ASMEBPVCV-2017 ARTICLE 24, SE-165/SE-165M STANDARD PRACTICE FOR LIQUID PENETRANT EXAMINATION FOR GENERAL INDUSTRY CxS SE-165/SE-165M cy (ldentica with ASTM SpecieationE165/2165M-12] 613ARTICLE 24, SE-165/SE-165M ASME BI Standard Practice for pvcv.2017 Liquid Penetrant Examination for General Industry 1. Scope 1.1 Thispractice covers procedures for penetrant examina tion of materials, Peneirant testing is a nondestructive testing method for detecting discontinuities thatareopento thesurface such 11 cracks, seams, laps, cold shuts, shrinkage, laminations, through eaks, orlack of fusion and isapplicable {0 in-proces final, and maintenance testing. Itcan be effectively uscd in the examination of nonporous, metallic materials, ferrous and nonferrous metals, and of nonmetallic materials such 11 non- porous glazed or fully densified ceramics, 14 well 14 certain ‘nonporous plastics, and glass. 1.2 This practice also provides areference: 1.2.1 By which a liguid peneirant examination process recommended or required by individual organizations can be reviewed to ascertain its applicability and completeness. 1.2.2 Forse in the preparationof process specificationsand procedures dealing with the liquid peneirant testing of parts and materials, Agreementby thecustomer requesting peneirant inspection is strongly recommended, All areas ofthis practice _maY be open to agreement berween the cognizant engineering ‘organization and the supplier, or specific direction from the ‘cognizant engineering organization, 1.2.3 For tse in the organization of facilites and personnel cconcemed with liquid penetrant testing, 1.3 This practice does not indicate or suggest criteria for valuation of the indications obtained by penetrant testing. Tt should be pointed cul, however, that after indications have been found, they must be interpreted or classified and then evaluated. For this purpose there must be a separate code, standard, of a specific agreement to define the type, size, 1d direction of indications considered acceplable, msidered unacceptable. 1.4 Units—The values stated in either ST units or inch: pound units are to be regarded separately 11 standard, ‘The ‘Values stated in each system may not be exact equivalents; therefore, each system shall beusedindependently ofthe other. ‘Combining values from the two systems may result in non- ‘conformance with the standard 15 This standard does not purport to address all of the safety concerns. if any, associated with its use. It is the responsibility of the user of this standard to establish appro. priate safety and health practices and determine the applica Bilty of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: D129'Test Method for Sulfur in Petroleum Products (Gen- cral High Pressure Decomposition Device Method) E516Praciive for Testing Thermal Conductivity Detectors ‘Used in Gas Chromatography [D808 Test Methed for Chlorine in New and Used Petroleum Products (High Pressure Decomposition Device Method) 1193 Specification for Reagent Water 1552 Test Method for Sulfurin Petroleum Products (High- ‘Temperature Method) 'D4327'Test Method for Anionsin Water by Suppressed Ton ‘Chromatography 433 Reference Photographs for Liquid Penetrant Inspec tion E543 Specification for Agencies Performing Nondestructive Testing E1208Practice for Fluorescent Liquid Penetrant Testing Using the Lipophilic Post-Emulsification Process £1209Practice for Fluorescent Liquid Penetrant Testing Using the Water- Washable Process E1210Practice for Fluorescent Liquid Penetrant Testing Using the Hydrophilic Post-Emulsification Process F1219Practice for Fluorescent Liquid Penetrant Testing Using the Solvent-Removable Process E1220Practice for Visible Penetrant Testing Using Solvent- Removable Process E1316'Terminology for Nondestructive Examinations E1417 Practice for Liquid Penctrant Testing esASMEBPVCV-2017 El418Practice for Visible Penetrant Testing Using the Water Washable Process E2297 Guide for Useof UV-A and Visible LightSourcesand “Melersused inthe Liquid Peneirantand Magnetic Panicle Methods 2.2 ASNT Document: SNT-TC-IARecommended Practice for Nondestructive ‘Testing Persone! Qualification and Certification ANSVASNTCP- 189 Standard for Qualification and Cet cation of Nondestructive Testing Personnel 23 Miliary Standard MIL-STD-410 Nondestructive Testing Personnel Qualifics- tion and Centfiation 2.4 APHA Standard: 429 Method for the Examination of Water and Wastewater 25 ATA Standard NAS-410Cerifcatio Test Personnel 2.6 SAE Standards: AMS 2644 Tnspection Material, Peneirant PL: AMS-2644 Qualified Products of Taspection Materials, Penetrant ind Qualification of Nondestructive 3, Terminology 3.1 The definitions relating to liquid peneirant examination, ‘which appear in Terminology E1316, shall apply to the terms used in this practice. 4. Summary of Practice 4.1 Liquid peneirant may consist of visible or fluorescent ‘material, ‘The liquid penetrant is applied evenly over the surface being examined and allowed to enter opendiscontinui ties. Afterasuitable dwell time, the excess surface penetrant is removed. A developer is applied to draw the entrapped pen- ctrant out of thediscontinuity and stain the developer. The test surface is then examined to determine the presence orabsence of indications [Nore I—Theéevelger may be omiteé by aprement berveer the ‘Nore 2 Flvorecentpevetrartexannaionshl not follow a visible eretesl examination unis the procedure hasbeen Guaed nace ance with 102, becatse visible dyes may ceuse cexerorsion oF ‘uerehingofBaorescen oes 4.2 Processing parameters, such 11 surface precleaning, penetrant dwell ime and excess penetrant removal methods, are dependenton the specific materials used, the nature ofthe partunder examination, that is, size, shape, surface conition, alloy) and type of discontinuities expected. ARTICLE 24, E-165/SE-165M 5. Significance and Use 5.1 Liquid peneirant testing methods indicate the presence, location and, toa limited extent, the nature and magnitude of the detected discontinuities. Each of the various peneirant ‘methods bas been designed for specific uses such 11 critical serviceitems, volume of pans, portability or localized areas of| ‘examination, The method selected will depend accordingly on the design and service requirements of the parts of materials being tested 6. Classification of Penetrant Materials and Methods 6.1 Liquid peneirant examination methods and types are classified in accordance with MTL-1-25135 and AMS 2644 1 listed in Table 1 6.2 Fluorescent Peneirant Testing (Type 1}—Fluorescent peneirant testing utilizes peneirants that fluoresce brilliantly ‘whenexcited by black light (UWA). The sensitivity of fluores ccent penetrants depends on their ability to be retained in the various size discontinuities during processing, and then to bleed out into the developer coating and produce indications that will Muoresce, Fluoresvent indicavions are many times brighter than thei surroundings when viewed under appropri- black light illumination. 623 Wsible Penetrant Testing (Type 2}Visible peneirant testing uses a pencirant that can be seen in visible light. The Peneirant is usually red, so that resultant indications produce a definite contrast with the white background of the developer. Visible penetrant indications must be viewed under adequate white light, 7. Materials 7.1 Liquid Peneirant Testing Materials consist of fuores- cent or visible penetrants, emulsifiers (oil-base and water base), removers (water and solvent), and developers (dry powder, aqueousand nonaqueous). family of liquid penctrant ‘examination materials consist of the applicable penetrant and emulsifier, 11 recommended by the manufacturer. Any liguid penetrant, remover and developer listed in QPI-25135/QPL- AMS2644 can be used, regardless of the manufacturer. Inter mixing of peneirants and emulsifiers from different manufac- turers is prohibited. ‘Norr 3—Referto 9.1 for spcil requirements forsufur, halogen ane slkal metal contr, ‘Narra While approved penetra materials wil not adversely alfect| ‘common metaliemateals, some p'stiesor rubbers may be swollen Of siuined hy cera penebans 7.2 Penetrants ‘TABLE:1 Classification of Penetrant Examination Types and Methods 7 re iveseon PrnerantPaerinaten dephe (eae ePonetan ener od _Pog oral, i ot Waa (see m3) emodG—Sohen:tenovabe(cee Tes Metod #1220) 615ARTICLE 24, SE-165/SE-165M 7.2.1 Post-Emulsifable Penetrants are insoluble in water and cannot be removed with water rinsing alone, Tey are formulated to be selectively removed from the surface using a separate emulsitir. Properly applied and given a proper emulsification time, the emulsifier combines with the excess surface pencirantto forma water washable mixture, whichcan be rinsedtrom the surface, leaving thesurfacefreeof excessive fluorescent background. Proper emulsification time must be experimentally established and maintained to ensure that ‘over emulsification does not result in loss of indications. 7.2.2 Water Washable Penetranas are formulated to be di- recily water washable from the surface of the test pat, afer suitable peneirant dwell time. Because the emulsifiers “built in,” water washable penetrants can be washed out of discon ruities ifthe rinsing step is too long oF too vigorous. I is therefore extremely important to exercise proper controlin the removal of excess surface peneirant (0 ensire agains over- ‘washing. Some peneirans are less resistant vo overwashing than others, $0 caution should be exercised 7.2.3 Solvent Removable Penetrants are formulated so that excess surface pencirantcan be removed by wiping until mest Of the peneirant has been removed. The remaining traces should be removed with the solvent remover (soe 8.6.4). To prevent removal of peneirant from discontinuities, care should be taken 0 avoid the use of excess solvent. Flushing the sarface with solvent to remove the Excess penetra is prohib ited 11 the peneirant indications couldeasly be washed away 1.3 Emalsifrs: 73.1 Lipophilc Fmulsfersare il-miscibe liquids used to emulsify the post emulsified penetrant on the surface of the part, rendering it water-washable, The individual characteris- ties of the emulsifier and penciran, and the geometrysurface roughness of the part material contribute to determining the emulsification time. 7.3.2 Hydrophilic Fmulsifiers are water miscible liquids used to eraulsify the excess post emulsified penetrant on the surface ofthe part, rendering it water-washable. These water bse emulsifiers (etergenctype removers) are supplied 1 cconcentraesto be diluted with waterand used 11adiporspray ‘The concentration, useand maintenance shall beinaccordance ‘with manufacturer's recommendations 7.3.2.1 Hydrophilic emulsifiers function by displacing the excess peneirnt film from the surface of the part through detergent action, The force ofthe water spray or aimechatical agitation in an open dip tank provides the scrubbing action “hilethe detergentdisplaces the film of penetrantfom the part surface. The individual characteristics of the emulsifier and pencirant, and the geometry and surface roughness of the part ‘material Coniribute to determining the emulsification time. Emulsification concentration shall Be monitored weekly using a suitable refractometer. 7.4 Solvent Removers—Solvent removers function by dis- solving the peneirant, making it possible to wipe the surface clean and free of excess penetrant. 7.5 Developers—Developers form a translucent or white absorptive coating that aids in bringing the penetrant out of surface discontinuities through blotting action, thus increasing the visibility ofthe indications, 616 ASMERPVCY.2017 7.5.1 Dry Powder Developers—Dry powder developers are used 1 1supplied, thats, free-flowing, non-caking powder (see 8.8.1).Care should be taken not to contaminate the developer ‘with fluorescent penetrant, 11 the contaminated developer specks can appear 11 peneirant indications 7.5.2. Aqueous Developers—Aqueous developers are nor. ‘mally supplied 11 dry powder particles to be either suspended (watersuspendable) of dissolved (water soluble) in water. The concentration, useand maintenance shall bein accordance with manafacturer’s recommendations, Water soluble developers shall not be used with Type 2 penetranis or Type 1, Method A penetrants. ‘Nore S—Aqueous developers may cause stripping indications if not propery appiec anc conoid. The procedure shouldbe qualified in Accordance With 102, 7.5.3 Nonaqueous Wet DevelopersNonaqueous wet devel ‘pers are supplied 1 suspensions of developer particles in a ronagueous solvent carrier ready for use 14 supplied. Nonaqueous, wet developers are sprayed on to form a thin ‘coating on thesurfaccof the part when dried, This thin coating serves tthe developing medium, Noe his typeof ees ened orapieony spy only 1.5.4 Liquid Film Developers ate solutions of colloidal suspensions of resins/polymer in a suitsble carrier, These developers will form a transparent or translucent coating On the surface of the part, Certain types of film developer may be slripped from the part and retained for record purposes (sce 884) 8 Procedure 8.1 The following processing parameters apply to both fluorescent and visible penetrant testing methods, 8.2 Temperature Limits—The temperature of the penctrant ‘materials and the surface ofthe pat to be processed shall be between 40? and 125°F[4°and 52°C] orthe procedure must be qualified atthe temperature used 11 deseribed in 10.2 83 Examination SequenceFinal peneirant examination shall be performed afer the completion of al operations that could cause surface-connected discontinuitics oF operations that could expose discontinuities not previously open to the surface. Such operations include, but are not limited to. srinding, welding straightening, machining, and heat eating Satisfactory inspection results can usually be obtained on surfaces in the as-welded, as-rolled, as-cast, as-forged, oF ceramies in the densified condition. 83.1 Surface Treament—Final peneiant examination may bbe performed prior totreatments thatcan smearthe surface but rot by thomselves cause surface discontinuities. Such ica rmenisinclude, bucarenotlimited to, vaporblastng, deburing, sanding, buffing, sandblasting, o lapping, Performance of final pencirant examination after such surface tcatments necessi tates that the part(s) be etched to remove sreared metal from the surface pri to testing unless otherwise agrocd by the contracting parties. Now tha final pneirant examination shal always precede surface peeningASMEBPVCV-2017 Norr]—-Sandor shorblatinacanclosediscontnutessoexteme cre should be taken to avoid masking discontinuities. Under cera reumsurees, however, grit hast with cera ar presses andlor rpedusimay be accplewihon sabsetet hig when ae by ‘Nar 8 Surace preparation of structural or electronic connie for poner esting by grin, sand lasting and etchineis not recom ‘ended because of the pote for cama 8.4 Precleaning—The success of any peneirant examination procedure is ercatly dependent upon the surrounding surface and discontinuity being free of any contaminant (solid or liquid) thatmightinterferewith the peneirant process, Allparts or areas of partsto be examined mast beclean and dry before the pencirant is applied. Tfonly a section of a part, such 11 ‘weld, including the heat affected zone is to be examined, all contaminants stall be removed from the area being examined 11 defined by the contracting partes. “Clean” is intended to mean tha the surface must be fee of rust, scale, welding ux, ‘weld spater, grease, punt, oly films, din, and s0 forth, right interfere with the pencirant process. All of these con- taminanis can prevent the peneirant from entcringdiscontinui- ties (see Annex on Cleaning of Parts and Material). 8.4.1 Drving after Cleaning—It is essential that the surface of parts be thoroughly dry after cleaning, since any liquid residue will hinder the entrance ofthe penctran. Drying may ‘be accomplished by warming the parts in drying ovens, with infrared lamps, forced ho air, or exposureto amientiempera- ture Nore 9—Residues from cleaning processes such as story alkalies ickling soluionsand chromates, i panicuar may adversely rest with the peretuntane reduce its sersitvty and perormarce, 8,5 Penetrant Applicasion—After the part hasbeen cleaned, ried, and is within the specified temperature range, the ‘peneiranc is applied to the surface to be examined $0 that the centre part or area under examination is completely covered ‘with penetrant. Applicationmethods include dipping, brushing, flooding, oF spraying. Small parts are quite often ‘placed in suitable baskets and dipped into a tank of penetranc. On larger pats, and those with complex geometries, penetrant can be applied effectively by brushing or spraying. Both conventional and electrostatic spray guns are effective means of applying ligaid penetrants to the part surfaces, Not all penetrant mate rials are suitable for electrostatic spray applications, so tests ARTICLE 24, E-165/SE-165M should be conducted prior o use. Electrostatic spray applica- tion can eliminate excess liquid build-up of peneicant on the part, minimize overspray, and minimize the amount of pen- ctrant entering hollow-cored passages which might serve 1 [eneirant reservoirs, causing severe bleedout problems during ‘examination, Aerosol sprays are conveniently portable and suitable for local application ‘Nore 10-With spray applications, isimportantthathere be proper ‘eatlation. This is generally accomplished throygh these of a propery esiged spray boot: and exhaust stem. 85.1 Penetrant Dwell Time—Alter application, allow ex- ‘cess penetrant to drain from the part (care should be taken to prevent pools of peneirant from forming on the part), while allowing for proper pencirant dwell time (sce Table 2). The length of time the penetrant must remain on the part (o allow proper peneiration shouldbe 11 recommendedby the peneirant ‘manufacturer. Table2, however, provides a guide for selection of penetrant dwell times for a Variety of materials, forms, and types of discontinuities. Unless otherwise specified, the dwell time shall not exceed the maximum recommended by the manufacturer 8.6 Penetrant Removal 8.6.1 Water Washable (Method Aj 86.1.1 Removal of Water Washable Penetrant—After the required peneirant dwell time, the excess penetrant on the surface being examined must be removed with water. TL.can be removed manually with a coarse spray or wiping the part ‘water-spray equipment, of by waterimmerson, For immersion rinsing, parts are completely immersed inthe water bath with airor mechanical agitation, {a)"Thetemperatareof the watershalbe maintained within the range of 50° to 100°F [10° to 38°C]. () Spray rinse water pressure shall not exceed 40 psi [275 Pal. When hydro-ar pressure spray guns are used, the air pressure should not exceed 25 psi [172 kPa]. Nore I1—Oversushing should be avoided, Excessive washing ea catse poner to be washee ou of dsconsnaises. With Muorescer peseusttmethods perform the manal insiagopertiovunder black Hg 0 that it can be ccteminee when the surface penetra has boen ‘alogte'y removed TABLE 2 Recommended Minimum Dwell Tine um om Typeoh Dr Tres nas Neto Fi Dieeraly Ponaran® Devel “onan apres, asin an wa ‘Golds, poelylakoF aon 5 70 brass, ‘ack (aos) “Srdbronce, anim and grioreerawealoys wougtmeterak—eeusons, eps cracks alters) ® © ‘orggs si Ccrbisestppectons lackot son, ors cracks 5 0 Passe alioms asks 8 0 Gass aliens racks 8 2 corm ‘liems ra, pores 5 * Trova gear S010 1257 [010520] Forierpeauresbeiween 40 and60°F [and WO] ecormenda minamawalime of 20rines grrr penavaranel rsinaccorsanzeweh® 5 tiewscprien me boginsas soon sswel cesione'coainghas ied on sae of ees 617 Pats (osorendedmininusn) Naxinum degre mein aosodance withARTICLE 24, SE-165/SE-165M 86.1.2 Removal by Wiping (Method C)—After the required peneirant divell time, the excess peneirant is removed by ‘wipingwitha dry, clean, lint-reeclotvtowel. Then useaclean lin-freeclothowel lightly moistened with Water oF solvent to remove the remaining tracesof surface penetrant 11 determined by examination under black light for uorescent methods and visible light for visible methods 8.6.2 Lipophilic Fmulsfication (Method Bi: 86.2.1 Application of Lipophilic Emulsiie—Aftr the re- quired penetrant dwell time, the excess peneirant on the part ‘must be emulsified by immersing or fooding the pats with the required emulsifier (the emulsifier combines with the excess surface penetrant and makes the mixture removable by water rinsing). Lipophilicemulsiiershall notbe appli by spray oF brush and the part or emulsier shall not be agitated while being immersed. After application of the emulsifier, the parts shall be drained and positioned in a manner that prevents the ‘emulsifier ftom pooling on the par). 8.6.2.2 Emulsfication Time—The emulsification time be- gins 11S09n 1rtheerulsiierisappiied. Me lengthof time that theemulsifieris allowedoremainona partandincontact with the peneirant is dependent on the type of emulsifier employed and the surface roughness. Nominal emulsificationtime should bee 11 recommended by the manufacturer. The actual emulsifi- cation time must be determined experimentally for each specific application. The surface finish (roaghness} of the part ‘sa significant factor inthe selection of and inthe emulsince: tion time of an emulsifier. Contact time shall be kept to the "minimum time to obtain an acceptable background and shall ‘ot exceed three minates 8.6.2.3 Post RinsingEffective post rinsing of the emulsi- fied penowant from the surface can be accomplished using either manual, semi-automated, or automated waterimmersion or spray equipment or combinations thereof. 8.6.24 Immersion-For immersion post rinsing, parts are completely immersed in the waterbath withair oF mechanical agitation. The amount of time the partis inthe bath should be the minimum required to remove the emulsified peneirant. In addition, the temperature range ofthe Water should be $0 to 100°F (10 to 38°C]. Any necessary touch up rinse after an irmmersion rinse shall meet the requirements of 86.25. 8.6.2.5 Spray Post Rinsing Elective post riasing follow {ng emulsification can also be accomplished by ether manual or automatic water spray rinsing. The walerLemperatue shall be berween 50 and 100°F [10 and 38°C]. The water spray pressure shall not exceed 40 psi [275 kPal when manual spray {Runs are used. When hydro air pressure spray guns are used, the airpressure should not exceed 25 psi [172 KPa] 8.6.2.6 Rinse Effectveness—If the emulsification and final rinse step is not effective, 11 evidenced by excessive residual surface peneirant afer emulsification and tasing; thoroughly reclean and completely reprocess the part. 86.3 Hydrophilic Fmulsifcarion (Method D) 863.1 Application of Hydrophilic Rerover—Following the required penetrant well time, the parts may be preinsed with ‘waler prior to the application of hydrophilic emulsifier. This prerinse allows forthe removal of excess surface penetra from the pars prior to emulsification $0 14 to minimize 618 ASMERPVCY.2017 penetrant contamination in the hydrophilic emulsifier bath, thereby extending its ite. Tis notnecessary toprernse a part iff spray application of emulsificr is used 8.6.32 Prerinsing Controls—Biective preinsingisaccom- plished by manual, semi-automated, orautomsted water spray Fnsingof the par(6) The waterspray pressure shallnotexcced 40 psi [275 kPalwhenmanual orhydro air spray gunsareused, ‘When hyaro-i pressure spray guns ae used, the air pressure shall not exceed 25 psi [172 kPa]. Water free of contaminants: that could clog spray norles of leave a residue onthe part(s) is recommended, 8.6.33 Applicarionof Emulsfier—Theresidual surface en- ‘ctranton part(s) must be emulsified by immersing the part(s) in fan agicated hydrophilic emulsifier bath or by spraying the part(s) with Waterlemalsifier solutions thereby rendering the remaining residual surface penetrant water-washable for the finalrinse station. The emulsification timebegins tt soont tthe emulsifier is applied, The length of time that the emulsifier is allowed to remain on a part and in contact withthe penetrant is dependent on the type of emulsifier employed and the surface roughness. The emulsification time should be deter mined experimentally for each specific aplication. The sur face finish (roughness of the part is a significant factor in determining the emulsification time necessary for an emulsi- fier. Contact emulsification time should be Kept to the least possible time consistent with an acceptable background and shall not exceed two minutes. 8.6.3.4 Immersion—For immersion application, parts shall toe completely immersed in the emulsifier bath. The hydro: philic emulsifier concentration shall be 11 recommended by the ‘anafacturer andthebathor parishall be gently agitated by air or mechanically throughout the eye. ‘The minimum ime to ‘obtain an acceptable background shall be used, but the dwell timeshall notbe more than two minutes unlessapprovedby the contracting pares. 8.6.3.5 Spray Application For spray applications, all part surfaces should be evenly and uniformly sprayed with a ‘wateriemulsifier solution 10 effectively emulsify the residual peneirant on part surfaces to render it water-washable, The concentration of the erulsfior for spray applicationshould be inaccordance with the manufacturer’srecommendations butt, shall not exceed 5% The water spray pressure should be less ‘than 40 psi [275kpa].Contact with the emulsifier shallbe: eee to the minimum time to oblain an acceptable backgroun. shaotencced (vo rit The watrlemportre sal be maintained between SO and 100°F [10 and 38°C]. 8.6.3.6 Post-Rinsing of Hydrophilic — Emulsified Peneirants-Eifecive postrinsing of emulsified peneiran from the surface can be accomplished using ethermanual OF automated Waler spray, waler immersion, or combinations thereof. The total rinse time shall not exceed two rinutes regardless of the number of rinse methods used. 8.63.7 Immersion Pos-Rinsing-Hf an agitated immersion rinse isused, the amount of time the part(s) (are) in the at shall be the minimum required (o remove the emulsified shall not exceed two minutes, In adition, the temperature range of the water shall be within 50 and 100°F [10 and 38°C}, Be aware that a touch-up rinse may beASMEBPVCV-2017 necessary after immersion rinse, but the total wash time sil shall not exceed two minutes 8.6.3.8 Spray Post-Rinsing—Bifecive post tinsing follow- ing emulsification can also be accomplished by manual, semi-automatic, or automatic water spray. The water spray pressure shall not exceed 40 psi [275 kPa] when manual or hydroair spray guns are used. When hy ¢ro-airpressure spray guns are used, the ir pressure shall not exceed 25 psi [172 KPa]. The water temperature shall be between 50 and 100°F [10 and 38°C. The spray rinse time shall be Tess than two ‘minutes, unless otherwise specified 8.6.39 Rinse Ffectiveness—If the emulsification and final rinsesteps are not effective, snevidenced by excessive residual surface penetrant after emulsification and rinsing, thoroughly reclean, and completely reprocess the part. 8.6.4 Removal of Solvent-Removable Penetrant (Method Ch-After the required peneirant dell time, the excess pen- exrant is removed by wiping with a dry. clean, lint-fee lothftowel. Then use a clean, lint-free clothfowel lightly moistened with solvent remover to remove the remaining traces of surface peneirant. Gentle wiping must be used to avoid removing pencirant ftom any discontinuity. On smooth surfaces, an aliemate method of removal can be done by wiping with a clean, dry cloth, Flushing the surface with solvent following the application ofthe penetrant and prior to developing is prohibited 8.7 Drying—Regandlessof thetype and method of penctrant used, drying the surface of the parts) is necessary prior 10 applying dry or nonaqueous developers or following the application of the aqueous developer. Drying time will vary with the type of drying usedand thesize, nature, geometry,and number of parts being processed 8.7.1 Drying Parameters—Componcnts shal be air dried at room temperature or in a drying oven, Room temperature drying can be aided by the use of fans. Oven temperaturesshall rot exceed 160°F [71°C]. Drying time shall only be that necessary to adequately dry the part, Components shall be removed from the oven afier drying. Components should not bee placed in the oven with pooled water or pooled aqueous solutionssuspensions, 8.8 Developer Application—There ate various modes of effective application ofthe vatioustypes of developers uch 1 «dusting, immersing, floodingor spraying. The developer form, the part size, configuration, and surface roughness will influ tence the choive of developer application. 88.1 Dry Ponder Developer (Forma)—Dry powder devel ‘opers shall be applied after the partis dry in such a manner 1 toensurecompletecoverageof the areaofinterest Pariscan be immersed in a container of dry developer orin a fuid bed of dry developer. They can also be dusted with the powder developer through a hand powder bulb of a conventional or electrostatic powder gun. Tes common and effective to apply dry powder in an enclosed dust chamber, which creates an effective and controlled dustcloud. Other means suited to the size and geometry ofthe specimen may be used, provided the powder is applied evenly over the entire surface being exam- ined, Excess developer powder may be removed by shaking or tapping the part, or by blowing with low-pressure dry, clean, ARTICLE 24, E-165/SE-165M compressed air not exceeding 5 psi [34 kPa]. Dry developers shall not be used with Type TT penetra. 8.8.2 Aqueous Developers (Forms B and C}—Water soluble developers (Form B) are prohibited for use with Type 2 pencirins or Type 1, Method A penetrants, Water suspendable developers (FormC) can be used with both Type | and Type 2 penetrants. Aqueous developers shall be applied to the part immediately alir the excess peneirant has been removed and rior to drying, Aqueous developers shall be prepared and maintained in accordance with the manufacturer sinstructions and appliedin such a manner 11 ensure complete, ¥en, part coverage. Aqueous developers may be applied by spraying, flowing, of immersing the part in a prepared developer bath Immerse the parts only long enough 10 coat all of the part sarfaces with the developer since indications may leach out if the parts are let in the bath too long. After the paris are removed from the developer bath, allow the parts to drain Drain all excess developer from recesses and trapped sections to eliminate pooling of developer, which can obscure discon Linuities. Dry the parts in accordance with 8.7. The dried developer coating appears 11a translucent or whivecoatingon the part 8.8.3 Nonaqueous Wet Developers (Forms D and E}—Ater ‘the excess penetrant has been removed and the surface has been dried, apply nonaqueous wet developer by spraying in sacha manner 1 to ensure complete par coverage with athin, even film of developer, The developer shall be applied in manner appropriate to the type of penerun! being used. For visible dyo, the developer must be applied thickly enough to provide a contrasting background. For fluorescent dye, the developer must be applied thinly (o produce a translucent ‘covering, Dipping of looding parts with honacueous develop- esis prohibited, because the solvent action of these types of ovelopers can fush o dissolve the penetrant from within the discontinuities. [Nar 12—The vapors fromthe volasesolvent carerin thedeveloper _may'be Favandons, Propet ven aorshuulebe provide ates, ul especialy wher the developer is applied inside lose are, 8.84 Liquid Film Developers—Apply by spraying 1 rec~ ommended by the manufacturer. Spray partsin sucha manner oensure complete paricoverage of the areabeingexamined with a thin, even film of developer. 8.8.5 Developing Time—The length of time the developeris| to remain on the patt prior to inspection shall be not less than ten minutes, Developing time begins immediately after the application of dry powder developer oF 11 soon 11 the wet {agueous or nonaqueous) developer coating is dry (thats, the ‘water or solvent carrier has evaporated (0 dryness). ‘The maximum permitied developing times shall be four hours for dry powder developer (Form A), two hours for aqueous developer (Forms B and C), and one hour for nonagueous developer (Forms D and E), 8.9 Inspection—Afterthe applicable development time, per forminspectionof the paris under visible or ultraviolet light 1 appropriate. Itmay be helpful to observe the bieed out during the development time 14 an aid in interpreting indications 89.1 Uliravioiet Light Examination—Examine pans tested swith Type I fluorescent peneirant under black light in a 619ARTICLE 24, SE-165/SE-165M darkened area, Ambient light shall not exceed 2 fe [21.5 Ix]. ‘The measurement shall be made with a suitable visible Tight sensor atthe inspection surface. Nore 13_Becuuse the fuorescen constituents the penctrant will ‘vent fade withaect expose tou toll Figs, erect exposure ‘Of the paft under est Lo uiavilt Tigh shouté be minimized wher nol removing exoesspenetrttor evaluating incations. 89.1.1 Black Light Level Control—Black lights shall pro- vide a minimum light intensity of 1000 uWlenr, ata distance of 15 in, [38.1 em], The intensity shall be checked daily to censure the required output (sce Guide E2297 for more infor ‘mation). Reflectors and filters shall also be checked daily for cleanliness and integrity. Cracked or broken ultraviolet filters shall be replaced immediately. Since dropiin line voltagecan ‘cause decreased black light output with consequent inconsis- lent performance, a constant-valtage transformer should be used when there is evidence of voltage fluctuation. ‘Nore {4 Ceri igh tery black ight may emit unccepabie ans of vse Tigh. wHeh cas case foreseen into isappeer Care shoul be ker oon y se bulessuibie for resent erlang rps 89.1.2 Black Light Warm-Uip—Unless otherwise specified by the manufacturer, allow the black light to warm up for a ‘minimum of five minute prior to use or measurement ofits intensity 8.9.1.3 Visual Adaptation—Personnel examining pats afer penetrant processing shall be in the darened area for atleast one minute before examining parts. Longer times may be necessary under some circumstances. Photochromic of tinted lenses stall notbe womdaring the processing andexamination of pans. 8.9.2 Visible Light Exannation—Inspect pats tested with ‘Type? visible peneirant underether natural orartiticil visible light. Proper illumination is required to ensure adequace sensitivity ofthe examination. A minimumlight imensity atthe examination surface of 100 Fe{ 1076 xis required (see Guide 2297 for more information. 8.9.3 Housekeeping—Keep the examination area free of imcerfering debris, including uorescent residues and objeoss 8.9.4 Indication Verication—For Type | inspections only, itis common practice to verify indications by wiping the ingication witha solvent dampened swab oF brush, allowing theareato dry, and redeveloping thearea, Redevelopment ime shall be a minimum of ten minutes, except nonaqueous redevelopment time should be a minimum of three mines, IF theindiction does not reappear, the original indicationmaybe considered false. This procedare may be performedup to two times for any given original indication 8.9.5 Fvalvation—All indications found during inspection shall be evaluated in accordance with acceptance criteria specified. Reference Photographs of indications are noted in F433), 8.10 Post Cleaning Post cleaning is necessary when re- sida penctrant or developer could interfere with subsequent processing or with service requirements. Tt is particularly important where residual peneiran testing materials might ccomiine with other factors inservice to produce corrosion and prior to vapor degreasing oF heat treating the part 11 these 620 ASMERPVCY.2017 processes can bake the developer onto the part, A suitable technique, such 11 simple water rinse, water spray, machine solvent soak, or ultrasonic cleaning may be employed (sce Annex A| for further information on posteleaning). ILis recommended that if developer removal is necessary, it should bbecarricd out 11 promptly 11 possibleafterexamination so that the developer doesnot adhere tothe part 9. Special Requirements 9.1 Impurities: 9.1.1 When using penetrant materials on austenitic stainless steels, tanium, nickel-base or other high-temperature alloy the nced to restrict certain impurities such 14 sulfur, halogens and alkali meals must be considered. These impurities may cause embritlement oF corrosion, particularly at elevated temperatures. Any such evaluation shall also include consider ation of the form in which the impurities are present, Some ‘penetra materials contain significant runs of these impa- Titis in the form of volatile organic solvents that normally ‘evaporate quickly and usually do not cause problems, Other materials may contain impurities, which are not volatile and ‘may roaet withthe part, particularlyin the presence of moisture or elevated temperatures 9.1.2. Because volatile solvents Teave the sur ‘without reaction under normal exami ctrant materials are normally subjected to an evaporation procedure to remove the solvents before the materials are analyzed for impurities. The residue from this procedure is then analyzed in accordance with Test Method D1552 or Test ‘Method D129 decomposition followed by Test Mcthod E516, Method B (Turhidimetric Method for sulfur.The residue may so be analyzed by Test Method DBO8 or Annex A2 on Methods for Measuring Total Chlorine Contentin Combustible Liquid Penetrant Materials (for halogens other than fluorine) and Annex A3 on Method for Measuring ‘Total Fluorine Content in Combustible Liquid Penetration Materials (For fluorine). An aliemative procedure, Annex A on Determina- tion of Anions by Ton Chromatography, provides a single instrumental technique for rapid sequential measurement of common anions such 1 chloride, fuoride, and sulfate. Alkali imoials in the residue are determined by'flame photometry, atomic absorption spectrophotomeiry, oF ion chromatography (sec ASTM D4327}, Narr 15—Somecurrertstrdansreuireimpuriyevelsofslfurané ingens to ro excess 1% of any one suspect element. Ths est however, mey be unaccepable for some applications, s0 the actual ‘maxima acceplaietmpurtytevel mastbe deca betwcensoppirand userona by case bass 9.2. Blevated-Temperature Testing—Where penetra testing is performed on parts that must be maintained at elevated temperature during examination, special penetrant materials nd processing techniques may be required. Such examination requires qualification in accordance with 10.2 and the mand- facturer’s recommendations shall be observed. 10. Qualification and Requalification 10.1 Personnel Qualification—When required by the customer, all peneirant testing personnel shall be qualified? certified inaccordance witha written procedure conforming toASMEBPVCV-2017 the applicable edition of recommended Practice SNT-TC.1A, ANSI/ASNT CP-189, NAS-410, or MIL-STD-410. 102 Procedure Qualification Qualification of procedures using_times, conditions, or materials differing from those specified inthis general practice or for new materials may be performed by any of several methods and should be agreed ‘upon by the contracting parties. A test piece containing one or rote discontinuities of the smallest relevant size is generally used. When agreed upon by the contracting partis, the test piece may contain real or simulated discontinuities, providing itdisplaysthe characteristics of thediscontinuitiesencountered in product examination 10.2.1 Requalifcationof the procedare to be used may be required when a change is made to the procedure of when material substitution is made. ARTICLE 24, E-165/SE-165M 10.3 Nondesiructive Testing Agency Qualification I a rondestractivetesting agency 11 described in Practice BS43 is used to perform the examination, the agency should meet the requirements of Practice E543, 10.4 Requalifcarion may be required when a change or subsicution is made inthe type of peneirant materials or inthe procedure (see 10.2), 11, Keywords 11.1 fluorescent liquid penetrant tesing; hydrophilic emul: sification; lipophilic emulsification; liquid pencirant testing; nondestractive testing; solvent removable; visible liquid pen: ctrant testing; water washable; post-emulsified; black light; ultraviolet light; visible light ANNEXES (Mandatory Information) Al, CLEANING OF PARTS AND MATERIALS AL.1 Choice of Cleaning Method Al.1.1 Thechaiee ofa suitablecleaning method isbasedon such actors a8:(/)type of contaminant tobe removed since no ‘one method removes all contaminants equally well; 2) effect of the cleaning method on the parts; (3) practialty of the cleaning method forthe par(for example, large part cannot bee pul into a small dogreaser of ulirasoni cleaner); and () spevificcleaning requirements ofthe purchaser. The following cleaning methods are recommended Al.I-L1 Detergent Cleaning —Detcrgent cleaners are non- flammable water soluble compounds concaining specially lected surfactants for wetting, penetrating, emulsifying, and saponitying various types of soils, such 11 grease and oily films, cating and machining fuids, and unpigmented drawing compounds, ctc, etergentcleanersimaybealkaline, neutral, Of acidic in nature, but must be noncorrosive tothe item being, inspected. The cleaning properties of do-ergentsolution facili tate complete removal of soils and contamination from the surface and void areas, thus preparing them to absorb the peneurant. Cleaning time should be 11 recommended by the ‘manufacturer of the cleaning compound. Al.11.2 Solvent Cleaning—There are a variety of solvent leanersthat can be effectively uilizedtodissolvesuchsoils 11 srease and oily films, waxes and sealans, pains, and in feneral, orpanic matter These solvens should be residue tee, especially when used 11 hand. wipe solvent or 11 adip-tank degreasing solvent, Solvent cleaners are not recommended for the removal of rustand scale, welding flux and spatter, and in neral, inorganic soils, Some cleaning solventsareflaramable ind can be toxic. Observe all mamfacturers' instructions and precautionary noes 621 Al.1.1.3 Vapor Degreasing Vapor degreasing is a pre ferred method of removing oil oF grease-type soils from the surface of parts and from open discontinuities. Tt will not remove inorganic-type soils (dit, corrosion, salts, etc), amd "may not femove resinous soils (plastic coatings, varnish, paint, 2%c.). Because of the short contact time, degreasing may not completely clean out deep discontinuities and a subsequent solvent soak is recommended. Al.L.1.4 Alkaline Cleaning: (a) Alkaline cleaners are nonflammable water solutions containing specially selected detergents for wetting, penetrating, emulsifying, and saponifying various types of soils. Hotalkaline solutions arealso used for rust removal and descaling to remove oxide scale which can mask surface discontinuities, Alkaline cleaner compounds must be used in accordance with the manufacturers’ recommendations, Parts cleaned by the alkaline cleaning process must be rinsed completely free of cleaner and thoroughly dried prior to the peneirant testing process (part temperature at the time of ‘penetrant application shall not exceed 125°F [52°C]. (b)Steam cleaning is a modification of the hot-‘ank alka- line cleaning method, which can be used for preparation of large, unwieldy pars, Tcwill remove inorganic soils and many ‘organic sols from the surface of parts, butmaynotreach tothe bottom of deep discontinuities, and a subsequent solvent soak is recommended, 1.1.1.5 Ultrasonic Cleaning-This method addsultrasonic agitation o solvent or detergent cleaning to improve cleaning cfficiency and decrease cleaning time. It should be used with ‘watcrand detergeot ifthe soil tobe removedis inorganic (rus, dint salts, corrosion products, etc.) and with organiesolventit the soil (be removed is organic (greaseand 0ARTICLE 24, SE-165/SE-165M After ultrasonic cleaning, parts must be rinsed completely fe of cleaner, thoroughly dried, and cooled to at least 125°F [52°C], before application of pencirant. AI.1.1.6 Paint Removal—Paint films can be effectively removed by bond release solvent paint remover or dlisintegrating-¢ype hot-tank alkaline paint strippers. In most cases, thepaint film must be completely removed toexposethe surface of the metal, Solvent-ypepaint removerscan be of the high-viscosity thickened type forspray or brush application or can be of low viscosity two-layertype for dip-tank application, Both types of solvent paint removers are generally used at ambient temperatures, 14 received. Hot-tank alkaline strippers should be used in accordance with the manufacturer's insiruc- tions. After paint removal, the parts must be thoroughly rinsed {o remove all contamination from the void openings, thor ‘oughly dried, and cooled to at least 125°F [52°C] before application of penetrant. AL.1.1.7 Mechanical Cleaning and Surface Conditioning — ‘Motal-removing processes such 11 fling, bufling, scraping, mechanical milling, drilling, reaming, grinding, liquid honing, sanding, lathe cutting, tumble or vibratory deburring, and abrasive blasting, including abrasives such 11 glass beads, sand, aluminum oxide, ligno-cellulose pellets, metalic shot, cic., are often used to remove such soils 18 carbon, rust and scale, and foundry adhering sands, 11 well a1 to deburr or produce a desired cosmetic elfect on the part. These processes ‘may decrease the effectiveness of the penetrant testing by “smearing or peening over metal surfaces and fling disconti ‘uities open to the surface, especially for sofi metals such as ‘aluminum, titanium, magnesiwn, and beryllium alloy. AL.L.1.8 Acid EtchingTnhibited acid solutions (pickling solutions) are routinely uscd for descaling part surfaces, Descaling is necessary to remove oxide scale, which can mask surface discontinuities and prevent penetrant from entering, ASMERPVCY.2017 Acid solutionsietchants are also used routinely to remove ‘smeared metal that peens over surface discontinuities. Such ‘tchants should be used in aecordance with the manufacturers’ recommendations, Nor: AL 1—Biched parts and materials should be saseé completely free of ethants,thestrfacerearaizedanc thorough y Grea by heat prior ‘wappliation of peretans, Acdsand chromates car adverse yafestihe Fuorescence of noescent materi, ‘Na A12—Whoreverthereisapossibiliy hydrogen embritlement asaresult ofacidsolutorfetching. the par should be bakes al asutble ‘emperatureforan appropriaetimetoremove tehsdrozer before further processing. Aer baking, the partshall be cooled to atemperatre below 12S°F [52°C] before applying penetra, 1.1.1.9 Air Firing of Ceramics—Ieating of aceramic part in a clean, oxidizing atmosphere is an effective way of removing moistureor ight organic soilor both, The maximum temperature that will not cause degradation ofthe propercesof the ceramic should be used, A1.2 Post Cleaning Al.2.1 Removal of Developer—Dry powder developer can be effectively removed with an air blow. off (fre2 of oil) oF i can be removed withwatcrrinsing. Wetdevelopercoatings can be removed effectively by water rinsing or water rinsing with detergent either by hand of with a mechanical assist (serub brushing, machine washing, etc), The soluble developer coal ings simply dissolve off of the part with a water rinse. 1.2.2. Residual penetrant may be removed through solvent action, Solvent soaking (15 min minimum), and ultrasonic solvent cleaning @ min minimum) techniques are recom mended, Th some cases, it is desirable to vapor degrease, then follow with a solvent Soak. The actual time required in the ‘vapor degreaser and solvent soak will depend on the nature of the part and should be determined experimentally A2, METHODSFOR MEASURING TOTAL CHLORINE CONTENT IN COMBUSTIBLELIQUID PENETRANT MATERIALS ‘A2.1 Seope and Application AA2.1.1 These methods cover the determination of chlorine in combustible liquid penetrant materials, liquid or solid. Its range of applicability is 0.001 to 5% using either of the crmative titrimetric procedures. The procedures assume bromine of iodine will not be present. If these elements are present, they will bedetected and reported chlorine. The full smount of these elements will not be reported. Chromate interferes with the procedures, causing low or nonexistent end points. The method is applicable only to materials that are ‘wcll combustible. A2.2 Summary of Methods 2.2.1 The sample is oxidized by combustion in a bom containing oxygen under pressure (see 2.2.1.1). Thechlorine ‘compounds thus liberated are absorbed in a sodium carbonate solution and the amount of chloride present is determined 622 titimetrcally ether agains silver nitrate with the end point elected potentiomerically (Method A) oF coulometrcally with the end point detected by current flow increase (Method B) A22.1-1 Safeny—Strit adherence to all of the provisions prescribed hereinafter ensures against explosive rapture ofthe bomb, or a blow-out, provided the bom is of proper design and construction and in. good mechanical condition. Tt is esirable, however, thatthe bomb be enclosed in a shield of steel plate at least ¥ in, [127 mm] thick, or equivalent protection be provided against unforeseeable contingencies. A23 Apparatus A23.1 Bomb, having acapacity of not less than 300m, so constructed that it will not Teak during the test, and that quantitative recovery of the liquids from the boris may be readily achieved. The inner surface of the bomb may bemadeASMEBPVCV-2017 of stainless steo! or any other material that will not bealTected by the combustion process of products. Materials used in the bomb assembly, such 11 the head gasket and leadwire insulation, shall be resistant to heat and chemical action, and shall not undergo any reaction that will affect the chlorine ‘content of the liquid in the bom, 23.2 SampleCup, platinum, 24mm inoutside diameter at the bottom, 27 mm in outside diameter atthe top, 12 mm in height outside and weighing 10 10 11 g, opaque fused silica, ‘wide-form with an oulside dismeter of 29 mm at the top, a height of 19 mm, and a $-mL capacity (Nore 1), or nickel (Kawin capsule form), top diameter of 28 mam, 15 mm in height, and S-mL capacity Nor A2.1—Fosed silica ecules are mach more economical and longer asng than planar. Afereackse, they shoul be sere out wilh fire, wet emery cloth, heated to dulled heat overt bree, soskee Jnhot waterfor Ih ther dre ané stored in adesiccator before use. A2.33 Firing Wire, platinum, approximately No, 26B & S eage. A23.4 Ignition Circuit (Note A2.2), capable of supplying sulicien current to ignite the nylon thread oF cotion wicking ‘without melting the wire Nore A22—Theswitchin the gitoncieuitshoulé beofa type that remains open except whe Held it cose positon by the operator, A235 Nylon Sewing Thread, or Cotton Wicking, white A2.4 Purity of Reagents 24.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, itis intended that all reagentsshall conform to the specifications of the Commitee on Analytical Reagents of the American Chemical Society, where such specifications are available, Other grades may be used pro- vided it is first ascertained that the reagent is of suffciendy high purity to permit its use without lessening the accuracy of the determination. A2.4.2 Unless otherwise indicated, references to watershall be understood to mean referce grade reagent water conforming to Specification D1193. A235 SamplePreparation 2.5.1 Penetrants, Developers, Emulsifiers, Magnetic Oils: 2.5.1.1 Weigh 50 g of test material into a 150-mm pets dish 2.5.1.2 Placethe 150-mm petrdish intoa 194°F [90°C ]to 212°F [100°C| over for 60 minutes {A2,5.1.3 Allow the test material (o cool to room tempera: ture, A2.5.2 Solvent Cleaners ‘A2.5.2.1 Take the tare weight of an aluminum dish, A25.2.2 Weigh 100g ofthe cleanerinto the aluminum dish ARTICLE 24, E-165/SE-165M 2.5.2.3 Place the aluminum dish on a hot piate in a fume hood. AA2.5.2.4 Let the material evaporate until the dish is nearly ry. ‘A2.S.2.5 Place the dish into a preheated oven from 194°F [90°C} to 212°F [100°C] for 10 minutes. ‘A2.5.2.6 Take the dish out of the oven and allow to cool 2.5.2.7 Reweigh the dish and record weight [Nats A2.3—For Cleaners the residueis less than SO ppm, repo therescie weight Ifthe weight is pester thar SOppm,proceec will he ‘bomb procedure A2.6 Decomposition A2.6.1 Reagents and Materials A26.1.1 Oxygen, fre of combustible compounds, availble ata pressure of 2.6.1.2 Sodium Carbonate Solution (50 g NayCOt)— Dissolve'50 g of anhydrous NesCOs oF 58.5 of NisCOxs0) oF 135 g of Na,COs-10H,0 im water and dilute 9 FL. 26.13 White Oi refined A262 Procedure: 2.6.2.1 Preparation of Bomb and Sample—Cut a piece of firing wire approximately 100 mm in length. Coil the middie section (about 20 mm) andattach the free ends tothe terminal, ‘Arrange the col so that itwill beabove and to onesie of the sample cup. Place 5 mL. of NagCOs solution in thebomb (Note AA2.4), place the cover on the bomb and vigorously shake for 15, § (odistribute the solution over the inside of the bors, Open the bomb, place the sample-filled sample cup in the terminal holder, and insert a short length of thread between the fring ‘wire and the sample, Use of a sample weight containing over 20 mg of chlorine may cause corrosion of the bomb. The sample weight should not exceed 0.4 ifthe expected chlorine contentis2.5 % of above. If thesample is solid, not more than 0.2 gshould be used, Use 0.8 gof whiteoil with solid samples. ‘Tf white ol will be used (NoteA2.5), add it tothe samplecup by means of a dropper at this time (see Note A2.6 and Note 2.7), ‘Nore A2.4Aferrepeteduse of the bomb for chlorinedcteinaton, file may be goticea on the inner surface, This éullnss shoule be ‘emaved by periocie polishing ofthe bor, A satisfactory method For {airg this to rtaethebomsina lathe at about 30Orpm and polish the inside surface with Grit No. 20 of equivalent poper coutec with aight ‘muchineoil to preventcuttng, ang ther. wil apusteof gr ee brome foxigeand wae Thisprovedrewillromavcall butveryceeppitsandpul ‘absghpolsh on thestrface Beforeussng the bom, eshoulabe washes With soap and water to remove oil oF pase left from the polishing Dperation: Bombs wi porous oF psc surfaces should never be wee ‘neeae ofthe lerdeney to retain éhlrin From sample to sample. Ts ‘recommenced to not ust more tr g total ef sampeeand wht of othe chlorine fee combs materi NavrA25—Ithesample ‘snot rely miscible with white il some other ranvlsile, cherie fee combustbelluent may beemployed in pice of white oll, However, the combined weigh of sample ane rromlatilecluent shall not exceee 1g Some solid additives are Fettively Inslube, butmaybe stisfactr ly bared wher covered wi Sayer of white ‘NavrA26—The practice ofrunningalteately samples high andlow {nchlorneconlent shoule be avoided wheneverpossibe,Tis PO," and SO,7 41250 mm, 4.3.8 Guard Colum, identical o separator columnexcept 4 50 mm, to protect separator column from fouling by particulates oF organics 4.3.9 Suppressor Column, high-capacity cation-exchange resincapable of converting eluant and separated anions otheit acid forms, 43.10 Syringe, minimum capacity of 2m and equipped witha male pressure fiting, ‘Ad Reagents A44.1 Purity of Reagents—Reagent grade chemicals shall bbe used in all tests, Unless otherwise indicated, itis intended that all reagents shall conform to the specifications of the ‘Committee on Analytical Reagents of the American Chemical Society, where such specifications areavalable °Other grade ‘may be used provided ivi first ascertained that the reagent sufficiently high purity to permit its use without lessening the accuracy of the determination, 4.4.2 Deionized or Disiiled Water froe frominterferences atthe minimum detection limit of each constituent and filtered through a 0.2-am membrane filter (o avoid plugging columns. ARTICLE 24, E-165/SE-165M 4.4.3 Eluant Solution, sodium bicarbonatc-sodium carbonate, 0,003M NaHCOs_ 0,0024M NaxCOs: dissolve 1,008 g NaH1COs and 1.0176 g NaCO, in walcrand dilute to 4L, A444 Regenerant Solution 1, HySO}, 1 N, use this repen- cerant when suppressor is not a continuously regenerated one. A4A.S Regenerant Solution 2, HsSOy 0.025N, dilute 2.8 mL cone H,S0, 104 L or 100mLregenerantsolution 1104 L. Uscthisregenerant with continuoustegeneration fiber suppres- AMA Standard Anion Solutions, 1000 mg/L, prepare a series of standard anion solutions by weighing the indicated amount of salt, dried to a constant weight at 105°C, to 1000 mL, Storein plasticbotlesin a refrigerator, these solutionsare sable for atleast one month, ren se sma Py wo g % & Xe Sr So Poe Pe sa ee AdA.T Combined Working Standard Solution, High Range—Combine 10 mL. of the Cr, F-, NOx, NOZ, and O,* standard anion solutions, 1 mL of the BP of the SO," standand solutions, dilute to 1000 a plastic hot protected from ight contains 10 m-each of PF, NOx, NOY, and PO," I mg Br" /L, and 100 mg S71. Propane fresh daily AdA.8 Combined Working Standard Solution, Low Range— Dilute 100 mL. combined working standard solution, high range, to 1000 mi. and store ina plastic botle protected from light;conzains 1.Omp/l.eachCr, F’, NOs, NOs, and PO,™, 0.1 mg BrTL, and 10mg SO,-/L. Prepare fresh daily. AGA9 Alternative Combined Working Standard Solutions — Prepare appropriate combinations according to anion concen- tration to be determined, TF NO and PO,™ are not included, the combined working standard is sable for ne raonth ‘A4S Sample Preparation AGS.1 Penetrants, Developers, Fmulsfiers, Magnetic Oils AG5.1.1 Weigh 50 g of test material into a 150-mm petri dish Ad 51.2 Placethe 150-cnm petridish intoa 194°F[90°Clto 212°F [100°C] oven for 60 minutes. AGS. Allow the test material to cool to room tempera- ture, 4.5.2 Solvent Cleaners. 45.2.1 Take the tare weight of an aluminum dish, Ad 5.2.2 Weigh 100g fthe cleaner into thealuminum dish Ad.5.2.3 Place the aluminum dish on ahot plate in a fume hood. ‘45.2.4 Let the material evaporate until the dish is nearly ary, 629ARTICLE 24, SE-165/SE-165M ‘A4.S.2.5 Place the dish into a preheated oven from 194°F [90°C] to 212°F [100°C] for 10 minutes. ‘4.5.2.6 Take the dish outof the oven and allow to cool ‘A45.27 Reweighthe dish and record weight, Narr A43-For Cleaners—Il the resis les hat 50 pom, report theres thelist pp pesec te ym procedare. ‘A4,6 Decomposition Procedure A4.6.1 Preparation of Bomb and Sample—Cut a piece of firing wire approximazely 100 mm in length. Coil the middle section (about 20mm)and attach the free ends to the terminals. “Arrange the coil so that it will be above and to one side of the sample cup. Place 5 mL. of NasCOYNaHCOs solution in the ‘bomb, place the cover om the bomb, and vigorously shake for 15s odistriburethe solution over the inside of the bom. Open the bomb, place the sample-filled sample cup in the terminal holder, and insert a short length of thread between the Firing wire and the sample. The sample weight used should not exceed | g. Ifthe sample isa solid, add a few drops of white oil at this time to ensure ignition of the sample. Narr Ad.4Useofsample weights contsning over20 mg of chlorine ‘mayeausecorosionof the pom. To avo ths itisrecommended tl for sampiescontsnirg over 2 Sochorie, the sample weight be baseé onthe Tovtowing Chlosne sare vite corns woo wos 2108. o4 o4 Stoo 02 be 01029 oF or 201080 Bos oF CAUTION: Do rotuse more thar 1g tote of sample ané white olor ‘other Fucrre-free comoustibe mata. 4.6.2 Addition of Oxygen-Place the sample cup in posi tion and arrange the nylon thread, or wisp of cottonso that the tend dips into the sample. Assemble the bomb and tighten the cover securely. Admit oxygen (sce NotcA4.5) slowly ((o avoid blowing the sample from thecup) until apressureisreached 1 indicated in Table Ad.1 Nor: A4.S—Itisrecommendadtonotaddoxyger or ignite the sample ifthe bomb has beer jared, cropped, or tted 4.63 Combustion—Immerse the bomb in a cold-water ‘bath, Connect the terminals to theopen elecstical circuit, Close the circuit to ignite the sample. Remove the bomb from the bath after immersion for at least 10 min, Release the pressure at aslow, uniform rate such that the operation requires not less than 1 min. Open the bomb and examine the contents. If traces TABLE AA.1 Gage Pressures Cape of Bor mi. ge resus. atm ‘nTe aso 0 ‘sot0400 2 oore4s0 2 ‘so10500, 2 "Tho rininur pressures acted in powsesiAKantongen ore covaustonane Inomadirumosiuts presen assy querer 630 ASMERPVCY.2017 of unburned oil or sooty deposits are found, discard the determination, and thoroughly clean the bomb before again putting it in use, A464 Collection of SolutionRemove the sample cup with clean forcepsand rinse with deionized water and filterthe ‘washings into a 100-mL. volumetric flask, Rinse the walls of the bomb shell with a fine siream of deionized water from a ‘wash bottle, and add the washings through the filler paper to thefiask. Next, rinse the bombcoverand terminals andaddthe ‘washings through the filter into the volumetric flask, Finally, add deionized water to bring the contents ofthe flask to the line, Use aliquots of this solution for the ion chromatography AIC) analysis. AAT Procedure A4.2.1 System Fquilibration—Turn on ion chromatograph and. agjust eluant flow rate to approximate the separation achieved in Fig. A4,1 (2 to 3 mL/min). Adjust detector to desired setting (usually 10 pmo} and let system come to equilibrium (15 to 20 min). A stable base Tine indicates equilibrium conditions. Adjust detector offset to zero-cut cluant conductivity; with the Fiber suppressor adjust the regen- eration fow rate tomaintain stability, usually 2,5 to3 mLmin, ‘Ad.7.1.1 Setup the ion chromatograph in accordance with the manufacturer's instructions 47.2 Calibrarion—Inject standards containing a single anion ora mixture and determineapproximate retention times, ‘Observed times Vary with conditions but ifstandardeluant and anion separator column afe used, retention alway isin the order F5, Cr, NOF, PO,” Br, NOS and SO; Inject at Teast thee different concentrations for cach anion to be rncasured and construct a calibration cure by ploting peak height or area against concentration om linear graph paper. Recalibrate whenever the detector setting is changed. With a system requiring suppressor regeneration, NO ~ interaction ‘withthe suppressor may lead to erroneous NO." results; meke this determination only when the suppressor is at the same stage of exhaustion 11 during standardization or recalibrate frequently. Inthistype of ysiem the waterdip (see Note A45) ‘may shift slightly during suppressor exkaustion and with a fast run column this may lead toslight interferencefor or « To climinate this interference, analyze standards that bracket FIG. Aa.1 Typical Anion ProfileASMEBPVCV-2017 the expected result or eliminate the water dip by diluting the sample with cluant oF by adding concentrated eluant 10 the sampleto givethe same HCO;-/CO¥” concentration Vin the cluant. I sample adjustments are made, adjust standards and blanks identically [Nor A4.5—Waterdip occurs because water conductivity samples less thaneluanteonduetvty (eluant cilted by wate) 4.7.2.1 If linearity is established for a given detector setting, it is acceptable to calibrate with a single standard. Record the peak height or area and retention time to permit calculation of the calibration factor, F. A4.1.3 Sample Analysis Remove sample particulates, if necessary, by itering through a prewashed 0.2-ym-pore-diam membrane filter. Using a prewashed syringe of 1 10 10 mL capacity equipped with a male luer fing inject sample or standard. Inject enough sample (o flush sample loop several limes: for 0,1 ml. sample loop inject atleast I mL. Switch ion chromatograph from load to injeet mode and record peak heights and rogention times on sirip chart recorder. After the last peak (SO )hasappeared and the conductivity signalhas returned (o base Line, another sample can be injected, ARTICLE 24, E-165/SE-165M A4.7.4 Regeneration—Forsystems without fiber suppressor regenerate with 1 N H,S0, in accordance with the manufac: turer's instructions when the conductivity base line exco 300 umho when the suppressor column is on lin. A488 Caleulation 4.8.1 Calculate concentration of each anion, in mg/L, by referring t© the appropriate calibration curve, Aliernatively, ‘when the response is shown to be Tinear, use the following equation: HUFLD (aan where: C= mpanionil., H = peak height or area, F = response factor—concentration of standardheight (or area) of standard, and D__= dilution factor for those samples requiring dilution, A4.9 Precision and Bias 49.1 Samples of reagent water (o which were added the common anions were analyzed in 15 laboratories with the results shown in Table A4.2. ‘TABLE 4.2 Precisionand Accuracy Observed for Anions at Various Concentration Levelsin Reagent Water mak Sms sion Arcane Ano ora Sper 0008 ret at Peron mot mgt = oe 7 308 038 E iat ie 3% oe & an ase os on & 2 # oe a8 & “ ah & * Soe Gas 008 Goo doe Ae aS ee ie 8 e 23 ea oo cae ee oF 88 ie os Be Se oto doe tee ee oe oa ots oF he 380 033 oie te nee e ae 6 a sae oS ase aor on sor “i 8 3 EH 631