.4 Purity of Reagenrs 42.4.1 Reagent gradechemicals shall be usedin all tests. Unless otherwise indicated, it is intended that all reagents shall conform to the specificationsof the Committee on Analytical Reagents of the American Chemical Society, wheresuchspecifications are available. Other gades may be used provided it is flnt ascetained thatrhereagent is of sufliciently high puriry

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to permit its use without lesseningthe accuracyof the ' determination. A2.42 Unless otherwise indicated, refercncesto water shall be understood to meanrefereegradereagent water conforming to Spe4ificatioh D 1f93. A2,5 Decomposition 425.1 Reagen* and,Materi-als: A2.5.7.1Oxygei, free of combustible material and halogen compounds, availableat a pressure of 40 atm (4.05 MPa). A2.5,1.2 Sodiun Carbonate Solution (50 g NazCO/L) - Dissolve 50 g of anhydrous Na2CO3 or . H2O)or 135g of Na2CO3 ^ lOti20 58-5g of Na2CO3 in 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 piece of firing wirc apprcximalely 100 mm in length. Coil the middle section(about 20 mm) and attachthe free endsto the terminals. Arrangethe coil so that it will be aboveandto one sideof the sample cup. Place 5 mL of Na2CO3 solution in the bomb (NoteA2.3),placethecoveron thebombandvigorously shakefor 15 s to distribute the solution over the inside of the bomb. Open the bornb, place the sample-filled samplecup ir the terminalholder,and inserta shon length of threadbetween the firing wire and sample. Use of a sample weight containing over 20 mg of chlorinemay cause conosionof thebomb.The sample weightshouidnot exceed 0.4 g if lhe expected chlorine content is 25Vo or above. If the sampleis solid, not more than 0.2 g should be used. Use 0.8 g of wirite oil with solid samples. If white oil will be used(Note A2.4), add it to the samplecup by meansof a dropper at rbis time (Csution, seeNotesA2.5 nd A2.6).
NOTE A2.3 - Aftcr tepated uscof rhebornbfor chlo.inc determina. tion, a 6lm may bc loticed o! the inncr ru.facc. This dullncss should b retnovedby Friodic polishin8of tic bomb. A satisfactory method fo. doing this is ro iot tc thc bomb in { larhc at abour 300 rpm and polish thc ihside surtaccwith Crit No. 2/0 or cquiyaleor paper coated vith a light rnlchitrc'oil !o prevcnt cutti!9, and then with a paste of grit-frec cbmmic oxrdc atrd watdr. This proccdurc will removc all but vcry dccp prtf and put a high polish on rh surface. Befo.e using thc botrh it shoutdbc wa,rbed rl,itlt rorp srd water !o rcmoveoil or pastclcft from tbe polishingopcration.Bomtls with porous or pincd surfacesshouldncvcr bc used bccauscof thc tendcncy to rctain chlorinc frD|n laqlc to ramplc. Csutlon: Do not use morc lhsn I g total of sanple ad wbitc oil or otherchlorincfrce codbustible matrial NOTE A2,4 - lf |}|e ;;pb is nor radily miscible with whir oil. some other nonlolatil., chloriDc-fr4combustiblc dilucnt may be

TABLE A2.1 GAGEPRESS URES

Pressure, Gage atm (MPa)
Capacityol Bonb, mL

mlna

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300 to 350 38 (3,85) 40 (4.05) 350 to 400 37 C.75) 400 to 450 30 (3.04) 32 0.24) 450 to 500 27 (2.14) 29 Q.94) ^The mlnimumpressures are specifred to proyideslf,icjert oxyget pressures forcomplete present combustion andthe maximum a safety reouirement.

employed in placeof white oil. Howevcr,rhe combiled weighrof samplcand nonvolatilcdilucnr shall not exceedI g. Some sol;d 6dditives insoluble, iro relari\,cJy but mry be satisfactorily bumed whcn covcrEd with a layer of white o;1. NOTE A2J - The practicaof runnirrgattemately sampleshigh and low io chlorinccontentshouldbe rvoided whenever nossibte. It is difficult lo ririselhe lnst traces of cblorinefrom rhe wr'rs ol dc bomband the tendency for residuai chlorineio carry over from ssmpleto samplehas beenobservcd in a nunrber of laboftrtories. Wben a sanplehigh in chlorinehrs preccded one low in chlofinc coDlentlhe lest or lhe Jow-cblorjre sarnple shouldbe repertcdand one or borh of the low valuesthus obtainedshouldbe coDsidered suspect if lhey do DotagEe wirhin lhe limirs of repearability of this tiethod.

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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 the samplefrom the cup) until a pressure is reachedas indicated in Table A2.1.
Note A2.6: Caution - Do nol add oxygenor ignite rhc sampleif the bombhas beeqjarred,dropped, or tilted.

[t2.5.23

Combustion -

Immerse the bomb in

a cold-water brth. Connectthe te:rmina,s to the open electrical circuk. Closethe circuit to ignite the sample. Removethe bomb from the bath after immersionfor at leastten minutes.Release the pressure at a slow, uniform rate suchthat the operatioo requiresnot less than I min. Openthe bomband examjnethe contents. If traces of unbumedoil or sooty deposits are found, discardthe determination, and thoroughly clean thc bomb beforeagair puttingit in use (Note A2.3). A2.6Analysis,Melhod A, Potertiometric Titration Procedure
479

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42.6.1 Apparatus: A2.6.1,1 Silvcr Billet Electode. 2OOI SECTION V

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42.6.7.2Glass Eleulode,pH measurement type. 42.6.1.3 Buret,25-rnLcapacity, gradu0.05_mL ations, 42,6.7,4 Millivolt Mere4 or expanded scalepH metei capableof measuring 0 to 220 mV.
Note A2.7 - An automarictiraror is highly reommended in placc of ilems 42.6.t.3 throuSh A2-6.1.4. Rcpeahbiliry rnd scnsiriviiy of the me[\od are-rnucheDhanced by thc auiomadc cquiprnenl thr'le muchtdiouseffo( is avoided. A2.6.2 Reageus and Materials:

each amount of AgNO3 solution and the amount of difference between the present rcading and the last rcading.Continueadding0.1-mL increments, making readingsand determiningdifferenccsbetweenreadines until a maximumdifference betweenreadingsis o-btained.Ihe total amomt of AgNO3 solution required to producethis maximum dfferential is ihe end ooint. Automatictihators continuously stir the sample,add titnnt, measurcthe potential difference,-ca.lculatethe differential, and plot'the differentialon a chart. The maximum differcntial is taken at the end poinr.
NOTE AZ8 - For mmi[rum 6.lsitiviry, 0,m282 /V ABNO3 sotution may be uscd wirh th. auromaticti!,ator, This dilurc riagent shouta *t blviti largc samplci or whcr chlorine conrJnt *"y b* F_d ovef 0,1% sincc thrsc tesB will cattsc cnd !,oints of l0 mi or hi8hr. Thc large amom( of $,atf urcd io such tit|atioos reduces thc ma-kin8 rhc cnd point ve.rydiffiJr lffrcltirl betwcr re.rdioSs, to detecl Fot chlodnc contcrt! dvcr l% io sample$of O.g or I IarStr, 0.282,lVASNO3 solutiotrwill bc rcquirDdio avoid exc;in; thc lo-n[ *,ater ditution lieit

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42.6.2.1 Acet o ne, chlorine-free.

42.6.2.2 M ethanol, chlorine-frce. 42.6.2,3 Sitver Nitratc Solution(0.0252 N) __ 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 (0.02g2 Nl - Dry a few grams of sodium chloride (NaCI) for 2 h at 130 to t50.C, weigh our t.6480 t 0.0005 s of rhe dried NaCl, dissolvein wrter, and dilute to I Ll 42.6.2.5 Sul,furic Acid (I + 2) _ Mix I volume of conccntratedsulfuric acid (H2SOa.sp. gr l.g4) with 2 volumes of water, A2,6.3 Collcction of Chlorine Solrrtioa- Remove the sample cup with clean forceps and place in a 40OmL beaker. Wash down the walls of the bomb shell rvilh a llne stream of metbanol from a wash bottle, and pour the washings into the bcaker. Rinse anv rcsiduc into the bcaker. Nex(, rinse the bomb cover and terminils into the beaker.FinalJy,rinse both inside and outside of the sample crucible into the beaker. Washiogs should equal but not exceed 100 mL. Add mcthanol to make I00 mL. 42.6.4 Deterntination of Chlorine - Add 5 mL of H2SOa(1:?) ro acidify the solurion(soJution should bc acid ro litmus and clear of whiLeN:r2CO3 precipibte). Add 100 nrl- of acetone. place thc electrodesin the solution, staft the sdner (if ntechanicalstiner is to be used), and begin titrarion. If tikirrion is manual, set tlre pH |lrctcr on the expanded nrjllivolrscaleand note tbe rcading. Add exactly 0.1 mL o[ AgNOr solution fronr the burct- Allow a fcw seconds stirring; then record the new millivolt reading. Subtract the se{ond reading from the first. Continue the tikation, notins 480

42.6,5 Blar* - Make blank determinationswith the amountof white oil rrsedb|]t omitting the sarnple. (Liquid samples normallyrequireonly 0.15 to 0.25 q of white oil while soljdsrequire0.? to 0.g g.) FolloJ normal procedure,making two or three test runs to be sure the results are within the limits of repeatabilitv for the test.Repeat this btankprocedure *henevernew batches of reagents or whiteoil are used_ The pumose of the blankrun is ro measuethe chlorinein *re wtrite oil, the reagents, and thatintroduced by contarnination. 42.6.6 Standardizatioz- Silver nitrate solutions are not permanenuy stable, so thc Aue activity should be checked when the solution is first made uo and then periodically during the tife of the solution.This is done by titration of 6 klown NaCl solution as follows: Prepare a mixture of the amounts of the chemicals (Na2CO3 solution,H2SO4 solution,acetone. and methanol) specified for the test. piDet in 5.0 mL of 0.0282-^NaCl solutionand ijrrateto rhe end point, Prepare andtiuate a similarmixtureof all the chemicals except theNaCI solution, thusobtaining a reagent blank reading. Calculate the normality of the AgNO3solution as follows:
^, _ /YAsNO. = --;;----;;' rA5.0xdx"61
vA

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where: NegNo,: norm;lity of the AgNOj solution, = normalityof the NaCl solution, JVN"cr Vr = millilitres of AgNO3solutiot usedfor the titration includingthe NaCl solution.and

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ARTICLE 24 _ LIQUID PENETRANT STANDARDS

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Vr = millilitres of AgNO3 solutionused for the titration of the reagentsonly. A2.6.7 Calculation - Calculaterhe chlorine content of the sampleas follows:
Chlorine, weight% = (ys- I/a) L x 3'545

A2.7 3 Reagent Preparation: NOTE A2.9 - The nofinal reagentprepara(ionprocess has been slighdy change4 duc to thc itlerfercnce fmm thc 50 rn|, of water aequircdto wssh the bomb. This modified processeliminares the intcrfcrrncc a4d does not alter lhe quality of rlrc tirration.

a
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where: Vs --

a t

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millilitres of AgNO3 solution used by the sample, Va = millilitresofAgNO3solution used by theblank, ly' = normaliry of the AgNO3 solution,and W = gramsof sampleused. A2.6.8 Precision and Accuracy:

M.73J Gelatin Solution - A typical preparation is: Add approximately I L or hot distilled or deionized water to the 6.2 g of dry gelatin mixture contained in one vial supplied by tbe equipment manufacturcr.Gendy heat with contiluousmixing unti] the gelatinis completely dissolvcd. 42.7.3,2Divide into aliquots eachsuffrcient for (Thiny millilihes is enough for one day's analyses. approximately eleven ritrations.)Keep the remainder in a refrigerator, but do not freczc.The solutionwill keep for about 6 nonths in tlre refrigerator.When readyto usetinrmerso the day's aliquotin hot water to liquefythe gelatin. /12,7.33 Glacid AceticAci.l-Nitric Acid SoIutror- A typical parrs ratiois 12.5 ro I (12.5 CII3COOH to I prrt HNO3). 42.7.3.4 Mix cnoughgclatin solution and of acetic acid-nitric acid mixture for one titration. (A qpical mixturc is 2.5 mL of ge)atinsolutionand 5,4 mL of acetic-nitric acid mixture.)
- Thesolution NOTE A2.10 m3ybeprcmjxed in a Iirgerqurnrity for convenience. but maynot be useable afrer24 h, 42.7.3.5 Run a! least thrce blank values and take an avenge according to the operating manual of the titraaor.Determine scparateblanks for both 5 drops of minetal oil and 20 drops of mineral oil. A2.7.4 Titration: 42.7.4.1 Weigh to the nearest0.1 g and record the weight of the 100-ntl- beakcr. 4,2.7.4.2 Removc the sample crucible tom the cover assemblysupport ring using a clean forceps, and, using a wash bottle, rinse both the inside and the outside with water inro the 100-mL beaker. 42.7.43 Empty rhe bomb shell into the I00mL beaker. Wash dou,n the sides of the bomb shell with water. using a waqh bo lc. A2.7.4.4 Remove (he cover assembly from the coyer assembly support, and, using the wash bottle, rinsethe underside,llte plxfinumwirc, and the terninals

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A2.6.8.1 The following criteria should be used for judging the acceptability of resulis: - Results A2.6,8,1,7Repeatability by rhe same analyst should not be considered suspe6t unlessihey differ by more than 0.006%or 10.5%of the value determined, whichever is higher. 42.6.8.1.2Reproducibiliry- Resultsby differ' ent laboratories should not be considered suspect unless they differ by morethar 0.013%or 2l-3% of the value detected, whicheveris higher. A2.6.8.1.3 Accuracy - The averagerecovery of the methodis 86% to 89% of the actualamount present. A2.7 Analysis, Method B, CoulometricTitration A2i7.l Apparatus: 42.7.1.1 CoulometricChloride Titrator. 42.7.1.2 Beakers, two, 100-mL, or glazed crucibles (preferably with ly2 in.-outside diameter bottom). 42.7.7,3Ref ri gerator. 42.7.2 Reagents: A2.7:2,1Acetic Acid, Glacial. A2.7-2.2 Dry Geladn rtixure. A2.7,2.3 Nitric Acid" L23.2.4 Sod.iwn Chloride Solution- 100 meq C/1. Dry a quantityof NaCl for 2 h at 130to 150.C. Weigh out 5.8440 g of ddedNaCl in a closed r 0.0005 container, dissolvein water,and dituteto I L.
481

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?001 sEcTIoN v
43. Meahodfor Measuring Total Ftuorine Contentin CombustibteLiquid penetrant Materlals A3.I Scope and Application 43.1.1 This methodcoversthe determination of fluorine.incombustible liquid penetrantmaterials,liquid or solid, that do not containappreciable amounti of intcrfcring elemen6, or haveany insoluble residueafter combustion. Its range of applicability is I to ?00 000 ppm. A3.1, Themeasure ofthe fluorine content emDlovs the fluorideselective ion eleckode. A3.2 Summary of Method
(r - B)x M Chte,rinr, ncighr q" -

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inro the same 100,-mL beakcr. The total amount of washingsshould be 50 t I g. 42.7.4.5 Add specifiedamounrsof gelatin mix_ turc and acetic acid-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 of washings includiog the decomposedsample. t2.7.4.6 TilJate usjng a coulometric titrimeter, according to operaiing manual proccdure. 42.7.5 Calculationr - Calculate the chloride ion concentration in the sample as fojlows:

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where:
R -

counter reading obtajned with the sample, averagecouoter readingobtainedwith average of the threeblank readings, standardizationconstllnt.This is dependent on the insLnrment ran8e sc(ting in uje andthereading obtainedwith a known amount of the 100 rneq of Cl per litre ol solurion, and weight (]f silmpleuscd.g.

A3.2.1The sampleis bxidizea Uy combustion in a bomt containing oxygen under pressure (Caution, see A.3.2.1.1). The ffuorinecompounds thus liberated areabsorbed il a sodiumcitrate solutionandthe amount of fluorine present is determinedpotentiometrically throughthe use of a fluorideselective ion electode. 43.2.1.1Safety- Strict adhercnce to all of the provisionsprescribed hereinafcer ensuresasains( explosive rupture of the bomb,or a blow_out, provided the bomb is of properdesignand consrrucrio;and in good mechanical condition.It is desirable,horvever. that the bomb be enclosed in a shield of steel plare at leastyz in. (12.7mrn) thick, or equivalent protection be providedagainstunforseeable contingencies. A3.3 Intcrferences A33.1 Silicon, calcium, aluminum, magnesium, and othermetals formingprecipitates with fluoride ion will interfere if theyarepresent in sufficientconcenr.ation to exceed thesolubilityof theirrespective fluorides. Insoluble rcsidue after combustion will entrainfluorine evenif otherwise solublc. A3.4 Apparatus A!.4.1 Bonb, havinga capacityof not less tha,l 300 mL, so constructed that it will not leak durins the test, and that quantitativerecovery of the liquidi from the bomb may be readily achieved.The inner surfaceof the bomb may be made of stainless steel or any other material tbat will not be affected by the combustion process or products. Materialsusedin the bombassembly, suchas the headgasketand leadwire insulation, shallbe resistant to heatandchemical acrion, and shallnot undergo any reaction that will affect the fluorinecontentof the liquid in the bomb.

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A?.7,6 Precisiottand Accurrtcy: 42.7.6.1Duplicate results by the same operator canbeexpcctcd to cxhibitthc following rclati.,,c standard deviations:
Ajrproxinr:rte % Ctrlorinc 1.0 and above

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0.1 0.003

RSD,% 0.l0 2.5 5.9

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42.7.6.2 The nlethod can bc expectedro rcport yalucs thilt t,ary from the truc valuc by the follorving anrounts;
0.1% chlodne and abovc 0.001 to 0.01% cl orine 12 !g%.

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42.7.6.3 If brominc is present, 36.52d cf the true amountwill bc reported. If iodineis present, 20.720 of the true amount will bc repcrtcd, Fluorine will not be detected. 482

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ARTICLE 24 _ UQT'ID PENETRAM STANDARDS

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A3.4.2 Sample Cnp, nickel, 20 inm in outsidc diameter at the bottom, 28 mm in outsidediameterat the top, and 16 mm in height;or platinunr, 24.mm in outside diameter at the bonom, 27 mm in outside diameter at the top, 12 nm in beight, ard weighing l0 to ll g. A3,4,3 Firing Wire, p[1ins61 approximatelyNo. 268&Sgage. 43,4.4 lgnition Circuit (Nol@A3.l), capableof supplying sufficient cunent to ignitr ttt nylon thread or cotton wicking without melting the wirc.

4353 Fluoride Solution, Stock (2000 ppm) Dissolve4.4200 r 0.0005 g of predried(at 130 to 150'C for I h, then cooled in a desiccator) sodium fluoridein distilled water and dilure to I L. 43,5,4 Oxygen,free of combustible materialand halogen compounds, rvailableat a pressure of 40 atm (4.05 MPa). !t3.5.5 Sodiun CitrarcSolution* Dissolve27 c of sodiumciuate dihydrate in waterand dilute to I L: 435,6 Sodium Hydroxide Solution (5 N) - Dissolve 200 g of sodium hydroxide(NaOH) pellets in wateranddiluteto I L; store in a polyethylene container. 43.5.7 WashSolution(Modiled TISAB,Total lonic Strength AdjustnentBuffer)- To 30CmL of distilled water, add32 mL of glacialaceticecid,6.6 g of sodium citrdtedihydrate, and 32.15g of sodiumchloride.Stir to dissolveand thcn adjust the pH to 5.3 using 5 ir' NaOH solution.Cool and dilure to I L. A3.5.8 lVhite Oil, refined, 43.6 Decomposition I,rocedure A3.6.7 Prepuration of Bomb and Sample- Cut a piecof firing wire approximately 100mm in lengthCoil the middle secrion(about20 mm) and artachthe free endsto the terminals. Arrangethe coil so that it will be above andto onc sideof thesample cup.place 10 mL of sodiumcirate solutionin the bomb. Dlace the ccver on the bomb, and vigorouslyshakefor 15 s to distribute the solutionover the insideof the bomb. Openthe bomb,placethe sample-filled samplecup in the terminal holder,and inserta shod lengthof thread between the firiqg \.vireand the sample.The sample Weightusedshould not exceedI g. If the sampleis a solid, add a few drops of wbite oil at this time to ensurcignition of the sample.
NOTE A3.3 - Us of sampteweiShts conrriningovcr 20 mg of cmori& may cause conrsion of thc bomb. To avoid this ir is rccommended that for samplescontaining .over 2% chlorine,the sample vcight be basfd on rhe foltowingrrble: Chlorinc Sample Whire Oil Content,% wclgor,g weighi,g 0,4 0.4 5rol0 0.2 0.6 l0 to 20 0.1 o.7 20 ro 50 0.05 0.7

NOTE A3.l Caudon - The rwiich in tl|c ignitiol cfucuitshall be of a typc that aEains opcrl crccpt Eheo h.ld id closcl posirion by thc opcr"ator.

43,4.5 Nylon Sewing Thread ot Corton Wicking, white. 43.4,6 Funnel,polypropylene (Note A3.2). 43.4,7 Volumetric F/as( polypropyleng 100-mL (Note A3.2). A3.4.8 Beaken polypropyleng 150-mL (Note A3.2), ' A3.4.9Pipet, 100-pL, Eppendorf-type (NoteA3.2). 43.4.10Magnetrc.Srirer andTFFcoatd magnetic stirring bar. A3.4,ll Fluoide Specifc lon Electrode and s\itable refercnce electode. 43.4.12 Mi ivob \leter capableof measuririgto 0.1 mV.
NOTE A3.2 - Classwareshouldncvcr bc uscdto baddb e nuoride solution as it *ill removefluoddr ioss ftold solutioD or on sub$equeot usecarry fluoride ion from a cooccntratd solutiotrto ode dhrc dilutc.

A3.5 Reagents 43.5,1 Purity of Reagerrr- Reigentgradechemi calsshallbe usedin all tests. Unless otherwise indicated, it is intended that all reagentsshall conform to the specificatioasof the Committeeon Analytical Reagents of the American ChemicalSociety,wherc suchspecificationsare available. Othergr-ades may be used,provided it is 6rst ascertainedthat the reagent is of sufficientlyhigh purity to perrnitits use without lessening the accuracy of the determination. A35.2 Punty of Water - Unlessotherwiseind! cated, all referencesto water shall be understgodto 'iiiter meanTlpe I reagent conformingto Specification D l193.
483

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Caution: Do not usc more than 1 g total of sample and white oil or other fluorine.freecombustibtematerial. A3.6.2 Addition of Orygen - Place rhe sample cup in position and anange the nylon tbread, or wisp of cotton so that the end dips into the sample.Assemble the bomb and tighlen the cover securely.Adnlit oxygen

sE-165 TABLE A3.1 GAGEPRESS URES

2001SEcTtoNv 43.7.4 Add 100 pL of stockfluoridesolutionand obtain the readingafter the samelength of time necessary for 43.7.3. A3.8 Calculation
40 37 32 29

Gage Pressurg atm ([4Pa)

Capacity oF8omb,:nL 3 0 0t o 3 5 0 350 to 400 400 to 450 4 5 0t o 5 0 0 min! 38 30

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.43.8,1 Calculate the fluorineconaent of the samnle as follows:

prcssrlre! " The minimum arc specifred to provide sufficient orygen for Complete combustion pressLlres present andthemarimum a safety requrfemeni.

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(Caution, Note A3.4) slowty (to avoid blowing the sample from the cup) until a pressureis reached as indicatedin Table A'3.1. - Do noraddoiygcn NOTEA3.4:Caution or ignitethcsample jarred, if tbf bornb hrs been dronpcd, or titted, 43.6,3 Conbustion - lnmerse the bomb in a cold-wxter barh. Connect the terminals to the open electrical circuit. Close rhe circuit to ignite the sample. Renrove the bomb fiom the bath after immersion for at leas( 10 rnin. Release the prcssure at a slow, uniform rate such thai the operation rcquircs not less than i min. Open the bomb and exanrinethe contents_ If traccs of unburned oil or sooty deposits are found, discard the determination, and thoroughly clean the bonrb bcforc again purringir in usc, 43.6,4 Collectiort oJ Fluorine Solution - Remove thc samplceup with clcrn ftx.ccps and rinsc with wash solution into a 100-mL voluncrric flask. Rinse the walls of thc bomb shell witL a fine streamof wash soludon front a wash bottlc, and add the washings to the dask. Ncxt, rinse thc bornb cover and terminals into thc voluntctrjc flrsk. I:inalJy,add wash solution to brirs lhc cottcnts of tl)c llxsk to thc lir)c. A3.i I,rocedure r\.1.7.1Ascenaiurhc slole (nrillivolrsper ten-fold changc irr conccntration) of rhc clectrode as describcd bv tl)c nrrnuliclurcr. A3.7.2 Obrain a blrnk soiutionby perfomring the procedurewithorrt a sarnplc. A3,7.3 Imll'Ierse the fluo de and reference electrodcs in solutionsand obtain thc equilibriumreading to 0.1 mV. (The condirionof tL)e electrode deiermines thc lcnglh of tine necessary to rcach equilibrium. This may be as littlc rs 5 nrin or ls ntuch as 20 min.) 484

wherc: ,CE| = pi11iuo1t in sarnple solution on addition "hange of 100 pL of stock fluoride solution, 482 = q;111uo1, iir blank solution on addition "hange of 100pL of the srockfluoridesolution, S : slope of fluoride electrode as determined in A3.7.1, and W : gramsof sample. A.3.9Preclsionand Bias - The results 43.9.1Repearability of rwo determinations by the sameanalyst should noi be considered s[spect unlessthey differ by more than 1.1 ppm (0.00011%) or 8.0%of the amounr detected, whichever is greater. - The results of two deter43.9,2ReproducrbrTiry minations by different laboratorics ihould not be consideredsuspect unlessthey differ by 6.7 ppm or 129.0% of (hc anlountdetccted, whicheveris greatcr. 43.93 Bl'as- The average recoveryof the method is 62 to 64% of the amountactuallypresentalthough 83 to 85Vorecoveries can be expectedwith proper technique. '

A4. Determinationof Anions by Ion Chronratography lvith Condustiyity Mexsutement A4.1 Scopcand Apptication A4.1.1 This rnethod is condensed fiom ASTM procedures and APHA Method 429 and cDtimized for the analysis of detrimental substances in oisanic based materials, It provides a singleinstrumentei technique for rapid,scquential measuremcnr of commonanions suchasbromide, chloride, fluoride,nitrate, nitrite,phosphate,and sulfate.

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ARTICLE 24 _ IJQUD PENETRANT STANDARDS

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A42 Summary of Method A4.2.1 The material.must be put in the form of an aqueoussolution before analysiscair be attempted. The sample is oxidized by combustion ir a bomb containing oxygen under, oressuraThe productsliberated are absorbedin the eluant present in the bomb' at the time of ignition: .This solution is washedfrom the bomb, filtered, and.diluted io a known volume. L4.2.1.1A nftena afquot of sampleis injected into a steam ofcsrbonate-bica6onate eluantandpassed through a series of ion exchangers. The anions of interest are separakd on the .basis of their relative affinities for a low capacity,stotrgly basic anion exchanger (guard and separator column). The separated anions are directd onto a stotrgly asidic catiotr exchanger(suppressor columa) wherethe-yarc converted to their highly conductiveacid form and the carbonatebicarbonateeluant is convertedto weakly conductive carbonic acid. The separated anionsin their acid form are measuredby conductivity. They arc identified on the basis of retention time as comparcdto standards. of peak arca or peak Quantitation is by measurement height.Blanks are prepared and analyzed in a similar fashion. - Any substance A4.2.2, Inrerferences that has a retentiontime coinciding with that of any anionto be determined will interfere. For examplgrelativelyhigh concentretionsof low-molecular-weight organic acids interfere with the deteminationof cblorideand fluoride. A high doncentrationof any one ion also interfercs with the resolutionof others. Sample dilution over@mes many interferences. To resolveuncertairtiesof identifcatior or quantitationuse the methodof known additions. Spuriouspeaksmay rcsult from contaminants in reagentwater, glasswarc, or sampleprricessing apparatus. Because small samplevolumesarc used,scrupulously avoid contamination. -The L423 Minimum Detectable Concentration minimum detectable@ncentrationof an anion is a function of sample size and corductivity scale used. Generally, detectable concentrations are in _rninimum the 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.L sampleloop and a lGpmho nrll-scalesettingon the conductivitydetector. Similar valuesmay be achieved by using a higherscale seningandan electronic integrator. A4.3 Apparatus A4.3.1Bomb,h'aving a capacity of not lessthan 300 mI-, so constructed that it will not leak durine

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the test, and that quantitdtive recoveryof the liquids from the bomb may be readily achicved.Tbe inner surfaceof the bomb may be made of stainless steel or any other materialthat will not be affectedby the combustion process or products. Materialsusedin the bomb assembly, srichas the headgasketand leadwire shallbe resista[tto heatandchemicdaction, . insulation, and shall not undergoa.nyreaction that will affect the chlorineconrentof the liquid in the bomb. L43.2 SampleCu2, platinum,24 rnm in outside diameter st the bottom,27 mm in outsidediameterat OIetop, 12 mm in heightoutside, and weighing lO to ll g; opaquefused silica, wide-formwith-an outside dia$eter of 29 mm at the top, a height of 19 mm, and a 5-mL capacity(Note A4.l), or r,ickel (Kawin capsuleform), top diameterof 28 mm, 15 mm in height,and 5-mL caplciry.
wOTB e+.t - Fusedsilica ctrcibles are ,tuch morE economical and longer lasting thar plali !nl. Afrer cach use, they shouldbe soubtrd out with finE, wet emcry clolh, hearedro dull red heat ovcr a bllrr,r,soated in hor wrter for I h tben dried and srored itr a desiccatorbelore reuse,

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1t4,33 Firing lVirc, platinum, approxin.atcly No. 26BandSgage. '443.4 lgnirion Ci?.c it (Note A4.2), capable of supplying sufficicnt curent to ignite the nylon threrd or cotton wicking without melting the wire. NOIE A4.2:Clution- Theswitch in theimi(ioncircuilshalt bc of a g'pc thatrcmrins opcn, crccplwhenlrct,lin cloredposition by ihc oPcrator. A43.5 Nyloz Scwhg Tlvead, or Corton Wicking, whiie. 443.6 lon Chronatogrcph, including an injection valvg a sample loop, gurrd, separator,and suppressor columns,a temperature-compensated small-volume conductivity cell (6 tr,L or less), and a strip cban recorder capable of full-scale response of 2 s or less. An electronicpeak integrator is optional. Thc ioo chromatograph shall be capable of delivering 2 to 5 mL eluant/ min at a pressure of 1400 fo 6900 kPa. 1t4.3.7 Anion Separator Column, wi:h styrene divinyl-benzene-basedlow-capacity pellicular anion-exchange resin capable of resolving Br., Cf, F-, NOj-, NO2-, PO43-, and SO+?-;4 x ?50 mm. 4,43.8 Guard Colwnn, identical to scparator column except 4 x 50 mm, to protect scpacatorcolumn frcm fouling by prrticulrrcsor orrlnics.

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2001 SECTIONV t\4.3,9 Suppressor Column, h\gh-capacitycationcxcbange resin capable of convettilrg aluant 3nd separated anions to their acid forrns. /14.3.10Syringe,minimunl capacityof Z mL and equippedwith a male prcssurefitring. A4,4 Reagents 44.4.7 Purity of Reagenl.r_ Reagent grade chemisals shall bc uscd in all cests. Unlessotfierwiie indicated, it is intended that all reagentsshall corform to the specificationsof thc Committec on Analydcal ReagenrJ of the American Chcmical Socicty, where such specificatlons are available. Othcr grades may be used, provided it is first ascertainedthat the reagent has s;ffi_ ciently hlgh purity to permit its use without lessening tlle accuracyof tllc determinijtion. 44.4.2 Deionizcd ot Dis ed lVater, free ftom intcrferences at the mininum detection limit of each consttucnt and llltcred through a 0.2_p,m membrane filrer to avoid plugging columns, 44.4.3 Lhttut,Sct/utrorr, scdiurnbicarbonate-sodium carbonare, 0.003ir,1Nal{cor- 0.0024M Na2coj: dissolve 1.C08g NallCO3 and 1,0176 I NazCOjin water and dilure to 4 L. 44.4.4 flagcncruutSolutiou I, H1SOa,I N, use Ihls regencrant \\ltcl sullprcssor is not a continuously rcgenerated ooc_ 44.4.5 Regcnerant Solnbn 2, H2SO4,0.025 N, dilutc 2.8 nL conc I.{2SO4 to 4 I_ or 10Crnl- regemrant solutjon I to 4 I_. Use tltis rcgenerant with continuous regeneration fiber suppressor svstcrn. 1,4.4.6 Srandtrd Atrian Solutiotts,100 n)g/L, preparc :J sericsof rtlndard aniorrsolutionsby weighing thc indicatcdrnlolrnt.of sait,dried io I constant weight at 105"C, ro 1000 mL. Srore jn plastic bottlesin a refrigerator; these solutious arc stable fot at least one nrorth.
S:Jt

Iight; containsl0 mg/l- eachof Cl-, F, NO3-, NO2-, and POa'-, I mg Br-lL, and 100 mg SOa2-/L. preparc fresh daily. 44.4.8 CombinedWorkingStandanl Solution,lnw Range- Dilute 100 mL combined workins standard solution, high range,to 1000mL and storei-na nlastic bottle protectedfmm light; contains 1.0 mslL each Cl-, F, NOi, NO2-, and pO43_, 0.1 mg ni-rt, anO l0 mg SO42-/L. Prepare fresh daily. !14,4.9 Altemative Combined Working Standnrd Solutions hepare appropriate combinations ac_ cording to anion concenhationto be determined. If NO2-andPOaL are not included,the combinedworking standard is stablefor one month. procedure A4.5 Decomposition 44,5,1 Preparation of Bomb and Sample_ C.tt a p_iece of firing wire approximately 100 mm in length. Coil the middle section(about20 mm) and artachthe free endsto the terminals. Arrangethe coil so that it will be aboveand to onesideof the sample cup. place 5 mL of Na2CO3/NaHCO3 solutionin the bomL.olace the coveron (he bomb,and vigorously shakefor 15 s to distribute the solution over the insideof the bomb. Openthe bomb,placethe sample-filled samp)e cup in the terminalholder,and insena short lenethof thiead betwcen the firing wire and the sample. The sample weightusedshouldnot exceedI g. If the samplei( a solid,add a few dropsof whire oil at this ri;le ro ensure ignition of the sample.
NOTE A4.3 - Use of samplcwcighrsconr.aining ovcr 20 mB ol cnrofine may cause corrosion of the bonb. To avojd rhis ri i, rcommcnded rhar for samplcs containingovcr Z% chlorinc, lhc sample weight be basi on the follorvinp: Chlorine Samplc White Oil .ontent, weight, werghl.I t 2to5 0.4 0.4 Jro l0 o.2 0.6 l0 (o 20 0.1 0.7 20 to 50 0.05 0,/

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t.IlrNorNo:_ PoorSooz-

clL t_6485 2,2too r.2876 | 3101 L4998 1.4330 l.8l4l

l.*aCl NJIIr NxNOr NaNOr KII2I}O: KrSO4

L4"4.7 Conbircd \4orking StandardSolution,High Rtlnge * Conlbinc i0 nrL of thc Cl-, F, NO3-, NOz-, and POa3-standrrdanion solutions,I mL of the Br-lnd 100 nrl ol rhc SO4l- sl:rnLlrrrd solutions, dilute to 1000 nrl-, ald store in a plastic bottle protectedfrom 486

CAUTION;Do not usemor!fur I g totalof:sainple andwhileoil ol o(her fluorine-free combustible maGrial. 44.5.2 Addition oI Oxygen _ place the sample cup in position and arrange the nylon thread, or wisp of cotton so that the end dips into tbe sample,Asscmble the bomb and righten the cover securely. Admir oxygcn -ttre (Caution, Note A4.4) slowly (to avoid blowing sample from the cup) until a pressure is reached as irdicated in Table A4.1.

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NOTE. - Do notaddorygcnor igniterhesrmple A4.4:.Caution

rr tnc t'omb las bcen jarrcd, droppcd, or tjlted.

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ARTICLE 24

UQUID PENETMNT STAN'DARDS

sE-16s

TABLE 44.I GAGEPRESSU RES

nL Capacity of Bomb,
300 to ,50 350 to 400 400 to 450 450 to 500

Pressures, Gage atn ' mina rnar 38

.37

30 27

' The mlnlmum pressures are speclfed to provide sufficient oxygen prcrentasatety pressures for complete combustion andthemaximum requirement. I f, 10 rl '!

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A4,53 Combustion- Irnmerse the bomb in a cold-water bath. Connect the terminsls to the open electrical circuit.Closethe circuitto igdte the sample. Removethe bomb from the bath after immersion for Release pressure a irt leastl0 min. the at slow,uniform requiresnot less than 1 rate such that the operation min. Open the bomb and examinethe contents. If oil or sooty are found, traces of unbumed deposits discard the determination, and thorougltlyclean the bomb beforeagainputtingit in use. - Remove the samA4.5.4Collection of Solution ple cup with clean forcepsand rinse with deionized water and filter the washingsinto a 100-mL volumettic flask. Rinse the walls of the bornb shell with a fine streamof deionizedvater ftom a wash bottle, and add the washings through the filter paperto the flask.Next, rinsetbebombcoverandterminals andaddthewashings through the filter into the volumetricflask. Finally, add deionized water to bring the contentsof the ffask to the line. Use aliquots of this solution for the ion (lC) analysis. chromi.tography 44.6 Procedure A4.6.1SystemEquilibration -'lurn on ion chromatograph and adjusteluantflow rate to appmximate the separationachievedin 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-aseline indicates.equilibrium conditions. Adjust detector offset to zem-out eluadt conductivity; flow with the fiber supprcssor adjuiJtthe regeneration rate to maintainstabiliay, usually2.5 to 3 ml/min. in accord44,6.1.1 Setup the ion chromatograph ance with ihe manufacturer's instructions. containing L4.6.2 Calibrabn - Inject standards a singleanionor a mixturcanddetermine approximate retentiontimes. Obsen ed times varv with conditions
48"t

F I G ,A 4 . 1 T Y P I C A A L NION PROFILE

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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 n calibrltion curve by plottingpeak height and construct or area againstcolcentration on lincr grapl) paper. Recalibrate whenever the deteclor setting is changed. With a system requiring suppressorregenention, NO2ilteraction with thc suppressormay lead to enoneous minaLiononly when the NOt results;make this dcter is at the same stage of exhaustion as during suppressor 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 for F analyzestandards or Cl-, To eliminrtc lhis inlcrferencc, that bracket the expected result or elinrinate the water dip by diluting ihe samplc with eluant or by adding concentrated eluant to the silmple to gjve the same as in thc clurnt. If sample HCOt/COJ- concentration adjustments are made, adjust stand rds and blanks identically.
Watcr dip .)ccurs bccausc wilcr cooductivity ir NOTE 44.4 sample is less lhan eluant conductivity (luanl is dilutcd by water)-

44.6.2.1 lt linearity is established for a 3iven detetor setting, it is acceptable to calibratc. with a single standard. Record dre peak height or area and retentiontime to pernrit calculationof tlie calibration factor. F. - RenrovesanrplepanicuA4.63 SampleAnaly.rr.r lates, if necessary,by filtering through a prewashed 0.2-pm-porediam menrbrane filtcr. Using a prewashed

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sE-165

2001 sEcItoN v
, TABLE A4.2 PRECISION ANDACCURACY OBSERVED FORANIONS AT VARIOUS CONCENTRATION LEVELS IN REAGENT WATER
SiogleAmaunt Amount overall operator Signifrcant Added, Found, Preclsion, Precision, Bias95% Aniofl mglL mg/L ms/L nglL Level
F0.48 F4.84 ct 0.76 cF 17 455 cf N0, ,,0.45 Nor 2r.8 Bf0.25 Br13.7 Pooto.t8 Poot0.49 N0r0.50 N0rt5.l 0.49 4.b4 0.86 r7.2 471 0.09 19.4 O.25 72,9 o.1o o,i4 0,3) 14,8

syringe of 1 to l0 mL capacity equipped with a malc luer fitting inject sample or standard. Inject enough sainple to flush sample loop several times: for 0.1 mL sample loop inject at Icast I mL. Switch ion chromatograph from load to injcct mode and rccord peak heights and retentjontimes on strip chart recordcr. After the last pcak (SO42-) has appeared and the conduccivity signal has returned to base line, another sanlple can be injected. - For systemswithout fiber 44.6.4 Regenerati.or suppressorregeneratewith I N H2SOain accordance with the manufacturer'sinstructionswhen the conductivity base line excecds 300 pmho when the suppressor column is on line. A4.7 Calculation 44,7.1 Calculate cr.nccntrationof each anion, in rug/L, by refcrring to the appropriatecalibration curve. Alternatively, when the responseis shown to be linear, use the following equation:
C = H x l : x D rvherc: C = ntB anion/L.

0.05 0.52 0.38 0.82

46

0.09 0.04 1,0 .0.06 0.15 0.16 0.07

soorS0o'-

o.5r
43.7

0.52
43.5

0.O3 0.46 0.11 O,41 13 0.04 1.3 0.02 0.6 0,03 0.I7 0.03 0.9 0.03 2,?

No No No No No Yes,neg Yes,neg No llo Yes,neg Yes,neg No No No No

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peak height or arca, response flctor - conceltration of standard/ hcjght (or arca)of srandard, and dilution factor for thosesamples requiringdiIulion.

A4.E Precisionand Bias A4.E.1Samples of reagentwater to which were addcdthe commonanionswereanalyzed in 15 laboratories with the resultsshown in Table A4.2.

488

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liquid Penetrcnt Inspection

Revised by J.S. Borucki. Ardrox Inc., qnd Gqil Jordon, HowmetCorporofion LIQUID PENETRANT INSPECTION is a nondestructivemethod of revealing discontinuities that are opento thc surfaces of $olid and essentially nonporousmaterials. Indications of a wide spectrum of flaw sizescan be found regardless of thc configurationof the workpieceand regardless of Ilaw oricntations.Liquid penetrantssecp into varioustypes of minute surfaceopeningsby capillaryaction.Bccause ofthis, the process is well suitedto the detection ofall typ6 of surface cracks, laps, porosity, shrinkageareas, laminations,and similar discontinuities, It is extensively usedfor the inspection of wroughtand cast productsof bothferrousand nonferrous metals. Dowder metalluryy parts, cemmics, plastiCs,and gLass objects. In practice,the liquid penetrantprocess is relatively simple to utilize and control. The equipment usedin liquid pnetrant inspectioncan vary from an atmngement of penetraflt, simpletankscontaining emulsifier, and developer to sophisticated computer-controlled processing automated and inspectiansystems.Establishing procedures and standardsfor the inspction of specific partsor productsis criticalfor optimumend resulls_ The liquid penetrantmethod does not dependon fe.romagnetism (as does, for example, particleinspection), magnetic and lhe arrangement ofthe discontinuities is not a factor. The penetrant methodis effective not only fo. detecting surface flaws in nonmagnetic metalsbut also for revealing surfaceflaws in a variety ofother nonmagnetic materials.Liquid penetrantinspectionis alsousedro inspectiremsmadefrom femomagnetic steels;generally, its sensitivityis by the intemal hydrostaticpressureof the liquid, Whenthe liquid comesinto contact with a solid surface, the cohesive fo.ce responsible for surface tension competes with the adhesiye force betweenthe molecules of the liquid and the solid surface. Theseforcesjointly determinethe contact angle,0, between the liquid and the surface (Fig. l). If 0 is less than 90" (Fig. la), the liquid is said to wet the surface, or to have goodwettingability: if the angleis equalto or greater than 90' (Fig. lb and c), the wettingability is considered poor. Phyrlcol Pdaclpler Closely relatedto wetting ability is the Liquid penetmnt inspection depc[ds phenomenon of capillaryriseor depression mainly on a penetmnt's effcctivclywetting (Fig.2). Ifthe contactangle,0, between the the surfaceof a solid workpicceor speci- liquid and the wall of the capillarytube is men, flowing over that surface to folm a Iessthan 90' (that is, if the liquid wets the continuous andreasonably uniformcpating, tubewall),the liquid meniscus in the tube is and then migratinginto cavities that are concave,and the liquid rises in the tube opento the surface. The cavities of interest (Fig. 2a). If 0 is equal to 90', there is no are usuallyexceedingly small,often invisi- capillarydepression or rise (Fig, 2b). If 0 is bleto the unaided eye,The abilityofa given greatrthan 90", the liquid is depressed in liquid to flow over a surface aDd enter the tubeanddoesnot wet the tubewall, and principallyon the the meniscus surfacecavitiesdepends is convex (Fig. 2c). In capilfollowing: lary rise (Fig. 2a), the meniscusdoes not pull rhe liquid up the tube; rather, the a Clearliressof tbe surface hydrostatic pressure immediately under ahe . Confrguration of the cavity meniscus is reducedby the distributionof . Cleanliness of the cavity the surfacetensionin the concavesurface, . Size of surfaceopening of the cavity and the liquid is pushedup the capillary . Surface tensionof the liquid tube by the hydraulicallytmnsmittedpres. Ability ofthe liquid to wet the sudace sureof the atmosphereat the fre surface of . Contactangleof the liquid the liquid outsidethe capillarytub. Figure The cohesive forcesbetween molecules of a 3 clearlyshowsthe forcesthat causeliquid liquid cause surface tension.An example of to rise in a capillarytube. the influence of surface tefision is the tenThe height to which the liquid rises is dency of free liquid, such as a droplet of directly proportionalto the surfacetension water, to cotrtlact iDto a sphere. In such a of the liquidandto the cosine of the angleof droDlet.surface tensionis counterbalanced contact,and it is inverselyproportionalto greater than that of magnetic particle inspecnon. The major limitation of liquid penetrant inspection is that it can detectooly imperfcctionsthat are opento the surfacaisoma other mcthod must be used for detecting subsurfaceflaws. Another factor that can limit thc us of Iiquid penetrdntsis .surface roughness proor porosity. Such surfaces duce excessivebackgroundand interfcrg with inspection.

good well n9

f ig.

y1'ff"tT:fi:jics

o5trl@id

by ihe onsle. e, hrrwn

d droplel of liquid ond c rclid *rfoe.

Good *{ine

t obtoiftd *hd 0 < eo'(o); poor wnin. w}ln

72 / t$erhods of Nondestructive Eyqluqtion

E!o Ri! or dep'e|rion in sdloll vcrticol copillo.y lub.!, drerniid by d' conrod ongl 0, breno liquid a .qilhry h,b. Io) g < 9C: dpilldrt ris. (b) 0 = 9o': m @pillory deFdrion or ds. (c) 0 > 9Oo:coFillory d.pr.lsion

the density of the liquid and to the radius of the capillary tube. If, as in Fig. 4, the capillarytube is closed,a wettingliquid will still rise in thc tube: however.there will be extra pressureresulting from the air and vapor compressedin the closed end of the tube, and the capillary rise will not b as great, These examples of surfaca wetting and capillary rise illustrate the basic physical principles by which a penctrant enters fine surfacc discoltinuities even though the practical cirCumstances encounterdin the use of liquid penetrants afe more complex than the6eexamplesmay suggest. Cracks, for example,are not capillary tubes, but simulate the basic interaction betweena liquid and a solid surface, which is responsible for the migration of penetrants into fine surface cracks.

offe.J.d hy lhe comFer*d ak fttrcpFd in th .lord .nd. Cohpore highr of liquid in tube +an i. Fig. 3 wi$ rhot in the tubs hre.

Fis. 4 rH"ifu'*fi ,:sHiiil"l,*ff;

The viscosityof the liquid is not a factor in the basicequationof capillaryrise. Viscosity is related to the rate at which a liquid will flow under some appliedunbalanced stress;in itself, viscosityhas a negligible ability. In general, effect on penetrating however,very viscousliquids are unsuitbecause ahey do not flow ableaspenetmnts rapidly eoough over the surface of the they requireexworkpice;consequently, cessivelylong periodsof time to migrate into fine flaws. property of a peneAnother necessary an adetant is its capabilityof dissolving quateamountof suitable fluorescent or viscompounds. Finally, the penetrant ibl-dye with a suitable liquid must be removable or emulsifier without presolvenUremover cipitatingthe dye. Just as it is imponant that a penetmlt flaws,it is alsoimportant that entrsurface the penetrant be retained in the flaws and emergefrom the flaw after the superficial coatiflg is removedfrom the surlaceand the is applied.It is apparently a pardeveloper adox that the sameintemctionbetweena thatcauses the liquidro liquidanda surface for entera fine openingis alsoresponsible from that opening.The resoits emergence lutiol of the paradoxis simple:Once the penetrant hasbeenfreedofexcess it surface to th entrapped liquid, becomes accessible which, under the effect of the adhesive forces betweenliquid and solid, spreads over the newly cleanedsurfaceuntil an (Fig. 5)is attained equilibriumdistribution Alrhough i|t some casesthe amountof penetrant in a surface beadat equilibrium to be detected visually, sensiis sufficient tivity is vastly increased by the use of a developer, of which there are several typs available(forms A, B, C, and D)When applied, a developerforms a fine system surfacefilm, that is, a spongelike of very fine, randomcapillarypaths.If the penetrant contactsthe powder,the powder then competeswith the freshly cleaned for the penetrant surfaceof the workpiece as it flows out of the defect. If thc devel-

Doriiward lorc (Fd) k qual to the weisht of th liquid colurm: Fd= zTtrzhEo Upward lorce (r.!) i.s qual to the surlace tension tim th FeiiBete! ot the Eeruscus: Fg = (?cos d) (2rrr) Wher r i! the inside rsdius of th capiUary tube, I ;s th hisht oI the liquid in th tube, a is accteratior due 1o sravity, , is deDsity ol the liquid, ? is sudace tnsioD, and 0 is the contact anale. .t Sdmoti. rho{,ins th. fcrc, invod in E:r rU' e .(pillory rie, th6 dowMrd fo@ from Eisln of *E lhuid Golumn,qnd $c uorord foe {rm 3urloctsrrion oloog tl|. m.ni!.!3 p.rin6i.r

oper is properly designed,it readily adsorbs the pnetrant from the flaw. The penefiantcontinues to migrateby capillary action, spreadingthrough the devloper until an equilibrium is reached. This migrating actiofl is illustmted schernatically in Fig. 6. The visibility of thc entrapped

rc*pixe rurfoce, ttn pcmlront rcmoir ns in o dii.onlino'ty Grcrg! b rhc srfo.. u.lil on cquilibr,um F

Fis. s H:ffi:iH:"fl9#**:

Liquid

Pentrant

lnsPection

/ 7

method A test . Water washable, sensitivityof the kerosene-and-whiting could be increased by hitting the object . Postemulsifiablelipophitic, metho'd B binctestedwith a hammerduring testing r Solventremovable,method C hydrophilic, methodI Th iesultingvibrationbroughtmore of the . Postemulsiliable keroscneout of (he cracks and onto the whitewash.Althoughthis test was not as Thesefour methodsare describedbelow. Wotsr-worhoble Penetrqnl (meth( sensitiveas those derived from it, it was quick, inexpensive, and rearonablyaccu- A) is designedso that the penetrao! from the surface rate.Thus. it orovideda vast improvement diiectly water washable not dos require a scp workpiece; il the over ordinaryvisualexamination. now rate emulsification step, as dos tl The first stepladiu to the methods penetrantmethods.h cr of the fluo- postemulsifiable availablewas the devetopment process workpiecesquickly at used lo be process R.C. Switzer. by rescentDenetrant This liquid, used jointly wirh a gr'owder efliciently. Ir is important, however, th developer, brought penefiart iNpction the washing operation be carefully co penetran water-washable from a relatively crude procdu.e to a more trolled because The esse to overwashing. pene- are susceDtible With fluolescent scieotificoperation. trant. minutc flaw$ could be readily detcct- tial operaiionsinvolved in this melhod a in Fig. ? schematically od wien erposedto ultravioletlight (com- iltustrated (mtho. monlvcalledblacklighO.This devlopment Portemulsifiqble peneirqnt$ th-detecti( ensure to designed ond D) are the I in breakthrough major a Denetrantwithin the flaw is greatly in- repreiented of minuic flaws in some materials.The' of detection of surfaceflaws. or enlargement ircasedby thc spreading are not directly water washabl the devclDenetrants included also work Switzer's thc indication. this chat"acteristic,the d&nger' of llcause meththe visible-color contrast oDment of the penetrantout of the flaws over'rashing od, which allowed for inspectionundcr tvolutlo.| ol tho Prccerc Althougi not as sen- reduced,The difrercnc betwen the wat white light conditions. method lies Tho exact origin of liquid penetrant in- sitive as fluorcscnt penetrantinspection' it washableand Dostemulsifiable an ;mulsifier prior to final rinsiD sDection is not known, but it has been is widely used in industry for noncritical the use of de- The emulsifier rEkes the tesidual surfa' Throughthe developments that the method evolved from the inspection. a.ssumed soluble in water so that the exce Dnetrant pentmnt inspection abov", liquid that the rust on a crack in a observation penetrant can be removal by tl "cribed surface inspecnondestructive a rnaior has bgcomc somewhat was plate storage in outdoor rteel water rinse. llerefore. che emu.lsificatit heavierthan the rust on the adjacentsurfac' tion method. must be carefully controlled so that tl time esas a result cf water seepitg into the crack surfac Dnetnnt bcomeswater soluble b to helped it had th oxide forcing out and Pe||slr.tnt molhcdt the oeretrant i( the llaws does not. T1 was a that oroduce.The oblious conslusion in the postemulsifiab involved opeAtions differences among vast Becauseof the iiouid purposelv introduced into surface illustrated schematicallyin Fig are has method it penetrant ilspection. for applicarions would again brought out then cri"t. ind syslemand in Fig. 9 for tl biin necersaryto refine and developth for the lipophil;c revealthe locationsof thosecracks. Despitc the addirion system. penetrants (lyp trvdropfrlfii I, lluorescent, of The or y material that fulfilled the known two tvDes steDs involvedwith the postemu Droc4ssins basic melhods into four tisible) rl, and tiire good wettability, viscosity, criteria of low Ihe wide variationsin rhe sfiabte rnerhoitsS and D, ths methodsa II was to accommodale and readvavailabilitywaskrosene. the most reliable for detecting minute flaw! principal factors: wider cracks following found,however.thai although Solvent-rcmovoblc Penctrqnl (methc wete someons showedup easily, finer being ofthe workpiece condition a Surface is availablefor use when it is necessal G) times missedbecauseof the difficully of insDcted onlv a localizedaf.eaof a wor' to insoct detectirig,by purely visual means,the small o Chtracteristias of the flaws to be dtectinipect a workpiece at the si piecc to or ffom them. exuding amounts of kerosene ed on a production inspectionb than iather The Eolution rvas to provide a contrasting . Time and placeof inspection the same tyPe of solvent sis. Normally, surfacthat would reveal smaller seepages o Size of the workpiece precleaning and for removing e used for of whiteThe propertis and availability o Sensitivityrequired pe[etrant process penetranl. This cess washmadeit the loeicalchoice'This meth' the rangeofapp and broadens convenient classihed od, known as thi kerosene-and-whiting The four melhodgare broadly penetrantinspections.Howeve cations of years. The a5: for many test, was the standard

rrg. c fflilij"" ti""ilJif ;:ll*,'hffif:

operoiion 2
W o t e r - w o s hr e m o v o l o f l i q u i dp n e l r o n tf r o h s u r f o c e

t ig,

ri*

**tlot

op"rqtiqr {s liquid Fdncrtqir inip'<iion q3i's rh worera$hoble !v5r'h

74 / Methods of Nondestructivc Evoluqtion

Emulsifid liquid penel.qni

O9rotion I Applicotio n o f liquid to su.toce Denelronl

oFerotio.? aoplicotio on t muGilie/ to liouidoenerronr

OpeErion 3 Combination oI emulsifiera.d liquid peneiranr mG rd

Operotion 4 Woter,rssh removol of l q o i d p e n e l r o n tf r o m s u r f o c e

Fig.

op"."rion'

1i" odd ion ro prlcteonins) for the poltenuliiffobls,

lipopl'ilic

liquid F.l'.tront

sy.r.m

becausethe solvent-removable method is labor intensive, it is not practical for many production applications, When properly conductedand when usedin the appropriate applications, the solvent-removable method can be one of the most sensitive penetrant methodsavailable.The operations for this process are illustratdschematically in Fig. to. Whicheverpenetralt methodis choseo, the degree and speed of excess pnetra[t removal depend on such processingcondi tronsas spmy nozzlecharacteristics, water prcssure afld temperature, duratioD of lhe nnse cycle, surfaceconditionof the workpiecc,aDdinherentremovalcharacteristics of the penetrant employed.

De3.rlptior

ol the Procerr

Regardless of the type of penetrant used, that is, fluorescent (type I) or visible(type II), penetrant iospectioo requires at least five essential steps,as follows. Surfqce Prrpqrofion. All surfaces to be inspected, whether localized or the entire workpiece, must be thoroughly cleanedand completely dried before being subjectcdto penetrant impection. Flaws cxposedto the sudac&mustbe free Fom oil, water. or other contaminattsif they are to be detected. PenetEtion. After the wod(piecc has treencleaned,pcnetrant is applied in a suitable mannet so as to form a film of the penetrant overthe surface. This film should

Prerinse, wateFwash

Application of emulsifie. !o l(qui<tpenetrani

rmainon the surfacclong enoughto allow maximumpenetration of the penetrant into any surfaceopenings that are prcsent. Removol of ExcssPenelrcnt. Excess penetrant musl be rcmoved from the surface. The removal method is detrminedbv thc lype ofpenetrant used.Somepenetranti can be simply washed away r ith water; others require the use of emulsifiers (lipophilic or hydrophilic) or solvent/removcr, Uniform rcmoval of excess surface penetrant is necessary for elTective inspection. but overremoval must b avoided. Developmsnt.Depending oD the form of developing aBent to be used,the workpiece ls driedeitherbeforeor directlyaffer application of the developer. The developer forms a lilm over the iurface. It acts as a blotter to assist the natural seepageof th penetrant out of surface openings and to spread it at the edges so as to enhance the penetrana indication. Inrpedion. After it is sufficientlydeveloped, the surfaceis visually examinedfo. indications of tnnetrant bleedback from surface openings, This examination must be performed in a suitableiospection environ. ment, Visible pcnetrantinspectionis per. tormed in good white light. When fluores. cenl pentrant is used, inspection is performed in a suitablydarkened areausing black (ultraviolet)light, which causesthe penetrant to fluorescebrilliantly.

E m u l s i f i e dl i q ! i d p e n e r r a n t

foterlols Ulod ln Petrotr{rnl Incpecilon

In additionto th penetrants themselves, liquidssuchasemulsifiers, solvent/cleaners and removers, and developers are required for conducting liquid penetrant inspection, Penetr.onls Thereare two basictyps of penetrants:

Operation 4 Coftbination of emutsifier and liq!id penel.ant

Ope..fon 5 Watepwash rcmovat ol tiquid pe^etant hom surtacs

a Fluorcscent, type I . Visible,type II Each type is availablefor any oneof the four

Fig.

9 ory..t"-

ro p{dldnins)ror E poitemulsifioble. 1i"oddition srhod D, hydropl'ilic tiquid penronr methods (water washable, postemulsifiable

lipophilic, and postemulsifiablehydrophilic,

Liquid Penetrcnt

Inipection

/ 7l

. Operolion I Applicorion ol liquid pnetront lo surfoce

Operotion e Solvnlcleoner removol of liquid penelront trom swfoce

Opfoiio. 3 Applicotion of

O p e r o l i o n4 Inspction

Fig.

tO

Op-"ri"*

1inoddirion ro pr6<loonins)for th6 lohenr-dnavobb liquid Fi.tnt

ly3tsm

and solventremovable) mentionedin the section "Penetra[t Methods" in this article. lype I fluorscent penet]lnt utilizes peoetrants that arc usually green in color and tluorescebrilliantly uder ultraviolet light. The sensitivity ofa fluoresceat pnetrant dependson its ability to form indications that appearas small sourcesof light io an otherwise dark area. Type I pcneffants are available in dillerent sensitivity levels classified as follows; t/2| . Level Ul ralow a Lerel li Low . Level 2: Medium o Level 3: High . Iatel 4i Ull.J.a,high lype ll visible penetrqnt employs a penehant that is usually red in color and produces vivid red indications in contrast to the light backgound of the applied developr under visible light. The visible pe[etrant ildications must be viewed under adequate white light. The sensitivityofvisible pen+ trants is regarded as Level I and adequate for many applications. Peneliqnt selcctionqnd u:e dependon th criticaliry of the iDspectioD, tbe condition of the workpiece surface, the type of ptocessing, and the desiredsensitivity(see the section "Selection of Penetralt Mthod" in this article). penetrcnts Method. A, water-washable are designed for the removal of excess surface penerant by water rinsing directly after a suitable penetmtion (dwell) time. The emulsifier is incorporatd into the water-washable penetraot. When this type of penetrant is used, it is extrcmely important that the removal ofexcess rurface pnetrant be properly controlled to prevent ovrwashing, which can cause the pnetraot tb be washed out of the flaws. Methods R and D, Iipophilic ond hydrophilic postemulsiftablepenetranl,t arc itl.soluble in water and therfornoare.novablcby water rinsing alone.They are designedto b selctivelyremoved from the surfacof the workpieby the useofa separate emulsifier. The emulsifrer,properly appliedand lft fo. a suitable emulsificationtime, combines with the excesssurfacepenetrantto form a waterwashablesurfacemixture that can be rinsed
a_-.

from the surfaceof the workpiec.The pnetrant that remains within the flaw is not subject to overwashing. However, proper emulsificationtime must be establishedexperimentallyand maintainedto ensure that overcmulsification,which results in the loss of flaws. doesnot occur. penelrunts MethodC, solvent-rcmovable by wipingwith clean,lint-free are removad materialuntil most tmcesof the penetrant have beenremoved.The remainingtraces by wipingwith clean,lint-free are removed material lighdy moistenedwith solvent. This type of pcnetrant is primarily used whre po.tability is required aDd for the areas.To minimize of localized inspection the possibilityof removingthe peoetrant the use of excessive from discontinuities, anounts of solventmust be avoided. Phyricol ond Chemicol chorcterirtic.. Both fluorescent and visible penetrants, postemulsifiable, or whetherwater washable, solventremovable,must haYecenain chemiif tbey are to cal and physicalcharacteristi'cs perform theirintended functions, The princiare asfollows: pal rquirements of penetrants

. Chemical stability and uniform physical consistency . A llash point not lower than 95 'C (200 "F); penetrantsthat have lower flash points constitute a potential fire hazard . A higlt degreeof wettabiliry a I-ow viscosityto permit better coverage and minimumdragout . Ability to penetratediscontinuitiesquickly and completely . Suffrcint brightnessand permanenceof color . Chemicalinenness with materials being iospectd and with containers . Low toxicily lo protectpersonDel . Slow drying characteristics r Ease of removal SolYent Cleoner/Removers . Inoffensive odor Solvent cleaner/removersdiffer fron . Low cost in that they removexcesssur emulsifiers . Resistance to ultraviolel light and heatfade face pentrantthrough direct solvent a( tion. There are two basic types of solven Emulsifiers removers: flammable and nonflammable free ( cleaners are essentially Emulsifiersare liquids used to rendet Flammable penetmtlton lhe surfaceof a work- halogens but are potential lir hazardl excess piecewaterwashable. Thereare two meth- Nonflammablecleanets are widely use( ods used in the poslemulsifiable methodl Howevr,they do containhalogelatdso

methodB, lipophilic,andmethodD, hydrc philic. Both can act over a range of du rations from a few seconds to severa minutes,depending on the viscosity,co! ceritmtion, method of application, an, chemicalcompositionof the emulsifier,a well as on the roughness of the workpiec surface.Th6 length of tirDe an emulsifie shouldremainin contactwith the penetrar employe, depends on the type of emulsifier ofthe workpiece surface andthe roughness Method B, lipophilic emulsilierr are o: areusedas supplied, based, andfunctionb: difrusion(Fig. ll). The emulsifierdiffuse film alld rendersit spon into the penetrant in watgr.The rate a taneously emulsifiable which it diffuscsinto th penet.antestab time. The emulsi lishesthe emulsification fier is fast acting, thus making the emul sificatiol operation very critical. Th, to act as long as it is ir emulsifier continues contactwith the workpiece;therefore,th, shouldtake placequickly tr rinseoperation cation. avoid overemulsifi Method D, hydophilic emulrifiers ar, water basedand are usually supplied a concentrates that are diluted in water t concentrationsof 5 to 30% for dip applica tions and0.05to 5% for sprayapplications Ilydrophr'lic emulsifiers function by displac ing excesspenetrantfrom the surfaceof th, part by detergent action(Fig. l2)- The forc ofdil of the watersprayor the air agitation tanks providesa scrubbingaction. Hydro philic emulsitieris slower acting than th, lipophilic emulsifier;therefore,it is easre action.In additiol t( to controlthe cleaning the emulsifierapplication,method D alsr wate a coarse requires a prerinsc,UtiliziDS helpsremovethe exces. spray,the prerinse of th to minimizecontamination Denetrant Lmulsifier.Of greater significarce,only ; very thin anduniformlayerofpenetrantwil remainon the surface,thus allowingeasl removalof the surfacelayer witb minimun from th opportunityofremovingpenetrant flaws. This step is required bccauseth penetrant is not misciblewith thehydrophil ic emulsifier. The penetmntmalufacturer shouldreco[ mend nominal emulsificatioo times for th spciJiq typ of emulsifierin use. Actu, emulsification times should be determine for the particular applicatior experimentally The manufacturershould also r@ommen the concentrationsfor hydrophilic emulsif, ers.

76 / lvlerhods of Nondestrucllye Evoluslion

_ Required PEpertioi. To carry out |ls Iuncttonsto the fullest possibieextent, a oeyeloper must have the following proper_ ues ot characterislics (rarely are all rhese characteris(ics presentto optimumdegrees rn any gven materialor formulation,but all must be considered in selecting a develop er): a The. developer must be adsorptive to Solutlon .ad dfitlsion maxrmize blottinq o It musthavefine-grain sizeand a particle shapethat will disperseand exposerne penetrantat a flaw to produce strong and sharply defined indications of flaws a It mustbe capable ofprovidinga conrrasr background for indicationswhen colorcontrastpenetrants are used a It must be easvto aDDlv . It mustform aihin. uniiorm coatingouer a surtace a k mustbe easilywette.d by the Denetrant Diffu.ion p.oceds at the flaw (the liquid must be allowedto Ai.sing spread ovcr the particlesurfaces) Flg. | | er-'*.r. n rt* frD.iioni,rs ot tipopriticeNtsifir, . It must be nonfluorescent if used wilh fluorescent penetrants vents, which may render thern unsuitable cations and the visible contrast of visible- I It must be easy to removeaftcr inspeclor some applications. uon penetrantindications. The developeralso a It must not contain ingredientsharmful to surfacepenetrantis removedby provides a blotting action, which .Excess sirves to wprng, usinglint-freecioths slightlymoisr- draw pnetrantfrom within pans being inspctrd or to equipment the flaw to the enedwith solventcleaner/remover. usedin the inspection lt is [ot surface,spreading operation the penet.ant and eDlargIecommended . It mustnot containingredients that cxcess penekant ing the appeamnce surface harmfulor of the {law, be_ rcmovedby flooding the surface with toxic !o the oprator The developer i$ a critical part of the solvent cleaner/remover, becausethe sot_ rDspction process;borderlineindications Developer Fonns. There are four foms vent will dissolvethe penglranlwithin the that might otherwise b missdcan be mads of developers in commonuse: defectandindications willnot be produced. visibleby the dvelopr. ln all applications . Form A, dry powder of liquid penetrantinspection,usc of a Developers developer is desirablebecauseit decreases a Form B, water soluble of a developer is to increase inspction.timeby hasteningthe appear- o Form C, water susDndible . The purpose the bnghtness a FormD; nonaqueous intensityof fluorcscentindi_ anceot tnotcallonssolventsuspendible The characteristics of each form are discussedbelow. .Dry powder developers (form at are wrdely used with fluorescena penetrants, but should not be used with visible-dye penetrants because aheydo not produca saustactory contrastcoatingon the surface or-lhe workpiecc,Ideally, dry powder deveropers shouldbe light and fluffy to allow lor easeof applicationand shouldcling to dry surfaces in'a fine film. The adherence of the powdershouldncitbe excessive, lhmor36 in rqueous as the amountof black light availablero energze lluorescent indications will be reduced. For purposes of storageand handhng as wellas appllcations, powdersshouldnoi be nygroscoprc, andthey shouldremaindry. If thcy pick up moisturwhen storedin areas of highhumidiry. rheywi losetheirabiliry to flow anddust easily,and they may agglomerate. pack. or lump up in containers or In developer chambers. For reasons of safe(y.dry powderdcvelopersshouldbe handled with care.Likc anv Agit.tion.nd otherdustparticle, Rinsing it can dry the skin ani omutsiricaiiod tmtate the lining of the air passages, causlng rmtation.Ifan operatorwill be working Fig. t 2 Ebmenr, in d,e frJ.oionins of Lydrophitic ed,kiti.rs conlrnuously at a deveioper station, rubber

Liquid Penetrqnt

Inspection

/ 77

operations are varietyof produclioninspection gloves and respiratorsmay be desirable, idg action beginsat once. Workpieces in a shoner periodof than the visible penefant methods,which Modern equipmentoften includesan 9x- ready for inspction are utilized primarily for localizedinspecspraybooth time. haustsystemon the developer are clasdevel- tions.As statedearlier,penehants Nonaqueoussolvent-suspendible dust chamber that prcor on the developr type: ventsdust from cscaping. Powderrecovery opers (form D) arc commonlyusedfor both sifiedon the basisof penetrant filtcrs are included in most such installa- the fluarescent and the visible penerant t Iype fi Fluorescent produces a | process. This form of developer tions. rype /I: Visible Water-solubledeveloperr (fom B) caltrbe white coating on the surface of the part. . MethodAi Water washable white col- . (type I) or visible This coatingyieldsthe maximum usedfor both fluorscent MethodRi PostemulsifiableJipophilic (typeII) postemulsifiablc or solvent-remov- or contrast with the red visible penetrant a MethodCt Solventremovable fluoresWater-soluble developers indication and extremely brilliant able pnetrants. . MethodD, Postemulsifiable-hydrophilic for use with water- cent indication. are not recommended devel- Penetrants are also classifiedin terms ol penetmnts, Nooaqueoussolvent-suspendible because of the potenwashable con- sensitivitylevels: in the ready-to-use tial to wash the penetrantfrom within tlle opcrsare supplied flaw if the developeris not very carcfully dition and contain particles of developer a Level t/2',Ultralow in a mixtureof volatilesolvents. a Level li l-,ow controlled. Water-solubledevelopersare suspended for their c supplied as a dry powder concenhate, The solventsare carefully selercd Level2: Meditm in water ilr recom- compatibility with the penetrants.Non- t Level 3: Iligh which is then dispersed developers proportions, solvent-suspendible usually from 0.12 to aqueous mended o Level 4: Ultrahigh 0.24WL (l to 2 lb/gal.).The bath concen- also contain surfactants in a dispersant gravitywith whosefunctionsare to coat the padicles Advqnlqger qnd limifolions of Pcnfor specific trationis monitored trqnl or agMethodr. Each pcnetrant method, reduge their tcndency to clump the appropriat hydrometr. Necessary and (either lipophilic wbethcr postemulsifiable includecor- glomerate. constituents of the developers devel- or hydrophilic),solventrcmovable,or waNonaqueoussolvent-suspndibl rosion inhibitorsand biocides,The advanusing fluorescentor visibletages of this form of developer are as fol- oDersare the most sensitive form of devel- ter washable, oper usedwith type I fluorescentpenetr&nts dye pcnetrants, has inherent advantages lows: the solvent action contributesto and limitations. . The prepared bath is completely soluble because andadsorption mechanisms, The postemulsifiable the absorption fluorescent peneand therefore dos not require any agita- In many cases wher tight, small flaws tran, methodis the mosl reliableand sensi tion the dry powder (form A), water- tivc pc[etrant method,This procedurewill . The deyeloper is applied pdor to drying, occur, (form B), and water-suspndible locate wide, shallowflaws as well as tight soluble the development time thus decreasing (fom C) developersdo not contact the cracks and is ideal for high-productio0 . Thc dried developerfilm on the workpiece eotrappeC pnetmnt, This results in the work. On the other hand, emulsification is completely water soluble and is thus failureofthe developer to createthe neces- requiresan additionalopration,which ioessily and completely removed following sary capillary action and surface tnsion creases cost. Also, this methodrequiresa inspction by simplewaterrinsi[g that serve to pull the penetrant from the water supply and facilities for inspection (f(nm C) ca solvent-suspendibleunder black light. The postemulsifiable, flaw. Th nonaqueous lVater-suspendible developers into lipophilic fluorescentpenetrantmethod is entemthe flaw aoddissolves be used with either fluorescnt (typ I) or developer visible (type II) penetrants.With fluorescent the penetrant.This action increasesthe less seositiveand less reliable than the penetrant, the drid coating of developer volume and reducesthe viscosity of the hydrophilic method. Its use is therefore must not fluoresce,nor may it absorbor filter penetrant.The manufacturermust carefully declining. The solvent-rcmovable select and compound the solvent mixture. fluoresce4lpene' out the black light used for inspection. water-suspfldible developersare sup- There are two types of solvent-basedevl- trant methode$ploys a proceduresimilal plied asa dry powderconcenkate, which is ooers: nonflammable(chlodnated solvcnts) to that usedfor the postemulsifiablefluoresthen dispersedin water in recommended a;d flammable (nonchlorinated solvents). cent method,except that cxcesspenetranl Thit proportions, usuallyfrom 0.(X to 0.12kg/L Both types are widely usd. Selectionis is removedwith a solvent/remover. for spot recommended (% to I lb/gal.).The amountof powder in basedon the nature of the application and methodis especially inspection or wherewater cannotbe conve. suspension must be carefully maintained. the type of alloy beingirlspected. dently usd, It is mor sensitivethan th( Too much or too little developr on the system, but thc gxtrem( water-washable surfaceof a workpiece can seriously afrect 3olecrlon ol caution and additional time required for sensitivity.Specificgravity checks should PenGt clt mdhod solventremovaloften precludeits use. be conducted routinely,usinga hydrgmeter The waterwashable fluorescent pene' to check the bath concentration.,Water- The size, shape, and weight of worksoluble developers contain dispersing pieces,as wcll as the number of similar trant methodis lhe fastestof the fluorescenl It is also highly sensitive,reli to be inspected, ofteninfluence procedures, agents to help retardsettlingand cakingas workpieces It can be economical. able,and reasonably well as inhibitorsto preventor retard cor- the selection of a pnetrant method. degree used for both small and large workpieces Sen itiyity ond Coit. The desired rosion of workpiecesand equipment,and How' on mostpart surfaces. and cost are usuallythe most andis effective biocidesto extend the working life of the of sensitivity aqueous solutions. ln addition, wetting important factors in selecting the proper ever, it will not rliably reveal open, shalagents are prcsentto ensureevencoverage penetrantmethodfor a given application. low flaws ifoverwashedand in somecases. sensi- dependingon the sensitivity level of th capable of the greatest of surfacesand ease of removal after in- The methods tivity arealsothe mostcostly.Many inspc- penetmnt,will not loatethe very tightesr spection. requirethe ultimatein sen- cracks. There is also the dangr of over watr-suspendible developeris applied tion operations numberin washing by applyingwater for an excessive before drying; therefore,developingtime sitivity,but therearea significant sufficien canbe decreased the heatfrom the which extreme sensitivityis not required periodof time or with a pressure because results. to rmove th penetrant from the flaws. drier helps to bring penetrahtback out of and may evenproducemisleading penThe postemulsljiable visible Penetrun On a practical basis,the fluorescent surfaceopenings. ln addition,with the developerfilm alreadyin place,the develop- etEnt methodsare employedin a wider method is used whenever sensitivity re

78 / fllethods of Nondestrucfive Evoluation

quhed is greaterthan that providedby the water-washable visible penetrantmethod, However. the addirionalstep of applying emulsifier makesthis sys(em more costly than the water-washable visible pcnetrant dye methodthat requireswater, but otherwise no locationlimitationsare imposed. The solvent-retuovable visiblepenetrunt methodhasa distinct advantage in that all the necssary ingredients are portable;ac. cordingly, it can be used in a practically limitless number of loations,both in the shopand in the field. Bccause of the Droblemsinvolvedin penetrant removal,however, the methodis genrally confinedto spot inspectionor to inspectionunder circumstances that prohibit the useof other methods because of workpiecesize or location. The watetwashable visible peneuant Jy.rtea is the fastest and simplest of all peneuanttechniques.It is, however, the least sensitivebecausethg prletfant is likely to be removedfrom wide, shallowflaws. Therefo.e,it is most useful in those applications where shallow and relatively wide flaws are not significant.This method is also the least sensitavefor locating tight cracks.It rcquiresa water source,but can be performedin almost any locatioo becauseneithpra darkened area nor electricity is required. able and reusable, and this has led to the adoption of the expendable technique for some very large workpieces.In this technique, penetrant is sprayed over the workpiecein a penetrantstation similar to tne one mentioried previously. The penetra[t is pressure storedin a separate tank ntted with a hoseand a spray nozde. The spray booth is not equipped with a sumpto recoverexcess penetrant. lnstead,the booth is fitted with water spraynozdes and a dmin so that it can serve the multiple purpose of draining and washing.A decision to use the expendabl The drain or dwell stations are aatually techniqueand related equipment should b roller-topbenches that holdthe partsduring based on a careftrlanalysisand considerarion the processing cycle. The usual arrange- ofcost,time,raleofproduction, andhandling ment is to positiona drain or dwell srauon proDlems. following each of the dip tanks, the wash Emuhifier Stqtion. The emulsifierliquid station,and the drying ovn. The suoun[s is contained in a tank of suflicicntsize and are describedin more detail below, depthto permitimmersion ofthe workpreces. PcnetrqntStqtion,The principalrequire- eitherindividually or in batches. Coversare mrt of a penetraotstatioDis that it provid sometimespmvided to reduce vaporafion, a means for coating workpieces with and drain valves are supplied for cleanout penetrant----either all over, for small work- when the bath has become contaminated. pieces,or over smallareasof large work- Suitabledrain racks are also a part of this pieceswhen only local inspcction is re- stationand are usedto prmit excessemulsiquircd. In addition, means should be fier to drain back into the tank, provided for draining penetht back excess If largeworkpieces must be coatedwith into the penetrant reservoir, unlessthc ex- emulsifier, methods must b devised to pendable technique is beingused,Draining achieve the fastestpossible coverage. Mul. racks usuallyservethc additionalpurpose tiple spraying or copiousflowing of emulsi. of providinga storage placefor partsduring fier from troughs or perforated pipes cafl be the time required for penetration(dwell used on some typcs of automatic equip umet. ment. For the local coatingof large worxSmall workpieccsare easily coated by pieces,spraying is often satisfactory, usug dippingthem into a resewoirof penetrant. the expendable technique described for the This may be doneindividually or in batches application of peoetmnt. in a wire basket, Prc- qnd Porhinse Slotionr. The warer The peneftant aontainer should be rinsing (washing)of small workpieces is equipped with an easilyremovable coverro frequently doneby hand,eitherindividually reduce evaporationwhen not in use. A or in batchesin wire baskets.The workdrain cock shouldalsobe providedto facil- pieces areheldin the washtank andcleaned itatc drainingof the tankfor cleaning. Con- with a hand-held spray using water at tap tainersare usuallymadeof steel,but stain- pressure andtemperature. The washtrough le$s steel containers should be used with or sink should be large enough and deep penetrants. water-base enough so that wolkpieces can be easily For large workpieces, penetrantis often tumed to cleanall surfaces. Splashshields applied by spmying or flowing.This is done shouldseparate the rinse statidnfrom premainlyfor convenielcebut also for econo- ceding (pnetrantor emulsifier)and iucmy, because (wet devgloper) the volumeofpenetmnt need- ceding stations. Rinsesta. ed to immcrse a large objectmaybe sogreat tio s are alwaysequipped with at leastone as to increaaeunnecessarily the original ultiaviolet light so that the progressof recost of installation,A small reservoir of movaloffluorcscent peletrantcan be easily penetrantequippedwith a pump, a hose, followed. anda $prayor flow nozzle is usuallyalmost The automatic rinsing of small work" ai fast a meansof coatinglargeobjectsas pieces is satisfactorily accomplishedby the dippingoperation, For this type of op- meansof a rotating table. Tbe basket is eration,the penetrant stationconsistsof a placedon the table, and water-spray heads suitably ve[tilated booth with a rotatable are properlylocatedso as to rinse all surgrill plaiformon whichthe workpiece is set. facesof the workpieces thoroughly. A drain under the platform retums peneSpecially built automatic washers for trant runofTto the sump,from which it is rinsing workpiecesthat are large and of pumped back to the spray nozzle- The irregularcontou are often installed.Spray prevents bqothenclosure the overspraying nozzles must be locatedto suit the individof penetrant on areasoutsidethe penetrant ual application. statroo. The removalof excsspenetrant by simIn somcapplications, it hasbeenfoundthat ply submerging the workpiecein water is only a smallamountof penetrantis rcover- generally nor recommended. However,in seriesof modular $ubunits.Each subunit performs a special task. The number of subunits in a processing line varieswith the typ of penetrantmethodused. The subuntts are: a Drain and/ordwell statiols a Penetrant and emulsiner stations a Pre- and post-wash stations . Drying sation a Developerstation . Inspcctionstation . Cleaning stations

Equlprnent Requliomontr
The quipmentused in the penetrantinspection processvaries from spray or aerosol cansto complex,automated, computerdriven processingsystems. Some of the moregenerally usedtypesofequipmentare described in the followingsections. Portcble Equipment For occasional inspections, especially in the field, where equipmentponabiliti is ncessary, minimalkits for eithervisibleor fluorescentpenetrantinspectionare commercially available. (Cenemlly, portable penearant applications are limited to localized areasor 6pot inspections rather than entirepart surfaces.) Sucha kit for visiblepenetranr inspection work includes a preclaner,a pnetrant, and a penetrant removerand developr, all in pressurized spraycans.Penetrant removal requireswipi.rg with lint-free cloths or papertowels. A similar kit is availablefor fluorescent work; a precleaner, a penetrant,penefant removr and developerare likewise supplied in pressurized cans.Cleaning ir aicomplished by wiping wirh lint-free cloths or papertowels. This kit includesa small, ponable black ligh( for conducringrhe insPection. Stotiondry Inspection Equipment The type of equipmentmost frequently used in fixed installationsconsists of a

tiqurd Penelrdnt Inspection / 7'

some cases,simple submersion in an airagitated water bath is satisfactory. The rinse stationis subjectto corrosion,All steelshouldbe protectedby rustproofingand painting. Mo$ sarisfactory,but more cos0y, is the use of stainless 6tcelequipment, Drying Stqtion. The rccirculating hot-air drier is one of the most importantequipment The drier must be large enough components. to easily handla the type and number of workpiecesbeing inspected.Heat input, air of workpieces flow, and rate of movement through the drier, as well as tempemture control, are all factorsthat must be balanced. The drier may be of the cabinet type, or it may be designedso that the workpiecespass tliough on a conveyor.Ifconveyor operation is usd, the spedmust be consideredwith thc required drying cycle, arefrequent. Electric-resistance elements ly used as sources of heat, but gas, hot water, and steam are also used. Heat input is controlled by suitably located thermoby workpiecesize, statsand is determined and Iate of movement. composition, equipment invariablyincludes Integrated the recirculating hot-air drier mentioned previously.Makeshiftdriersare sometimes becausenothing better is availused----often able. Elctric or gas hot-air blowers of commercialdesign have been used, but is possibecause oo controlof temperature and are ble, these are very unsatisfactory basis. ordinarilyusedonly on an emergency Infrared lamps are not suitablefor drying washed workpieces,becausethe radiant heatcannotbe readilycontrolled. Equipment designedto handle workpicesof specialsize and shaperequiresa speciallydesigneddrier- Each drier is a problem involving a engineering separate special combination of workpiece composition, mass, surfacearea, speedof movcunique to ment, and other considerations the circumstances, DevelopsrStqtion.The typ andlocation ofthe developr stationdepend on whether dry or wet developer is to be used. For dry developer, the developer station is downstramftom the drier, but for wet developer precedes it immediately the drier, following the rinse station. The dry4eveloper starior.usually consists of a simple bin containingthe powder, Dried workpiecesar dipped into lhe powdr, and the excess powder is shaken off. targer wo*pieces may not be so easilyimmersdin the powder, soa scoopis lsually providedfor thmwing powder over the surfaces, after whichthe excss is shaken off. The developer bin shouldbe e4uippdwith an asily rcmovablecover to protectthe developrfrom dust anddirt when not in use. Dust control aystems are sometimes used.Control rcededwhendry developeris across is accomplished by a suction opening the back of the bin at the top, which draws off any developer dust that rises out of the air is passedthrough bin. The dust-laden dust filter bags,from which the developr can be reclaimedfor further us (Fig. l3). Developer powder can also b applied This systemrequiresno with air pressure, bin, but it doesrequirea boothor a cabinet and also makesdust collectionmandalory. Equipmenlfor the automaticapplication of dry developer consists of a cabinet through which the dried workpieces are passedon a conveyor. The air in the cabinet is laden with dust that is kept agitatedby means of a blower. As workpiecespass through, all surfacesare brought into contact with developer powder carried by the from the cabinet air. Air mustbe exhausled or cleaned by being and either recirculaled passedthrough a dust-collecting filter. Wet develope4when used, is contained in a tank similar to that used for pnetrant or emulsifier. The hnk should be deep enoughto permit workpiecesto be suu Thereshouldalso in the developer. merged be a rack or conveyor on which parts can rest after dipping. This will pennit excess develooerto run back into the tank. developerbaths settle out Suspendible when not in use; therefore, a paddle for agstirringshouldbe provided.Continuous the settlingrate bcause itation is essential is rapid. Pumpsare sometimesiocorporated into the developer station for {lowing the developer over large workpieces through a hoseand nozzleand for keepiogthe developr agitated. In automaticunits, special methodsof applyingdeveloperare required.Flow-on methods are frequently used. This technique requires a nozzle arrangement that permits the workpiecesto be covered lhoroughlyand quickly. Inrpe<tion Stotion. Essentially,the inspection station is simply a worktable on which workpieces calr b handled uoder

Fis. 13H#m,:iH:$H *. *
proper lighting. For fluorescentmethod! by a curtai the tableis usuallysurrounded or hood to excludemost of the white ligt from the area.For visible{ry peoetrants, hood is not necessary, Oenerally,black (ulhaviolet) lights (10 W or greater)are mounted on brackets fror which they can be liftd and moved abol by hand. Because of aheheat given off b blacklights,goodair circulationis essentil in black lieht booths. For automatic inspection, workpicces ar moved through booths equipped with spl cunains, either by hand, monorail, or b conveyor. In some large iospcction instalL tions, fully enclosedrooms have ben bui for black light inspection.Accssto thc rool is providedby a lighl lock. Inspection roon mustbe laid out etrrcientlyto preventrsJect workpices from reentering the prcductio line. Figurcs 14 and 15 illustrate typical pel and their layot etrantinspectioncomponents in an inspctionstation installation. Automdied Inspeclion

Equlpment
For manyyears,th pnetrantinspectio of production parts has been a manual ol

Slalio. t Slolion 3

Stotion5 Drying

Stotio. 2 Oroininq

li9hr

Fig.

14

cqliPftd unii fo' in'F<tins rc*Pi6<' bv *E EtcFwchot lf*ril#T#fs"

80 / l|tethods of Nondeslructive Evoluotion

Liquid developer lonk

( r o2 r)

EiartArro[99mg.tof3qUir,nnluredinonefoundryforthc|jquidF.ncrrodiBPeclio.ofo|or9ewrieiyo{cd6|ing!|origid+.iIi.orioE.[{dnyofl||sCo3lin9!rii. hondl;is bl. cMe or rcll6r @nvaybr.

emtion of moving parts from station to station through the penetrant line. Properly trainedand motivatedoperatorswill do an job of processing xcellerit and inspecting parts as well as conholling the process. There are, howeyer, many situations in

which manual processingsimply cannot keep up wiih the production rates required properly. or conrol the process Theuseofautomated inspection systems, therefore, a significant hasbecome factorin performingpnetrantinspections of high-

ii||rx{i; {I

i'l: t ''f

,ir
t

volumeproductionparts.Modern automated penetrantinspection systems provide precise process and repeatable control, improvedinspection proreliability,increased ductivity,and lower inspectioncosts. Automatedpenetrant inspectionsystems incorporate prograrnmablelogic control (PLC)units,which are programmed to control the handliDsof parts fhrough the syslem. to controlthe processing cycleprecisely, and to monitor the functiols at each processing station.Figures 16 to 18 show typical automatedpenelmnt systemscurrently in use.

Procleonlng
Regardless chosen,adeof the penetrant quate precleaning of workpiecesprior to penetrant inspction is absolutely necessary for accurateresults.Without adequate removal of surface contamination,relevant indications may be missedbeaause:
.X'

rffi:::;g'r I

,Sl$ ;;i: I

r e

Iffilttlrritffli
c"rEBS K!ar5;

. The perretrartdoesnot enter the flaw . The penetrant losesits ability to identify the flaw because it reactswith something alreadyin it . The sulfaceimmediately tbe surrounding penetrant flaw retains enough to maskthe true appearance of the flaw

(owr .obor 3hoM lch d lfie he .obor 3hoM (lowr left) ro left) to tronrfer tronrfer workpi*s $lurio.s nedpd to insDecl .omoonentr.

inep<r'on eq'ripdnl setup(uppr lfr) wiih d@-op of oproror chdkins PtC ponel(!pF rie. rr '- /( o Automoted ris[l), wtri.fr includer (l@er f.iil Ho #'tsi;ti *ren dlploy lti.# righ). h1n?r,:1ffi:;*.5y:, Jg,H ne rerup ifforpororos mdrenidl H."trff hondlins devi..r ffi l,Hriiffi from toiion to 3loriono.d to oppl), perekdnh ond orhr

(false) Also, nonrelevant indications may bc caused by residualmaterialsholdingpeneIrants. Cleoning methodr are generallyclassified as chemical, mechanical,solvent, or any combination of these.

tiquid

Penetranl InspGtion / 8l

immersion is by far the most effective of ensuring cleanparts,but it canbe means a very expensive capitalequipment investment. methods uses Cleaning andtheir common are listed in Table l. A majo. factor in the ofa cleaning selection method is thetypoi to be removedand the type of contaminant alloy being cleaned.This is usually quite evident,but costlyerrorscan be avoided by accurateidentilication of the contaminant. Beforethe decision is madeto usea specific it is goodpracticeto testthe methmethod, od on knownflawsto ensurethat it will not maskthe flaws. imponant in choosing a cleaning Equally of the composition of methodis knowledge beingcleaned. For example, lhc workpiece abrasivetumbling can gffctively remove burrs from a machinedsteel castingand leave a surface that is fully inspectable. This however. method. is not sui(able for aluminumor magnesium, because it smears these metals and frequently hides flaws. Particua cleanlar care must be takenin selecting fabricated ing methodfor workpieces from morethan one alloy (brazedassemblies are Fig. | 7 rypi.ot *romotd flooresent peErrdnr iNpcction i.lrollotio. notable examples);a chcmical claning methodto removescale,stgpoff matedal, Chemicol cleaning methods include alka- metal over them or by fillirg them with or flux must be chosencarefullyto ensure pickling or chemica.l abrasivematerial.This is more likely to that neitherthe brazenor the componnts line or acid cleaning, etching,and moltensalt bath cleaning will be attacked. happenqith soft metals than with hard of the assembly Mechanical cleaning methodr inch)de metals. must Ihe rurfoce finirh of the workpiece tumbling,wet blasting,dry abrasive blastWhen further proSolvent cleaning methods itlcfude vapot always be considered, water degreasing, ing, wire brushing, and high-pressure solventspraying,solventwip- ccssing is scheduled, suchas machining or or steam cleaning. Mechanicalcleaning ing, and ultrasonicimmersionusing sol- final polishing,or when a surfacefidish of pin,)or coarscr methodsshouldbe usedwith carebecause vents.Probably the most commonmethod 3.20pm (125 an is allowed, they oftenmaskflawsby smcaring adjacent is vapor degreasing. However,ultrasonic abrasivecleaningmethod is frequentlya goodchoice. Generally, chemical cleaning methodshave fewer degrading effectson (unfinishthanmechanical methods surface usedis stronglycorrosive lessthe chemical beingcleaned). Steam cleanto the material ing and solvent cleaningrarely have any elfect on surfacefinish. Some materialsare subject to delayed as a resultof impropercleaning. reactions Two notable examplesare high-strength to steeland titanium.lf it is ever necessary chemically etch a high-strength steel workpiece,it shouldbe bakedat an appropriate for a sumcient tim to avoid temperature hydrogen embrittlement.This should be but done as soon after etchingas possible no later than I h. Titanium alloys can be subject to delayedcracking if they rctain compounds and are then cxhalogenated posed to temperatures exceeding480'C 'F). CoDsequen y, halogenated sol{900 ventsshouldnot be usedfor titaniumandits alloys if their completeremovalcannotbe ensured. Choiceofcleaningmethodmay bedictatSafetyand Health Aded by Occupational Protection ministrationand Environmental Agency heallh and safery regulationsq5 Quantitiesof materialsthat will be used, o'* "rkpeces' s<h Fig. r 8 i:Tffi1#mi*:::*:lll**.'1";;x",m1JJ.g',9" anddispostoxicity, fi ltering,neutralization

82 / tnethods of Nondestru.tiye

Eyolustion workpieces, and requiredcustomerspecificationsfor process parameters. Postemulsif iable Method The processing cyclesfor the postemuisifiable processes, methodB (lipophilic;ano method D (hydrophilic) are illustrated in the processing (Fig. 19 and 20, flow diagrams respectively).The major difference between the two methods,as describedbelow, is the additionalprerinsesteputilized in methodD. Appli<otion of Penelront. Workpieces shouldbe thoroughly and uniformlycoated wrth penetrant by flowing, brushing, swabbing, dipping, or spraying. Small workpiecesrequiringcompletesurfaceinspection are usually placed in a basket and dippedin the penetrant. Larger workpieces arusuallybrushed or spmyed.Electrostatic spray applicationis also very effective and economical. After the workpiecehas beencoated with a light nlm ofpenerant, it shouldbe positioned so that it candmin and so that excesspenetrantcannot collect in pools. Workpieces should not be submerged duringthe entire penetration dwell time. Heating the workpiece is also not necessary or recommended. becausecertaindisadvantages can occur, suchas volatilization of the penetrant, difficulty in washing, and a decrease in fluorescence. Dwell Time.After the penetrarthasben appliedto the workpiecesurface,iI should be allowedto remainlong enoughfor completepenetration into the flaws. Dwell time will vary, depending mainly on the size of the defects sought,cleanliness ofthe workpiece,and sensitivityand viscosityof the penetrant. In most cases. howver.a minimumof l0 minanda maximum of 30rninis adequate for both fluorescentand visiblepnetrant types.A lengthydwell time could causethe penetrant to begindrying on the sudace, resulting in difficult removal. If dryingdoesoccur,it is necessary to reapply the penetrantto wt the surfaceand then begin the removalsteps,Recommendations from the penetrant supplierwill helpestablish the time, but experimentation will determineoptimumdwell time. Prerinse.!fllrcn using methodD (hydrophilic). a coarsewaterspray prerinseis needed to assist in penetmnt removal andto reducecontamination of the emulsifier.A coarse water spmyis recommended. using a pressure of275to 345kpa (40to 50psi).The prerinse watertemperature shouldbe l0 to .l{} "C (50 to 100 'F)- The prerinsetime shouldbe kept to a minimum(rhatis, 30 to 90 s) becauscthe purpose is to remove excess penetrant so that the emulsifier does not become quickly. contaminatcd Emulsifier Applicotion, It is veryimportant that all surfaces of the workpiecebe coatcdwith the emulsifier at the same time. Smallworkpieces aredippedindividually or in batches in baskets oron racks, whichever

T-oble| Applicqtions of vqrious .hethods of precleoning lor liqsid penetrcnt inrpection

Abrasive rrmbling. . .. .. ,

Dry abrasiv Brii blastine.

. .. Removing liehl scitr, bu6, wetd,nS 0ux, b.aze stopoff,rus1, criti.g hotd, andcore mareriat; should nor b urd on soft m.ralssuchas aluhinum. maSnstum, o. titanium .. Removine tighror heavys.ab, nor, sropoff,rust, castins moldsd corc mrrial, spraycd coalings. carbon dposils-in seneral, any friabledepo3il. Can

weiabrasive s.it bralrins.

."Y.tfjfi'"f"ffi1herc

surface ad bettercontrolofdimnsions are requircd W i r t ' r u s h i n s . .-,. . . . . . . . . . . R e m o v i ntg ight d q o s i t so f s . i t e ,f l u x , d s t o p o f i Hirh-Flsurw ater a n ds t e a m . . . . . .- . . - . . . - . . - . - . . . . . O r d i n a r i lu w i i ha na l k d i n e ya d c t e a n o r. d e t a r g n r ; rmovins typicalmachine shopsoilssuchas culring polishjng oils. compounds, chips,and erase, deposil$ from lectical dhcharge machiningi used whcn surfacc finirh mustbc mainrained; inerpensive UltEsoric ckani. . ,.... -. .. Ordinarity usd*irh dtergent andwa:a.o. wiih ^ solvnt; removin8 adhercnt shopsoil from tarSe quanlities of sdall pans Alkalineclaoin8 ...... _. .... Removins bmzestopoff,rust, scate, oiL, 8rcass, polisbingmllerial, and carbondeposits: ordinarily usedon hrg. anicbs wberhandmerho& @ roo laboriousi alsousedon alumi.ln fo. grossmetal .... Strong solurion fo s r r m o v i nh ge a v y s c a t em ; itd solutions fo.lighr scale:weak(elching) solutions tor

depo,ils a.erishr, teuer

A c i dc t e a n i n.S ..........

Morren sart barh creanins .

Solrr[t nethods Vaporde$aiing-..... . . Solventwiping-.-.-..-.-

. .jiliilliiJ':11"""ffi,# fl:f,l ,"","

.. ,. Renovinsrypicallhop !oil, oit, snd srcas;usuany employs chlorinatd solvntst not suirabte for ..,. San as for vapordcsreasinS excepla hanooperauont may .mploy nonch'orinared solvcntst usedfor localized low-volum.cleanina

inspction.For example, excessiveoverwashing or overemulsification can remove the penetrant from the flaws; minimal Pcnlrunt Intpettlon washing or undremulsification can result in excessive background, whish could Prorecrlng P.rarhotert mask the flaws and render them undetectIt is extremelyimportantto understand able. the significance of adhednc to the estabProcessing time in each station, the lishedprocess parameters ior a givenap, equipment used, and other factors can vary plication.Failureto control the process widely, depending on workpiece size and parameters will affect the quality of the shape, production quantities of similar

al techniques, andworker protection all are crucial factors.

Fig,

I 9

e.**'i"s

nd dios.dmlor rhe posremukifiobte, mothod B, tipoFtriti. perer.oo lyjrm taqoid

liquid

Peneiront Insprtion / 83

ately prior to drying by dip, flow-on, or No agitation spraytechniques. of the developer bath is required,Removalof the developer coating from the surface of the workpiece is required and easily accomplished coating because the drieddeveloper is water solubleand thereforecompletely removable by a water rinse. (form C) is Woter-suspendihle developer appliedjust after the final washand immediately before dryiag. Dip, flow-on, and sprayarc common merhods of application. Caremustbe takento agitate ttredeveloper thoroughlyso that all particlesare in suspe$sion;otherwise,control of the concentration of the appliedcoatingis impossible. Removalof the waier-suspendible developer can best be achieyed by water spray on rinsing,If allowedto remainindefinitely Fig. 2O e.*"i"s {|ow diosrom f,' rhe po3r,.muhiffobl., rettrod o, tydrophili. liquid p..trdrt ryr,eD the workpiece,the develope.cao becoDe dilncult to remove. nonaqueousdevelmay removepenetrants So(vent-suspendible is the most convenient.For large work- too muchpressur pieces, methods muslbe devised to achieve fro:n the flaws. A coarsewater spray is oper lJormD) is alwaysappliedafterdrying and can be assisted with air by spraying, oither with aerosolcontainers the fastestpossible coverage; two methods recommended methor electrostatic Lo- (the combined water and atr pressure or by coDventional often usedare sprayingo. immersing. spraying produces recommend- ods. Proper a thin. uni not exceed the prcssure calizedemulsification of large workpieces should in producby spraying. can be achieved The tempera- ed for water alone). Water tempemtur form layer that is very sensitive at a relativelycon- ing either tluorescent or red visible ture of the emulsifieris not extremelycrit- shouldbe maintained can be re- indications.The volatility of the solvent ical, but a rangeof 20 to 30 'C (70to 90 'F) stant level. Most penetrants with water in a rangeof makesit impracticalto use in open tanks. is preferred. movedeffectively 'F). Not only would thre bc solventloss, reEmulsiJication Time-The lengthof time l0 to 40 "C (50 to 100 of the developer, DryiDg is best done jD a recirculating duciogthe effectiveness the emulsifieris allowedto remainon the vapor coII- but there would also be a hazardous workpiece andin contactwith the penetrant hot-air drier that is thermostatically is the emulsificationtime and depends trclled. The temperaturein the d.ier ts condition,Dipping, pquring, and brushing and200 are Dot suitablefor applying solvent-susbetween 65and95'C ( 150 employed, normally mainlyon the type of emulsifier its concentration, and on the surlace condi- oF). The tempcratureof lhe workpieces pendibledeveloper. Deyelopingfime. ln general.l0 mih is tion of the workpieces. Recommeodationsshould not be permittdto exceed70 "C in the recommended not remain minimum developing should by the manufacturer of the emulsifiercan (160'F).Workpieces of the developer form used, drying time regardless asguidelines, serve but tbeoptimum timefor lhe drjer any longerthan necessaryl within a few min- The developingtime begins immediately workpiece by is normallyaccomplished a specific mustbe established of the developer,Excesdryingat hightemperatures after applicatioo exprimenution. The surfacelinish, size, utes,Excessive iime is seldomnecessary of the inspection, sive developing ofthe workpiece will deter- canimpairthe sensitivity andcomposition of bleeding drying time will vary, the exact and usuallyresultsin excessive mioemoreprecisely the choise ofemulsifier Because which can obscureflaw delinexperimentally indications, andemulsification time time shouldbe determined dme. Emulsification eat|0n. mnges from approximately 30 s to 3 min and for eachtype of workpiecc. Inspection$, develAfter the prescribed on the form of deDevclopingdepends is directlyrelated of tbe b the concertralion time,the inspection should begin. If emulsification emulsifier. time is exces- veloperto be used.Varioustypesof devel- opmenr The inspectionarea should be properly blow. sive, penetrantwill b removedfrom the opersare discussed inspecpowderfformA) is applied darkened for fluorescentpenetrant Dry-developer flaws,makingdetection impossible. black light intensityi5 Rinsing, For all methods,removingthe afler the workpiece has beefl dried and can tion. Recommeodd to 1600pwcm?. The intensityof the penetrantfrom the workpieceis probably be appliedin a varietyof ways. The most 1000 Electrostat- black light should be verified at regular is dusting or spraying. the mostimportantstepin obtaining repto- common by the useof a suitable blacklight is alsoveryeffective. In intervals ducibleresults,If penetnot removalis per- ic sprayapplication the meter such as a digital radiometer.The formedproperly,psnetrant will be stripped somecases,applicatiol by immersing developer is intensity of the black light should be alinlo thedry powder from the surface only in the workpiece andwill remain espe- lowed to warm up prior to use-generally For simpleapplications, flaws. More variabi,ityin individualtech- permissible. only a po'iign of the sudace of for about l0 min. The inspector should nique entcrs into this particuiarphaseof cially ia/hn a 1-min to darkness; inspection than any other step.Therefore, a large part is being inspected,applying allow time for adapting White light inExcess period is usuallyadequate. removalmust be performedwith the same with a soft brushis oftenadequate. from the work- tensity shouldnot exceed20 lx (2 ftc) to can be removed sequcnce of operationstime aftr time if developer environmen(. kPa, or 20 ensurethe bestinspection are to be rcproducible. results This is espe- pieceby a gentleair blast (1,10 Visible-penetdntsystemsprovide vivid for tightor psi, maximum)or by shaking or gentle ciallyirnportant wheninspecting Whichever means of applicarion is red indicationsthat can be seenin visible rapping. shallowflaws. Rinse time should be dcrermined experi- chosn,it is impodanl lhal the workpiece light. Lighling intensityshouldbe adequate by a fioe to ensureproper inspection;320to 540 lx andevenlycovered mentally it usually bc completely for spcificworkpieces; (30 to 50 ftc) is recommcnded. Lighting varics from l0 s to 2 min. Forspray rinsing. film of developer. (form B) is ap- intensity intershould be verified at regular developer Water-soluble waterpressuieshouldbe constant, A pressureof about275kPa (,$ psi) is desirable; pliedjust after the final washand immedi- vals by the use of a suitable white light

E4 / ,Vtthodsof Nondestructiye Evqluqtion

to remove excess penetrant surt-ace willalso dissolve the penetrant]rom within the Itaws, The processing paramete$ for the useof developer are the sameas those described above for the postemulsifiable method, Dry-powderdevelopers, however,are no( recommelded for us with the visiblesolvent-removable penetrant method.

Portcl,ecnlng
Someresiducwill rcmainon workprcces after penetrant inspection is compleGd.In manycases, this residue hasno delerenous effectsin subsequent processing or in serFig, 2 | r*"i"e f|ow diosromfor rhaword-wqshobtc tiquidFeironr ,rrren vice. There are. however,instances in which postcleaning is required. Resldues can result in the formationof voids durios meter such as a digital radiometer. Detailed rinsing is desirableto remoye tnacious subsequent weldingor unwanted stopoffin infomation on inspection techniquesrs background fl uorescence. This techniqrie, brazing,in thc contamination of surfaces availablein the sections"Inspection and however, must be very carefullycontrolled (whichcan causetroublein heat treating), Evaluation"and "specificationsand Stan- to en5urc thatoverwashing doesnotoccur. or in unigyol3!1g lsaqtions in chemicarprodads" in this article. ForspEy rinsing, a nominalwater pres- cessing opcrations. sure of 140 to 215 kPa (20 to 40 pai) is Drasticchemical or mechanical methods Wofer-Wdshqble Method recommended; too much Dressure can re- areseldom required postcleaning. for When indicated by th flow diagramin Fig. sult in overwashing, that i;. the removalof justilied by the volumeof u,ork. an emur- _As 21,the processing cyclefor the water-wash- penelrant from within flaws, Hydro-air sion cleaningline is effectiveand rcasonable method is similar to that for Ine spraygunscan be used.The air pressure, ablein cost.In special circumstances, ullrapostemulsifiable method. The difference however.should not exceed170 kpa (2j soniccleaning may be the only satisfactory lies ilr the penetrant removalsteD.As dis- psi). The temperature of the water should way of cleaning deep crevices or small cussedin the section "Material; Useo ln be controlled to l0 to 40 .C (50 to 100.F). holes. However, solvents or detersentPenetrantInspection" in this article, the Drying,developing, andiospection process aidedsteamor water is almosi alwavisufwater-washable penetrants have a built-in pammeters are the sameasthe Dosaemulsi-ficienl,fhe useof steam with detereenr is emulsifier, thusliminating lhe needlor an fiable methodprocessparameteridescribed probablythe most effective of all me-thods_ emulsilication step. One rinse operatron ls in the section"Postemulsifiable Method', It has a scrubbing actionthat removesdeall thal is required,and the washing opcra- in this article. -because velopers,the heat and detergent.emove tion shouldbe carefullycontrolled pnetrants, it leavs a workpiece hot water-washable penetrants are susceptible Solvenl-Remoyoble llethod enough to promoterapid,evendrying, and to overwashing, The basicsequence ofoperations for the il rs harmless to ncarlyall materials. Vapor linre time shouldbe determined exDeri- solvent-rcmovable pnetrant system is gen- degreasing is very effectivefor removing mentally for a specific workpiece; it usually erally similarro that followedfor the otner penetrants. but it is practically worthless for variesfrom l0 s to 2 min. The bestpractical methodsA typical sequence is shownby removing developers. lt is frquentlyused wayofestablishing rinse timeis to viewlhe the flow diagram in Fig. 22. A norabti In combrnatron wilh steam cleanins. If this workpiece under a blacklighrwhilerinsing difference is lhat rvith the solvent-removcombination is used,the steamileaning andwashing only unlil thefluorescent back- able methodthe excesspenetrantis rc- shouldalwaysbe donefirst because vaDor gxoundis removedto a satisfactory degree. movedby wipingwith clean,lint-free mate- degreasing bakes on developer films, -warant On some applica{ions. suchas caitings, an nal moistened with solvent.It is imoonanr Whereconditions do not or Derrmmerston nnse lollowed by a final sDray to undershndthat floodingthe woikpiece mit permanent cleaoing installations, hand wipingwith solvents is effective,Dried developer films canbe brushcd ofr, andresidual penetrants can be rinsedoff by solvent spraying or wipedoff with a solvent-damDenedcloth,

Qrollry Arrorlnce of Poretrc|rl lnrpectlolr fleierlolr

It is important to provide the conrrols necessaryto ensure that the Denelrant ma_ terials and equipment are operating at an acceptable level of performance. The frequency of the required checks should be based on a facility operaring for a full, one-shifl oreration daily. ln general. iI is Sooo practtceto check the overall system perlonnance on a daily basis. This check

Eig. 22

Procesing llo*

didgrdm for rhe rot*nr-remoyobt.

liqurd pemtronr rysrcm

Liquid Penetrcnt Inspection / 85

shouldbe pcrforme.d by pr(rcessing a known Toble 2 Intervols ot which defect standard through theline,usiogappr+ sol.rtionr, fight sou"6e5, and syttem pnateprocessing parimctersandcomparing performcnce should be checked the indications thus obtainedto those ot!. taioedwith fresh,uDused penetrant rn.dterial lr.qhn.t R.quifrn.nt when thc performence sample\. of the in-ure materials fallsbelowthatofthe unused materials, the in-uscmaterialquality shouldbe b n s h t n e s.s - - . . . . . Q u a n e d y Not lssthan907. checked with the appropriatetests (as describedbelow)and corrected prior to conE4ualto ductingany further penetrantinspection. quality Key assurance teststo be periodically conducted on in-use penetrants. Removabilily A walr {method mulsifiers,and developersare listed in w r s h o n l y ] . . . . . . . . M o n l h l y Equalto Table 2. Also listed are the intervals at which the light sourcesand the overall w.ter onrent systemperformadce shouldbe checked. (nelhod A water Military Standard the spe6866specifies cific test procedure to use for the lestsdeo n l y ) .. . . . . . . . . . - M o n t h l y finedin Table2- Penetrants by sp|ay Contamination......Wekly applied application from sealedcontainers are not likely to be exposedto th same working Emulsifiers Removabiiity . ... . -. Wekly Eqml lo environment aswith opndip tanksand are therefore not required tested to be asdefined in Table2 unless contamination is suspected. (merliod Conlaminationof the emulsifer must also be considered. Method B, lipophilic emulsifiers inherentlybecomecontaminated by penetrantthrough the normal processing ofparts coated with penetFntbeing dippedinto the emulsifier.It is imperative, therefore, thatthe lipophilicemulsifier have (that is, l07o)for penetralt a hightolerance contamination. Watercontamination of th lipophilic emulsifieris always a potential problemdue to the natureof the process. Generally,5% water cootamination can be tolerated. Method D, hydrophilic emulsifiersarc not normally subject to appreciable amounts of penelran( contaminalion, mainly because of the prerinseprocessing step, which removesmost of the excesssurface penetrdntbefo.e emulsificatioo.Because hydrophilic emulsifiersare water based, water contamination is not a problem,exccpt for the fact that the bath concenratidn mustbe maintained at the prescribed limits. In general,emulsifiersthat becomeseverelycontaminated will not properlyemulsify the surfacepenetrant or the parrs. Periodicmonitoring is essntial. Developermust also be maintaiq9! to properperformance. ensure Contamifiition of the dry.powderdeveloper with water or in the air cao resultin caking.Dry moisture developersmust rcmain fluffy and free flowing if they are to performproperly. [n addition, contamination from the fluorescentpenetmnt mugtnot occur. Fluorescent specksin the developerpowder could be misinterpreied asan indication.Wet developer (solubleor suspendible) mus( not become coDtaminated with penetrantor any contaminant that could affect its ability to wet and evenlycover the workpicce.

mt|hlerlncc

ol fllterlnlJ

B, l i p o p h i l i c.). . . . . . . M o . t h l y

(method D,

l,ydroFbilic)..,,-.. weekly With constantopen-bnk use, penctrant 3% aboveinnial matedals are inherently subject to potential deterio.ation. Such lactors as evaporation C o n l a m i ni o n . , . . . . W e e k l y losss and contarnirralion from various so[rcescancontribute to deterioration. It is Developrs form-.Daily Musr be lluJly, essential, therefore, to monitorthecondition D.y-dev.lopr of thesematerials as described in Table2. Contaminarion......Daily The evqporotionof the volatileconstituents of penetrants can aller their chemisal and pedormancecharacteristics, thus re102 mm (4 i..) suiting id changes in inherentbrightness, (soluble removability, and sensitivity.Liquid peneAcu.ous and traot materialsqualified to MIL-I-25135D develoDer (and slbsequeDtrevisions)have a flash Wctlid!r'coverage. . , - Daily point requiremqnt of a minimumof 95 'C (200 "F) (per Pensky Martensflash point test procedure), assuringthe minimization ContaDiDation . -.. .. Daily of evaporation losss. The <ontqminotion of water-washable penetrantwith water is the most frequent Concenllarion. . . . . . . Wcekly $ourc ofdilficulty. Whenpresent beyond a critical percentage, this contamination will render the penetrant tank useless, For speciiied postemulsifiable penetrants, Minimumlmo watercontaminationis not ascritical a problem, because t n m( l J i n . ) wateris usuallynot miscible with postemulMinimum2?m lx sifiablepenetraots and will separate from {200tlc) the penehant,which can then be subse- syslcm perfomance . . . Daily quentlyremoved. Watercontamination can be minimizedby implementing and followrlrgproperprocessing procedurcs. It is important to recognizethat acid (ca[yover from precleaning) nantsdo no particular harm unlesspresentto contamination will renderfluorescentDenetrants ineffec- the extent that the bath is scummy with tive. Acid contamination chanees the con- floating or suspended foreign material. Reasistencyof the penetrantandlamages or sonable care should be taken to keep the destroysthe fluorescent penetrdnt clean. Workpieces containing addye. Dusl. dirl and lint. and simild.foreign hering sand and di.t from the shop floor materials get into the penetrant in the ordi- should be cleaned before bcing dippd into nary courseof shop urage.Thesecolttami- the penetrant.

lrerlnlng errrd Certlllcotion ol Pertonnl

The apparent simplicityof th peoetrant methodis deceptive. Very slightvariations in performing process the penetrant and the inspection recan invalidatethe inspection sultsby failingto indicateall flaws. Therefore, many companiesrequire that penetrant inspectian be conducted only by tiained and certified personnel.Minimum requirements for personnel trainingandcertificationare described by variousmilitary and industry specificatiors(such as MILSTD-410 and ASNT SNT-TC-lA). The followingare examples ofthe most commonly followedtrainingprograms;however,spe' ciflc cusiomer training requirementsare usuallydefinedwithin the contract, lroining is mioimalfor level I penetrant inspection (personnel oprators responsible for the processing). However,the penetrant processmust be correctly performed to ensuleaccumteilspction. Opratortraining consists of the satisfactorycompletion of a periodof on+he-jobtrainifl9,as deter-

t6 / methods of Nondestruclive

Evoluotion
indication exceeds allowable limits, it must be evalualed. One of the most common and accurale ways ofmeasuring indications is to lay a flat gage of the maximum acceptabie dimension of discontinuity over the indication. If the indication is not coopletely covered by the gaBe, it is not acceptable, Evoluolion. Each indication that is not acceptableshould be evaluated, It may actually be unacceptable, it may be worse than it appears, it may be false, it may be real, but nonrelevant, or it may actually be acceptable upon closer examination. One common method of evaluation includes the followjngsteps: . Wipe the area of the indication wirh a small brush or clean cloth that is dampened with a solvent . Dust the area with a dry dveloper or spray it with a light coat of nonaqueous developer . Remeasureunder lighting appropriate for the type of penetrant used If the discontinuitv originally appeared to be of excessive length because of bleeding of penetrant along a scratch, creyice, or machining mark, this witl be evident to a trained eye. Fioally, to gain maximum assurancethat the indication is properly interpreted, it is good practice to wipe the surface again with solvent-dampened cotton aod examine the indication area with a magnifyinggla,:sand ample white lighr- This final evaluation may show that the indication is even larger than originally measured, but was not shown in its entirety because the ends were too tight to hold enough penetrant to reach the surface and become visible. Dirporition of Unocceptoble Work. pie<er. A travel ticket wi[[ ubually accampany each workpiece or lot of workpieces. Provision should be made on this ticket to indicate the future handling ofunacceptable marerial. rhat is, scrapping, rework, repair, or review board action. There is oftcn room on such tickets for a brief descriDtion of the indicatiqn, More often, indications are identilied directly on the workpiece by circling them with some type of marking that is harmless to the material and not easily removed by accident, but removable when desired. Rewoil<ing an unacceptable flaw is often allowable to some specified limit; iodications can be removed by sanding, grinding, chipping. or machining. Rpair weldrng is sometimes needed: in this ca!e. the iddication should be removed as in reworkine beforc it is repair welded, or welding may move the flaw to a new location. In addition, it is imperative that all entrapped pcn, et.ant be removed prior to rpair welding, because entrapped penetrant is likely to initiate a new flaw. Verification that the indication and the entrappcd penetrant have been removed is required.

Tqble 3 Common types, locqtions, qnd choracteristics of flowg or discontinuities reveqled by liquid penetrqnt inspection

ShnnkaA ce r a c k s ... . . . . . - . , . . . . C a s r i n g (s a l lm e t a l s ) - - - f o tn , r ls u r f a c c s H o rr e a r s ........-... -......_.. Casling (a t side st t m e r a h l - a in Cold shots . . . . . . . . . . . . . . . . . . _ . . C i s t i n s(s allmetatsFc ah r anse s in c.ossscction Foldr.. . Casring {\ a l lm e r r l . t a n y w h c r e l n c l u s i o.n .s . . . . . .. . ...... ... ccsrinsf so .rerng...heer. brr-anywhere M i c r o s h r i n k ap go er e s. . . . . , . . . - . C a s t i n g s + n y w h . e k P s . . . . . . - - . . . . . - . - . - . . . .F o r g i n g bs a,r a n y w h e r e ForSinS cracts... .. .. . . - .. . _. .. . Fo.sines{r insideor ourside comcrs andat charge3 in fioss sctiotr . . . . . . . . . . . . . F o r c i n s \ . b a r -n e a s , . o m e r rc e n r e r lp.. : L2mrna0ons...... S h e e r - - -c sd r ges c e n t eb r ead c r a ( k \ . . . . . . . . . . . . . . w e t d s + r c e n r eo rf r e , n f o r c e m c n r Cracksin hed-affected zooe .. .. - Wlds+r edSe o{ tiDtorcemenl CEler cracks . . . . - . . . . . . . . . . . . . . Welds----at cnd of head p o r o l i r y. . . . . . . . . . . . - . . . . . . . . . . c n s r i n g s w . elds Grindins c a c k s .- . . . . . . . . . . _- . . . A n y h a . dn e r a t - g r o u n d sudaces c r a c r s.. . , . . . . . . . . . . . . . H ; t l r c a l e d Quench sreel S l . e s s - c o n o s ic om n cks -... , . , ,. . Anymetal F a l i S uf e f a c k s . .. . . . . . . . . . . . . . . . A n y n r e i a l NoDElevrra inditions(s) W e l ds p a r i r r. . . . - . . - . . . . . . . . . . . A . c w e l d s Incomplete pent.arion . . .. .. . .. . Pilter*elds Su.face cxpulsion . .. . . . . . . . . . . . . R e s ; s t a n c we ctds S.ulTmarks- . . , . . . . . . . . . . . . , . . . Seamvtds P r c s s - fiin l t r f a c.e ........- --... Pressfirs Bra2 r u n o t r. . . . . . . . . . . . _. . . . . . B r a i e dp a r l s Buns . . . . . . . _. . . . . . . _. . . . . . . _. _ Machind oa.s Nicks, d e n t ss , cratches . ., . . . . . . . A l t r a r t s
(.1 Th.* @y b. prchibit d tlavi, bur ar usMllr iosiddcd Tishl, shallow Ti8ht, shallow Ti8hi. shallow, intermirent Sponsy Tight or open

Tiehl or open TiShr or opn

Sph$ical Ti8ht. shallow, random Tisht to ope\, oxidized Tighl lo oFni may show conosion Tighl

Orr.D, flrll weld lenstl Raised metal at weld edSe Surfee of sam welds Edse of cxcess bmze Bleeds heavily Visibl r{iihout per.trant aids

no.it.rant in pichnt t.siins.

of flaws that can be found by penetrant inspection, together with their likely locations and their characteristics. Intpe<lion Toolt, Ao inspector must have tools that are capable of providing thr required accuracy. These tools usuallv include suitable measuring devices, a flashlight. small quantities of solvent, small quantities ofdry developersor aerosol cans ofnoDaqueouswet developers,pocket magnifieE rangingfrom 3 to l0 x, and a suitable black light for fluorescent penetrants or suflicient white light for visible penetranrs. Photographic standardsor workpieces that have specific known flaws ar somelimes used as inspection aids. A typi(ol in.pe<rion beginswith an overall examination to determine that the workpiece has been properly processetland is in satisfactory condition for inspection- Inspection should not begin until the wet developersare completely dry. Ifdeveloper Iilms are too thick, if penetraot bleedout appearsexccssive,or if the penetrant background is excessive. the workDieceshould be cleanedand reproccssed*hcn rhe inspector is satisfied that the workDiecc rs inspectable, it is examined according to a specifiedplan to be suaeno arcas bave been missed. An experienced inspector can h3pe.tlon and Ev.rluoflon readily deternjne which indications are After the penetrant process is completed, within acceptable Iimitsand which onesarc rnspection and cvaluationof the workFiece not. The inspcctor then measuresall otner begin. Table I lists the more common types indications. If thc lengthor diameterof an

mined by immediate suEErvision. conducted undgr the Suidancc of a certified level I rnspector. Training for level ll inspectors (personnel responsible for the inspection and evaluation) is more extensive than that for rne level I operatorr. Training usually consisrs of 40 h of formal faining, followed by several \rreeksof on-lhe-job lraining under the supervision ofa designated lrainer,usually a cenified level II oterator. Certificolion. Personnel of sufficient backgroundand training in the principle5 ano procedures ol penetrantinsnection arc usually certified by the successiul comple(ion of a practical Iest, \rhrch demonstrate5 their prcficiency in penetrant techniqucs, and a written test, which documcnts thcir knowledge of pcnetrant inspection-Cerlilied personnel are alro normallyrcquiredto pass a periodic eye examination, which includes a color-vision test. Certification can be obtainedon-site through a certified level lll inspector who may be with an outside sourcc contncted to certify personnel or a company empioyee who has been certified as a level III inspector by thc appropnate agency.

Liquid Penetrant l.tble 4 Prrttiol listing of siondqrdt cnd lpccificotions for liquid pnetrarnl inspeation
Tnk d .rpLdlld ol Ctnded d ip..iadrlon

lnspeclion

I 87

A S T M - E - 1 6.5 . . . . . . . . . . . . . . . . . . . - - . . . , . . . . . . S t a n d a rP dr a c r i cfe or Liouid-PenetB lnt sDectio ne t h o d M 270 ASTM-E . . . - . . . . S t a n d a rD o\f T e m s R e l a t ' nie de f i n r t i o n o Liqud-Penetrmr .{STM-E-I?06 ASTM-E-1209 ASTM'E-1210 ASTM-E-1219 ASTM-E-I?20 ASTM-E-Il3J ASTM-D-2512 T.st for AMSSAE spelficqtions . ... - Flooresc.nt Peoetmat ltrspction-AircEfl ard Ensift ComDoncnt Maintenaoc
ASME rpd'llcllid|s

. . . .. .. Sle&rd Metbodfor Fluore:|cenl Ljquid-Pentrant Examination UlinCth Lipophilit PostEnulsificalion Prff.ss . -. .. ., Stadard Methodfor Fluorescenl-Pentrant Examinalion Usins thc WaleFw8fi a6le P.Gess . . - . .. . Standard Metbodlor Fluorcscent-Penelrant EEminationU$ine rhe Hydroph'licPosrEmuhificdtion Proces\ .. - . -. Slandard Merhodfor Fluo.cscnGPenet.ant ExahinationUsirs lbc SolvcncReft ovablcPrmss . .. .... Slandanl Methodib. Visible,PnIran! ExaDjrrljon Usirs rbe SolvenrRemovable Process . .. .. . . Srandard lh Brighthls Test Mthodfo. Comparing of Fluorescnl Pnetrants . . . . - . . Compalibiliiy of Malerials with Liquid OJ(ygen Sensitivity fireshold Techdique) llJnpact

penetrant inspection, or canbe donelocally by applyingthe materials with smallbrushesor swabs. Folseond Nonrelevoni Inditqtions. Beaausepenetmnt inspectionprovides only indirect indicationsor flaws, it caonoralwaysbe determined aafirst glancwhether an indicationis real, false,or nonrelevant, A real indicationis causedby an undesirableflaw, suchasa crack.A falseindicalion is an accumulation of penetra.tt not caused by a discontinuity in the workpiece,suchas a drop of penetrantleft on the workpiece inadvertently. A nonrelevant indication is an eotrapmentof penetraotcaused by a feature that is acceptable even though it may exceedallowableindication lengths, suchas a press-fitinterface,

Speclflcctlonr ttnd Standerdt

It hasnot beenpracticalto establish any typ of universalstandardization, because of the wide variety of componentsaIId assemblies subjected to penetrantinspection, the differences in the types of discontinuities commonto them, and the ditrerencesin the degreeof integrity required. qualitystandards Generally, for the typsof discoltinuities detectedby penetrant inare established spection by one or rhoreof the followingmethods: . Adoption of standardsthat have been successfully usedfor simjlarworkpieces . Evaluation of the results of penetrant inspection by destructive examination . Experimental andtheoretical stressanalysrs

U,S. hilit rr sd gowmhedl speclftitiort MIL-STD{E66....-.-.-.....,......,.........MilitaryStandardInspection,LiquidPenetant MIL-STD-4|0 -. . , . . . . . . . . . , . . . . , . . . . - . . . . . . . N o n d e s t r u c t iT v cs r i n P g c r s o n nQ e ls a l i f i c a a i o & ns MIL-14135.........-.-....,............,...lnsDctionMaterials.Penelrant MIL-I-25105....,,.....-.......,.....-,....,tnsi,eclionUnrr,nuorescentPneirant,TypeMA-2 MILI-2510,6.. ,. ........... -.,. .. -,.... .. .,. InsFction U n i t ,F l u o r e s c eP nc t n e t m r tT , y t ' cM A - 3 MILSTD-?7I (Shipst. . . . . , . . . . . . . . . . . . . . . . . - . Nondcs.dclive Tcstios Re4uiremcDts fo. lr.lal!

Spocif icqtioni, Normally, a specification is a document that delineatesdesign or performance A spesification requirements. should include the mthodsof inspection and the requirements basedon the inspection or test procedurc.With pfletmna indimcult. Too often spection, this becomes the wordingin quality specitications is ambiguousand meaningless, such as "workpieces shall be free from detrimeDtal defects" or "workpieceshaving questionable indicationc shallbe held for review by " the properauthorities, Specification$ applicable to penetrantinspection are genenlly divided into two broadcategories: thoseinvolving materials andequipment, andthoseconcemingmethods and standards.Therc a.e, however, standards several andspcifications that are in commonuse;someof theseare listed in wJl)wdtd-woiioh. 'iquid Fis. 2s ffffiJ#Lii*.:,ii:il (il""ffi:iTfl:.f# *lif,,f;#H, Table 4, Because the equipmentused for penetrantinspectioncovers such a broad scope,that is, raoging from small diptaflk Because reworkingis usuallyrequired,it ofthe etching fluid should be rinsed off, and setups to large au(omated installattons, is good p.acticeto finish it olf with moder- the area should be thoroughly d ed before most emphasis and specificain standards ately fine sauding,followed by chemical rcprmessing for reinspection. Reprocessing tionshasbeenplacedon the materials u$ed etching to remove metal.All traces can be the samc as original processing for in this inspection processsmeared

88 / Methods of Nondeslructive lvalustion

Control SFtems. In conjunction with the sDcifications listed in Table 4, several methods and several types of standards are used to check the effectiveness of liquid penetrants. Ooe oi the oldest and most frequently used methods involves chromlum-cracked panels, which are available in sets containing fine, medium, and coarse cracks. Many other types of inspection standards have been produced--often for spcilic indicalions needed for a unique

of inlegrity factorbeingthedegree aoplication. A comparison of indications principal Al onc extreme.lor certalnnonf;om two water-washablepenetrants of dif- reouired. e applied to a ferent sensitivity that were palel containing fine chromium-cracked rromium-cracked -rs shownin Fi8, 23. cracks acks shown A.aepfqnceqnd reiectionttqndotds for inspection are usuallyesliquid penetrant for cachindividualitem or group tablished of items by the designer.In most cases, acceptanceand rejection standardsare with similaritems,the on experience based

criiical items, the standard may permit all some specific types of discontinuities over the workpieceor in specifiedareas. is often appliedonly on a samInspection pling basis for noncritical items. At the oppositeextreme, items are subjectedto are exinspection, and lequirements 100% to the point ofdefiningthe iremelystringent area. on each soecific limitations