astm e 165 (liquidos penetrantes).pdf

An American National StandardDesignation: E 165 – 02 Standard Test Method for Liquid Penetrant Examination1 This standard is issued under the fixed designation E 165; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval. 1. Scope D 129 Test Method for Sulfur in Petroleum Products (Gen- 1.1 This test method2 covers procedures for penetrant ex- eral Bomb Method)3 amination of materials. They are nondestructive testing meth- D 516 Test Method for Sulfate Ion in Water4 --``,,,,`,,,,``,`,```,,,``,``,,-`-`,,`,,`,`,,`--- ods for detecting discontinuities that are open to the surface D 808 Test Method for Chlorine in New and Used Petro- such as cracks, seams, laps, cold shuts, laminations, through leum Products (Bomb Method)3 leaks, or lack of fusion and are applicable to in-process, final, D 1193 Specification for Reagent Water4 and maintenance examination. They can be effectively used in D 1552 Test Method for Sulfur in Petroleum Products the examination of nonporous, metallic materials, both ferrous (High-Temperature Method)3 and nonferrous, and of nonmetallic materials such as glazed or D 4327 Test Method for Anions in Water by Chemically fully densified ceramics, certain nonporous plastics, and glass. Suppressed Ion Chromatography4 1.2 This test method also provides a reference: E 433 Reference Photographs for Liquid Penetrant Inspec- 1.2.1 By which a liquid penetrant examination process tion5 recommended or required by individual organizations can be E 543 Practice for Evaluating Agencies that Perform Non- reviewed to ascertain its applicability and completeness. destructive Testing5 1.2.2 For use in the preparation of process specifications E 1208 Test Method for Fluorescent Liquid Penetrant Ex- dealing with the liquid penetrant examination of materials and amination Using the Lipophilic Post-Emulsification Pro- parts. Agreement by the user and the supplier regarding cess5 specific techniques is strongly recommended. E 1209 Test Method for Fluorescent Liquid Penetrant Ex- 1.2.3 For use in the organization of the facilities and amination Using the Water-Washable Process5 personnel concerned with the liquid penetrant examination. E 1210 Test Method for Fluorescent Liquid Penetrant Ex- 1.3 This test method does not indicate or suggest criteria for amination Using the Hydrophilic Post-Emulsification Pro- evaluation of the indications obtained. It should be pointed out, cess5 however, that after indications have been produced, they must E 1219 Test Method for Fluorescent Liquid Penetrant Ex- be interpreted or classified and then evaluated. For this purpose amination Using the Solvent-Removable Process5 there must be a separate code or specification or a specific E 1220 Test Method for Visible Penetrant Examination agreement to define the type, size, location, and direction of Using the Solvent-Removable Process5 indications considered acceptable, and those considered unac- E 1316 Terminology for Nondestructive Examinations5 ceptable. E 1418 Test Method for Visible Penetrant Examination 1.4 The values stated in inch-pound units are to be regarded Using the Water-Washable Process5 as the standard. SI units are provided for information only. 2.2 ASNT Document: 6 1.5 This standard does not purport to address all of the Recommended Practice SNT-TC-1A for Nondestructive safety concerns, if any, associated with its use. It is the Testing Personnel Qualification and Certification responsibility of the user of this standard to establish appro- ANSI/ASNT CP-189 Standard for Qualification and Certi- priate safety and health practices and determine the applica- fication of Nondestructive Testing Personnel bility of regulatory limitations prior to use. 2.3 Military Standard: MIL-STD-410 Nondestructive Testing Personnel Qualifica- 2. Referenced Documents tion and Certification7 2.1 ASTM Standards: 2.4 APHA Standard: 1 3 This test method is under the jurisdiction of ASTM Committee E07 on Annual Book of ASTM Standards, Vol 05.01. 4 Nondestructive Testing and is the direct responsibility of Subcommittee E07.03 on Annual Book of ASTM Standards, Vol 11.01. 5 Liquid Penetrant and Magnetic Particle Methods. Annual Book of ASTM Standards, Vol 03.03. 6 Current edition approved February 10, 2002. Published April 2002. Originally Available from the American Society for Nondestructive Testing, 1711 Arlin- published as E 165 – 60 T. Last previous edition E 165 – 95. gate Lane, Columbus, OH 43228-0518. 2 7 For ASME Boiler and Pressure Vessel Code applications see related Recom- Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 mended Test Method SE-165 in the Code. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS. Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. Copyright ASTM International 1 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale, 08/09/2005 09:01:58 MDT E 165 429 Method for the Examination of Water and Wastewater8 require the use of black light. However, visible penetrant 2.5 AIA Standard: indications must be viewed under adequate white light (see NAS-410 Certification and Qualification of Nondestructive 8.9.2.1). Test Personnel6 TABLE 1 Classification of Penetrant Examination Types and 3. Terminology Methods 3.1 The definitions relating to liquid penetrant examination, Type I—Fluorescent Penetrant Examination which appear in Terminology E 1316, shall apply to the terms Method A—Water-washable (see Test Method E 1209) Method B—Post-emulsifiable, lipophilic (see Test Method E 1208) used in this standard. Method C—Solvent removable (see Test Method E 1219) Method D—Post-emulsifiable, hydrophilic (see Test Method E 1210) 4. Summary of Test Method Type II—Visible Penetrant Examination 4.1 A liquid penetrant which may be a visible or a fluores- Method A—Water-washable (see Test Method E 1418) cent material is applied evenly over the surface being examined Method C—Solvent removable (see Test Method E 1220) and allowed to enter open discontinuities. After a suitable dwell time, the excess surface penetrant is removed. A devel- oper is applied to draw the entrapped penetrant out of the 7. Types of Materials discontinuity and stain the developer. The test surface is then 7.1 Liquid penetrant examination materials (see Notes 3 examined to determine the presence or absence of indications. and 4) consist of fluorescent and visible penetrants, emulsifiers NOTE 1—The developer may be omitted by agreement between pur- (oil-base and water-base), solvent removers and developers. A chaser and supplier. family of liquid penetrant examination materials consists of the NOTE 2—Caution: Fluorescent penetrant examination shall not follow applicable penetrant and emulsifier or remover, as recom- a visible penetrant examination unless the procedure has been qualified in mended by the manufacturer. Intermixing of penetrants and accordance with 10.2, because visible dyes may cause deterioration or emulsifiers from various manufacturers is not recommended. quenching of fluorescent dyes. NOTE 3—Refer to 9.1 for special requirements for sulfur, halogen and 4.2 Processing parameters, such as surface precleaning, alkali metal content. penetration time and excess penetrant removal methods, are NOTE 4—Caution: While approved penetrant materials will not ad- determined by the specific materials used, the nature of the part versely affect common metallic materials, some plastics or rubbers may be under examination, (that is, size, shape, surface condition, swollen or stained by certain penetrants. alloy) and type of discontinuities expected. 7.2 Penetrants: 7.2.1 Post-Emulsifiable Penetrants are designed to be in- 5. Significance and Use soluble in water and cannot be removed with water rinsing 5.1 Liquid penetrant examination methods indicate the pres- alone. They are designed to be selectively removed from the ence, location and, to a limited extent, the nature and magni- surface using a separate emulsifier. The emulsifier, properly tude of the detected discontinuities. Each of the various applied and given a proper emulsification time, combines with methods has been designed for specific uses such as critical the excess surface penetrant to form a water-washable mixture, service items, volume of parts, portability or localized areas of which can be rinsed from the surface, leaving the surface free examination. The method selected will depend accordingly on of fluorescent background. Proper emulsification time must be --``,,,,`,,,,``,`,```,,,``,``,,-`-`,,`,,`,`,,`--- the service requirements. experimentally established and maintained to ensure that over-emulsification does not occur, resulting in loss of indica- 6. Classification of Penetrations and Methods tions. 6.1 Liquid penetrant examination methods and types are 7.2.2 Water-Washable Penetrants are designed to be di- classified as shown in Table 1. rectly water-washable from the surface of the test part, after a 6.2 Fluorescent penetrant examination utilizes penetrants suitable penetrant dwell time. Because the emulsifier is “built- that fluoresce brilliantly when excited by black light (see in” to the water-washable penetrant, it is extremely important 8.9.1.2). The sensitivity of fluorescent penetrants depends on to exercise proper process control in removal of excess surface their ability to be retained in the various size discontinuities penetrant to ensure against overwashing. Water-washable pen- during processing, then to bleed out into the developer coating etrants can be washed out of discontinuities if the rinsing step and produce indications that will fluoresce. Fluorescent indi- is too long or too vigorous. Some penetrants are less resistant cations are many times brighter than their surroundings when to overwashing than others. viewed under black light illumination. 7.2.3 Solvent-Removable Penetrants are designed so that 6.3 Visible penetrant examination uses a penetrant that can excess surface penetrant can be removed by wiping until most be seen in visible light. The penetrant is usually red, so that the of the penetrant has been removed. The remaining traces indications produce a definite contrast with the white back- should be removed with the solvent remover (see 8.6.4.1). To ground of the developer. The visible penetrant process does not minimize removal of penetrant from discontinuities, care should be taken to avoid the use of excess solvent. Flushing the surface with solvent to remove the excess penetrant is prohib- 8 Available from American Public Health Association, Publication Office, 1015 ited. Fifteenth Street, NW, Washington, DC 20005. 7.3 Emulsifiers: Copyright ASTM International 2 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale, 08/09/2005 09:01:58 MDT may adversely 8. The emulsification time will vary. depending on its conditioning by grinding. grease. However. Figs.2.5).. All of these suspensions of resins/polymer in a suitable carrier. coating on the surface of the part when dried. and so forth. The concentration.``.6.. surface preparation by powder particles to be either suspended or dissolved (soluble) grinding. pickling solutions and chromates. these may be removed by wiping with clean lint-free excess penetrant film from the surface of the part through cloths. penetrant as described in 8.3. wet developers form a as a weld.5.`. use and maintenance shall be generally less easily rinsed away and are therefore less suitable in accordance with manufacturer’s recommendations.``. surface and discontinuity being free of any contaminant (solid or liquid) that might interfere with the penetrant process. as-cast.3.8.3. which can be monitored by the use of a suitable follow shot. scale. thus that degrades the effectiveness of penetrant examination.2. in particular. All 7. and so forth..4 Removal of Surface Contaminants: NOTE 5—Caution: Aqueous developers may cause stripping of indica- 8. Drying may Copyright ASTM International 3 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. graphite.5. dirt.4 Liquid Film Developers are solutions or colloidal that might interfere with the penetrant process. They are either slow. ined as defined by the contracting parties.. surface the process of bringing the penetrant out of open discontinui. as-rolled. These contaminants can prevent the penetrant from entering discon- developers will form a transparent or translucent coating on the tinuities (see Annex on Cleaning of Parts and Materials).. welding by spray only. A1.`.1.3). etching shall be per- 7..3 Nonaqueous Wet Developers are supplied as suspen. and between 40° and 125°F (4° and 52°C).1 Dry Powder Developers are used as supplied (that is.6.1 Lipophilic Emulsifiers are oil-miscible liquids used to fluorescent and visible penetrant examination methods (see emulsify the excess oily penetrant on the surface of the part. Sensitive penetrants are dip or spray. 8.) 7. skin and when penetrant entrapment in surface irregularities 7. materials and the surface of the part to be processed should be depending on their viscosity and chemical composition..4. The rate of diffusion establishes 8.4. including the heat affected zone is to be examined.1. parts or areas of parts to be examined must be clean and dry sions of developer particles in a nonaqueous solvent carrier before the penetrant is applied. procedure as described in 10. “Clean” is intended NOTE 6—Caution: This type of developer is intended for application to mean that the surface must be free of rust.1. machining. non-caking powder) in accordance with 8. react with the penetrant and reduce its sensitivity and performance. grit blasting free-flowing. rendering it water-washable. 7. might mask the indications of unacceptable discontinuities or --``. Where it is not practical also the surface roughness of the area being examined (see to comply with these temperature limitations. treatments or service usage have produced a surface condition ties through blotting action of the applied developer. NOTE 7—When agreed between purchaser and supplier.3 Surface Conditioning Prior to Penetrant Examination— surface of the part. grit or vapor blasting to remove the peened refractometer. insulating materials.6. since any liquid 8. polishing or etching shall concentration. while the detergent displaces the film of penetrant from the part vapor degreasing or chemical removing processes. 08/09/2005 09:01:58 MDT . 7. Nonaqueous.5.``.8. as the penetrant specks can appear as nuities and extreme care should be used with grinding and machining indications. (See increasing the visibility of the indications. qualify the 8.2 Temperature Limits—The temperature of the penetrant the emulsification time. without subsequent etching may be an acceptable cleaning method.. flux. E 165 7.5.2 at the temperature of intended 7.1 The following processing guidelines apply to both residue will hinder the entrance of the penetrant. rendering it water-washable (see 8.4 Solvent Removers function by dissolving the penetrant.5 Developers—Development of penetrant indications is formed when evidence exists that previous cleaning. paint. sand blasting and etching for penetrant examination is not recommended because of the potential for damage.4. Procedure of parts be thoroughly dry after cleaning.. 8.3)..2. use and maintenance shall be in accordance with manufacturer’s recommendations (see 8. When only loose surface residuals are 7. used to emulsify the excess oily fluorescent penetrant on the 8..6. 1-3). weld spatter.-`-`. or as-forged conditions (or for supplied as concentrates to be diluted with water and used as a ceramics in the densified conditions). Surface surface.8.4).2 Drying after Cleaning—It is essential that the surface 8. which serves as all contaminants shall be removed from the area being exam- the developing medium (see 8. in water. oily films. unless otherwise specified.`--- making it possible to wipe the surface clean and free of excess otherwise interfere with the effectiveness of the examination. The concentration.8 for precautions. for rough surfaces.1 Hydrophilic emulsifiers function by displacing the present.2 and 8. should be done using cleaning solvents. The procedure should be tion procedure is greatly dependent upon the surrounding qualified in accordance with 10. precleaning of metals to remove processing detergent action.1 Precleaning—The success of any penetrant examina- tions if not properly applied and controlled.```.2). agitation in an open dip tank provides the scrubbing action coatings. such ready for use as supplied. scale.8.2 Hydrophilic Emulsifiers are water-miscible liquids use and as agreed to by the contracting parties.`.`.or fast-acting. The force of the water spray or air/mechanical residuals such as oil.`. operations to avoid masking discontinuities.2 Aqueous Developers are normally supplied as dry NOTE 9—For structural or electronic ceramics. If only a section of a part. Care should be taken not to contaminate the developer with NOTE 8—Caution: Sand or shot blasting may possibly close disconti- fluorescent penetrant. For metals.. Satisfactory results usually may be obtained on surfaces in the These water-base emulsifiers (detergent-type removers) are as-welded. surface of the part. Certain types of film developer may be NOTE 10—Caution: Residues from cleaning processes such as strong stripped from the part and retained for record purposes (see alkalies. sand. 08/09/2005 09:01:58 MDT . (See 8. or exposure to ambient tempera. flooding.. Solvent Alkaline Steam Acid Etch grease Wash (See 8.1) Mechanical Paint Stripper Ultrasonic Detergent DRY (See 8.8) Developer Dry (Aqueous) DEVELOP DRY Developer. Both conventional infrared lamps. Ultrasonic Solvent Soak grease Clean Outgoing Parts FIG.7) Dry. and those with complex geometries. application can eliminate excess liquid build-up of penetrant on dried.7) (See 8.``..9. forced hot air.4.`. with applied effectively by brushing or spraying. Aerosol sprays are conveniently portable and 8. Small parts are quite often placed in NOTE 11—Caution: Not all penetrant materials are suitable for elec- suitable baskets and dipped into a tank of penetrant.`.`--- Fluorescent (See 8..`.`. liquid penetrants to the part surfaces.1) Spray Dip DRY DEVELOP (See 8.``. or spraying. the the part.``. examination.. On larger trostatic spray applications. E 165 Incoming Parts PRECLEAN Vapor De.1) Examine Visible (See 8. and is within the specified temperature range. parts.5... Electrostatic spray 8... brushing. it is important that there Copyright ASTM International 4 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. so tests should be conducted prior to use.`.8) (See 8. Nonaqueous or Dry Liquid Film EXAMINE --``.-`-`.2) Dry PENETRANT Apply Water- APPLICATION Washable (See 8. penetrant can be NOTE 12—Warning: With spray applications. and minimize the amount of penetrant is applied to the surface to be examined so that the penetrant entering hollow-cored passages which might serve as entire part or area under examination is completely covered penetrant reservoirs.1 Modes of Application—There are various modes of suitable for local application.) Dry Vapor De. 1 General Procedure Flowsheet for Penetrant Examination Using the Water-Washable Process (Test Method E 1209 for Fluorescent and Test Method E 1220 for Visible Light) be accomplished by warming the parts in drying ovens.2) Mechanical Water Rinse Detergent Wash POST CLEAN (See 8.10 and An- nex A1 on Post Cleaning.```..5 Penetrant Application—After the part has been cleaned.5) Penetrant FINAL RINSE Water Wash (See 8. minimize overspray.. causing severe bleedout problems during with penetrant.4. and electrostatic spray guns are effective means of applying ture.6..9.. effective application of penetrant such as dipping. `.``.. 08/09/2005 09:01:58 MDT .`.-`-`.`..`.`..```....`--- Copyright ASTM International 5 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale....``..``.. 2 General Procedure Flowsheet for Post-emulsifiable Method --``.. E 165 FIG. 08/09/2005 09:01:58 MDT .4.`.``..7) Dry --``.2) Mechanical Water Rinse Detergent Wash POST CLEAN (See 8.6. The 8. E 165 Incoming Parts PRECLEAN Vapor De- Alkaline Steam Solvent Wash Acid Etch (See 8.. Table 2.4) Wipe-Off DRY (See 8. allow ex.2) Dry PENETRANT Apply APPLICATION Solvent- (See 8. and operation. This is generally accomplished through the use of a NOTE 13—For some specific applications in structural ceramics (for properly designed spray booth and exhaust system. provides a guide for selection examined must be removed with water. 3 Solvent-Removable Penetrant Examination General Procedure Flowsheet (Test Method E 1219 for Fluorescent and Test Method E 1220 for Visible Light) be proper ventilation. For immersion rinsing. the excess penetrant on the surface being manufacturer.9. parts are completely im- manufacturer.5. It can be washed off manually.`. detecting parting lines in slip-cast material)..```. mersed in the water bath with air or mechanical agitation. the required penetrant dwell time should be determined experimentally and may be 8.2 Penetrant Dwell Time—After application.1) Examine Visible (See 8. Unless otherwise specified.5) Removable Fluorescent Penetrant REMOVE EXCESS PENETRANT Solvent (See 8.`..`. while 8.1 Water Washable: length of time the penetrant must remain on the part to allow 8.6..1..7) Dry DEVELOP Nonaqueous (See 8.1 Removal of Excess Penetrant—After the required proper penetration should be as recommended by the penetrant penetration time.4. cess penetrant to drain from the part (care should be taken to prevent pools of penetrant from forming on the part). by the use of types of discontinuity...1) grease Mechanical Paint Stripper Ultrasonic Detergent DRY (See 8.9. however.6..``. forms. usually a washing of penetrant dwell times for a variety of materials.`..8) Wet or Liquid Aqueous Film Devel.6 Penetrant Removal allowing for proper penetrant dwell time (see Table 2).. example.``.10 and An- nex A1 on Post Cleaning) Dry Vapor De. Ultrasonic Solvent Soak grease Clean Outgoing Parts FIG.-`-`. the dwell automatic or semi-automatic water-spray equipment or by time shall not exceed the maximum recommended by the immersion. Copyright ASTM International 6 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. Developer oper DRY (see 8. longer than that shown in Table 1 and its notes..`--- EXAMINE Fluorescent (See 8. separating the penetrant from for each specific application.``. Contact time should be plished by either manual or automated water spray rinsing of kept to the least possible time consistent with an acceptable the parts as follows: background and should not exceed the maximum time speci. Caution: A touch-up rinse may be NOTE 14—Caution: Avoid overwashing.. cracks (all forms) 10 10 forgings. 8. (a) The maximum dip-rinse time should not exceed 120 s --``. the excess penetrant on the part must be surface penetrant after emulsification and rinsing. s unless otherwise specified by part or materials specification. The time and temperature should be kept constant.6. (a) Control rinse water temperature within the range of 50° etrant removal may be performed by wiping the surface with a to 100°F (10° to 38°C).4° and 10°C).4 Immersion—For immersion post rinsing.`. minimizes possible oily penetrant pollution in the final rinse tion time should be as recommended by the manufacturer.6. thereby penetrant is dependent on the type of emulsifier employed and extending its life..2 Removal by Wiping—In special applications.2.3 Post Rinsing—Effective post rinsing of the emulsi- must be avoided. parts are (a) The temperature of the water should be relatively completely immersed in the water bath with air or mechanical constant and should be maintained within the range of 50° to agitation. as evidenced by excessive residual etration time. Maximum development time in accordance with 8.6. prior to emulsification (8. (b) The temperature of the water should be relatively (c) Rinse time should not exceed 120 s unless otherwise constant and should be maintained within the range of 50° to specified by part of material specification.3. castings and welds cold shuts.5. C Development time begins as soon as wet developer coating has dried on surface of parts (recommended minimum). This step allows for the 8. prerinsing of penetrated parts the surface condition (smooth or rough). either manual.1 Application of Emulsifier—After the required pen. it is recommended that the parts be prerinsed with water part(s).7) and reclean the part.. rinse step is not effective.3.2 Emulsification Dwell Time begins as soon as the removal of excess surface penetrant from the parts prior to emulsifier has been applied. spray nozzles or leave a residue on parts.`. 40 psi (280 kPa). B Maximum penetrant dwell time in accordance with 8.. under black light for fluorescent methods and white light for (c) The maximum spray rinse time should not exceed 120 visible methods. then reapply the penetrant for or spray equipment or combinations thereof.2.3). 5 10 brass cracks (all forms) and bronze. laps. semi-automated. penetrant to be washed out of discontinuities.2..6.`. the part is a significant factor in the selection of and in the 8.. For temperatures between 40° and 50°F (4. lack of fusion. or automatic water spray rinsing of the parts as follows: 8. as fied penetrant from the surface can be accomplished using evidenced by excessive residual surface penetrant after rinsing.6. cracks 5 10 Plastic all forms cracks 5 10 Glass all forms cracks 5 10 Ceramic all forms cracks. Nominal emulsifica. the prescribed dwell time. absorbent material dampened with water until the excess (b) Spray rinse water pressure should not exceed 40 psi surface penetrant is removed. The step of this process.2 Lipophilic Emulsification: 8. or automated water immersion dry (see 8. porosity. Excessive washing can cause necessary after immersion..5 Spray Post Rinsing—Effective post rinsing follow- methods perform the rinsing operation under black light so that it can be ing emulsification can also be accomplished by either manual determined when the surface penetrant has been adequately removed. plate Carbide-tipped tools lack of fusion...``. clean. 8. as determined by examination (275 kPa). With fluorescent penetrant 8.7) emulsified by immersing or flooding the parts with the required and reclean the part and reapply the penetrant for the pre- emulsifier (the emulsifier combines with the excess surface scribed dwell time.3 Hydrophilic Emulsification: ing).`. titanium and high-temperature alloys wrought materials—extrusions. This is accomplished by collecting the actual emulsification time must be determined experimentally prerinsings in a holding tank..2. 100°F (10° to 38°C). The surface finish (roughness) of water. recommend a minimum dwell time of 20 minutes.. penetrant and makes the mixture removable with water rins.6. After application of the emulsifier. 100°F (10° to 38°C). Accumulation of water in pockets or recesses of the surface 8. the parts are drained in 8.-`-`. dry (see 8.6. porosity 5 10 A For temperature range from 50° to 125°F (10° to 52°C). 08/09/2005 09:01:58 MDT .1.``.6.2.8. porosity.`. Copyright ASTM International 7 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale.6 Rinse Effectiveness—If the emulsification and final 8.6. If the final rinse step is not effective. In addition. magnesium. The length of time that the emulsification so as to minimize the degree of penetrant emulsifier is allowed to remain on a part and in contact with the contamination in the hydrophilic emulsifier bath. 8.2.6.```.2 Prerinsing Controls—Effective prerinsing is accom- emulsification time of an emulsifier. E 165 TABLE 2 Recommended Minimum Dwell Times Type of Dwell TimesA (minutes) Material Form Discontinuity PenetrantB DeveloperC Aluminum.6.6..6.`--- (b) Spray-rinse water pressure should not be greater than unless otherwise specified by part or material specification.3. (a) Water should be free of contaminants that could clog fied for the part or material.2. steel. pen.1 Prerinsing—Directly after the required penetration a manner that prevents the emulsifier from pooling on the time. dusting.. Parts can be immersed in a tions thereof. Oven temperatures shall of an emulsifier.4 Immersion—For immersion application.`. by difficulty in removing the excess penetrant. can be post-rinsed by water spray rinsing as follows: (d) Prerinse time should be the least possible time (nomi.3. to ensure complete part coverage.6. (c) Spray rinse at a water pressure of 25 to 40 psi (175 to 8. Then using a lint-free material lightly moistened with emulsifier should be gently agitated throughout the contact solvent remover the remaining traces are gently wiped to avoid cycle..6).``. surface condition. possible.3.`. penetrant on parts.1 Drying Parameters—Components shall be air dried at the prerinse step.``.5) thereby rendering the 8.1 Removal of Excess Penetrant—After the required remaining residual surface penetrant water-washable in the penetration time.. unless otherwise approved by the cognizant engineering the application of the aqueous developer. Other means suited to the size and geometry (b) The maximum dip rinse time should not exceed 120 s of the specimen may be used. air and 40 psi (280 kPa) max for water. nature. container of dry developer or in a fluid bed of dry developer.3. the penetrant and prior to developing is prohibited.6 Post-Rinsing of Hydrophilic Emulsified Parts— forth.9 If the emulsification and final rinse steps are not 8. aqueous solutions/suspensions. The hydrophilic removed. lint-free material and 8.8 Developer Application: (d) Contact time should be kept to the minimum consistent 8. but should not exceed 5 %. configura- cation.`--- etration time and following the prerinse. with the size. Nominal use concentration for immersion appli. E 165 (b) Control water temperature within the range of 50 to unless otherwise specified by part or material specification. 08/09/2005 09:01:58 MDT .6.7 Immersion Post-Rinsing—Parts are to be completely They can also be dusted with the powder developer through a immersed in the water bath with air or mechanical agitation. will influence the choice of developer application. (a) Control rinse water temperature within the range of 50 nally 60 s maximum) to provide a consistent residue of to 100°F (10 to 38°C). trolled dust cloud.6..3.7. and so 8.-`-`.8. and number of parts under examination. 8. dry the part (see cations is 20 %... If the wiping step is not effective.4 Solvent-Removable Penetrants: the part(s) with the emulsifier (8. the excess penetrant is removed insofar as final rinse station (8.6. 100°F (10 to 38°C).6.7). parts are emulsified by the spray application room temperature or in a drying oven.3. The size.. effective.3 Application of Emulsifier—After the required pen. 8. part(s) in a hydrophilic emulsifier bath (8. or should be applied immediately after drying in such a manner as automated water immersion or spray equipment or combina. 8.. removing penetrant from discontinuities. tion.2 Dry Powder Developer—Dry powder developers can be accomplished using either manual. 8. Drying time shall only be that uniformly sprayed to effectively emulsify the residual pen. number of parts to be processed.5 Spray Application—For spray application following 8.`. (275 kPa). removed from the oven immediately after drying.1 Modes of Application—There are various modes of with an acceptable background and should not exceed 120 s or effective application of the various types of developers such as the maximum time stipulated by the part or material specifi.4. hand powder bulb or a conventional or electrostatic powder (a) The temperature of the water should be relatively gun. 8. Components (a) The concentration of the emulsifier for spray applica.6. Caution: A touch-up rinse may be necessary after immersion. which creates an effective and con- 100°F (10 to 38°C). immersing.. Drying time will vary organization. 8. (b) Bath temperatures should be maintained between 50 Flushing the surface with solvent following the application of and 100°F (10 to 38°C).6. (e) Remove water trapped in cavities using filtered shop air (c) The maximum spray rinse time should not exceed 120 at a nominal pressure of 25 psi (175 kPa) or a suction device s unless otherwise specified by part or materials specification. as evidenced manufacturer.7) and reclean the penetrant on part(s) must be emulsified by immersing the part and reapply the penetrant for the prescribed dwell time. dry (see 8.`. as evidenced by excessive residual surface penetrant --``.6.2 Drying Time Limits—Do not allow parts to remain in (b) Temperature to be maintained at 50 to 100°F (10 to the drying oven any longer than is necessary to dry the surface. Wash time is to be as specified by the part (b) Spray rinse water pressure should not exceed 40 psi or material specification.3.. shall not be placed in the oven with pooled water or pooled tion should be in accordance with the manufacturer’s recom. mendations.6.7 Drying—Drying the surface of the part(s) is necessary quired for adequate surface removal and should not exceed two prior to applying dry or nonaqueous developers or following min. by using wipers of a dry.3. provided the powder is dusted Copyright ASTM International 8 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. semi-automated.. 8.4) or by spraying 8.3.``.3. It is common and effective to apply dry powder in an constant and should be maintained within the range of 50 to enclosed dust chamber. clean. Times over 30 min in the dryer may impair the sensitivity of (c) The spray pressure should be 25 psi (175 kPa) max for the examination. (c) Immersion contact time should be the minimum re. 38°C). Effective post-rinsing of emulsified penetrant from the surface 8. Components shall be etrant on part surfaces to render it water-washable.7.3.`. the residual surface after emulsification and rinsing. Avoid the use of (a) Bath concentration should be as recommended by the excess solvent. and reapply the penetrant for the prescribed dwell time. All part surfaces should be evenly and not exceed 160°F (71°C).```.6. parts are repeating the operation until most traces of penetrant have been completely immersed in the emulsifier bath.. to remove water from pooled areas.8 Spray Post-Rinsing—Following emulsification parts 275 kPa). necessary to adequately dry the part.8. flooding or spraying.6.6. `. the 8.4 Evaluation—Unless otherwise agreed... must be replaced before further use. even film of developer.3 Black Light Warm-Up—Allow the black light to part coverage with a thin. E 165 evenly over the entire surface being examined..3 Aqueous Developers—Aqueous soluble developers Visible ambient light should not exceed 2 ft candles (20 Lx).. even film of developer. Defective bulbs.8.9. The maximum cases where residual penetrant or developer could interfere permitted developing times shall be 4 h for dry powder with subsequent processing or with service requirements. higher intensity levels may be required.9. prepared developer bath. 8. It is good practice to observe the bleedout while may be removed by shaking or tapping the part. NOTE 17—Caution: If parts are left in the bath too long. volatile solvent 8. Adequate closed volume.9.6 to allow for rinse.1 Visible Light Level—Visible penetrant indications in all cases.9 Examination—Perform examination of parts after the produce corrosion. should not be used with Type 2 penetrants or Type 1.9. It is common to immerse the parts in a (UV) filters should be replaced immediately. Aqueous suspendable developers can be used photographic-type visible light meter on the surface being with both Type 1 and Type 2 penetrants. which can obscure discon- voltage fluctuation. indications. NOTE 19—The recommended minimum light intensity in 8. For critical examinations.8. Spray parts in such a manner site of 100 fc (1000 Lx) is recommended. 2 h for aqueous developer and 1 h for nonaqueous particularly important where residual penetrant examination developer.4 Nonaqueous Wet Developers—After the excess pen.`. such as a simple water applicable development time as specified in 8. Since a drop in line voltage can cause decreased black light Then remove parts from the developer bath and allow to drain. indications may leach out. Aqueous developers examined.7.. vapor degreasing. Care should be taken to use only bulbs NOTE 16—Caution: Atomized spraying is not recommended since a certified by the supplier to be suitable for such examination spotty film may result. Immerse parts only long enough to which radiate UV energy.2 Visible Light Examination: developer carrier may be hazardous. A suitable technique.9. such as a process drum or a small storage tank.``. since they may flush or dissolve the penetrant from times may be necessary under some circumstances.. (aqueous and nonaqueous) developer coating is dry (that is. purposes.1 Visible Ambient Light Level—Examine fluorescent penetrant indications under black light in a darkened area. should be applied to the part immediately after the excess 8.9. Cracked or broken ultraviolet or immersing the part.. Reflectors and filters should be checked daily developers may be applied by spraying (see Note 16)..1. interfering debris. NOTE 18—Warning: The vapors from the evaporating. including fluorescent objects. examination. to remain on the part prior to examination should be not less 8.1.2 is 8. solvent bleedout of penetrant from discontinuities into the developer soak. Practice good 8. tinuities. Aqueous required output. The dried Caution: Certain high-intensity black light may emit unac- developer coating appears as a translucent or white coating on ceptable amounts of visible light. require the use of a dryer. as to ensure complete part coverage of the area being examined 8.`. apply developer by spraying in such a manner as to ensure complete 8. etrant has been removed and the surface has been dried.6 Developing Time—The length of time the developer is housekeeping at all times.9.1. it is normal than 10 min. Developing time begins immediately after the practice to interpret and evaluate the discontinuity based on the application of dry powder developer and as soon as the wet size of the indication (see Reference Photographs E 433). coat all of the part surfaces with the developer (see Note 17)..8.`. illumination is required to ensure no loss in the sensitivity of 8. waterspray.`--- penetrant has been removed and prior to drying. or by blowing applying the developer as an aid in interpreting and evaluating with low-pressure 5 psi (34 kPa) dry.```.2. within the discontinuities because of the solvent action of these NOTE 20—Caution: Photochromic lenses shall not be worn during types of developers.1. 08/09/2005 09:01:58 MDT . or ultrasonic cleaning may be employed (see Annex on Copyright ASTM International 9 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. at the examination surface. developers should be prepared and maintained in accordance The black light wavelength shall be in the range of 320 to 380 with the manufacturer’s instructions and applied in such a nm.``.1.. The intensity should be checked weekly to ensure the manner as to ensure complete. which will cause fluorescent the part. the examination.10 Post Cleaning—Post cleaning is necessary in those solvent carrier has evaporated to dryness).3 Housekeeping—Keep the examination area free of with a thin. but especially when the surface to be examined is inside a can be examined in either natural or artificial light. temperature and do not.. 8.4 Visual Adaptation—The examiner should be in the Dipping or flooding parts with nonaqueous developers is darkened area for at least 1 min before examining parts. part coverage. therefore.9.1 Fluorescent Light Examination: NOTE 15—Caution: The air stream intensity should be established experimentally for each application.2 Black Light Level Control—Black lights shall pro- --``. Excess powder coating. 8. machine wash. It is developer. a constant- Drain all excess developer from recesses and trapped sections voltage transformer should be used when there is evidence of to eliminate pooling of developer. clean. Dry the parts in accordance with 8. for cleanliness and integrity.5 Liquid Film Developers—Apply by spraying as rec.8. output with consequent inconsistent performance. indications to disappear. Longer prohibited. even.9. flowing.9. Aqueous vide a minimum of 1000 µW/cm2. intended for general usage.``. materials might combine with other factors in service to 8.-`-`.. Method The measurement should be made with a suitable A penetrants. These types warm up for a minimum of 10 min prior to its use or of developer carrier evaporate very rapidly at normal room measurement of the intensity of the ultraviolet light emitted. A minimum light intensity at the examination ommended by the manufacturer.8.`. Proper ventilation should be provided 8. 8. compressed air. 2). Detergent cleaners may be alkaline. (2) effect saponifying various types of soils.1. the need to restrict impurities such as sulfur. and (4) acidic in nature.1.``. particularly at elevated tempera- tures. Alkali metals in the residue are determined by nondestructive testing. ANSI/ASNT CP-189. CLEANING OF PARTS AND MATERIALS A1. cutting and machining fluids. The residue may also be analyzed by Test used to perform the examination. However. 10.. Manufacturer’s steels.1 Choice of Cleaning Method A1. pen. liquid penetrant testing.`. Keywords phy. Some penetrant supplier agreement. penetrating. (3) practicality of the films.-`-`. Qualification and Requalification embrittlement or corrosion.`. providing it displays the characteristics of the then analyzed in accordance with Test Method D 129..4 Requalification may be required when a change or (for halogens other than fluorine) and Annex A3 on Method for substitution is made in the type of penetrant materials or in the Measuring Total Fluorine Content in Combustible Liquid procedure (see 10. using times or conditions differing from those specified or for 9. and unpigmented drawing cleaning method for the part (for example.. Vapor degreasing can bake the developer on parts.``. The test piece may contain real or simulated analyzed for impurities. --``. Method D 1552. and one method removes all contaminants equally well. Special Requirements examination is performed on parts that must be maintained at elevated temperature during examination. 11. Penetration Materials (for fluorine). it should be carried out as promptly as possible after sulfur and halogens exceeding 1 % of any one suspect element may be examination so that it does not “fix” on the part. An alternative procedure. a large part cannot compounds. recommendations should be observed. nickel-base or other high-temperature alloys. provides a single instrumental technique for rapid sequen. Other materials SNT-TC-1A. E 165 Post Cleaning). Such examination 9. Method B (Turbidimetric nondestructive testing agency as described in Practice E 543 is Method) for sulfur.1 fluorescent liquid penetrant testing.2 Because volatile solvents leave the surface quickly new materials may be performed by any of several methods without reaction under normal examination procedures. These normally evaporate conforming to the applicable edition of recommended Practice quickly and usually do not cause problems. lipophilic emulsification.1 Detergent Cleaning—Detergent cleaners are non- A1. such as grease and oily of the cleaning method on the parts. considered excessive.2 Procedure Qualification—Qualification of procedures elevated temperatures. visible liquid pen- flame photometry or atomic absorption spectrophotometry.. Test discontinuities encountered in product examination.`--- Annex A4 on Determination of Anions by Ion Chromatogra. These impurities may cause 10. A test piece etrant materials are normally subjected to an evaporation containing one or more discontinuities of the smallest relevant procedure to remove the solvents before the materials are size is used. and should be agreed by the contracting parties.2.1 When using penetrant materials on austenitic stainless requires qualification in accordance with 10. The following inspected. the agency shall meet the Method D 808 or Annex A2 on Methods for Measuring Total requirements of Practice E 543.. etrant testing. emulsifying.`. fluoride.1. or Test Method D 129 decomposition fol. this high a level may be unacceptable for some applications. hydrophilic emul- tial measurement of common anions such as chloride. neutral. with the part. all examination personnel shall be materials contain significant amounts of these impurities in the qualified/certified in accordance with a written procedure form of volatile organic solvents.1 The choice of a suitable cleaning method is based on flammable water-soluble compounds containing specially se- such factors as: (1) type of contaminant to be removed since no lected surfactants for wetting. The residue from this procedure is discontinuities. special materials and 9.2 Evaluated-Temperature Examination—Where penetrant 9.. 9.1 Personnel Qualification—When required by user/ the form in which the impurities are present. titanium. Chlorine Content in Combustible Liquid Penetrant Materials 10. The cleaning properties of detergent solutions facili- cleaning methods are recommended: tate complete removal of soils and contamination from the Copyright ASTM International 10 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale..`. sification. solvent removable.. halogens and alkali metals must be considered.1 Impurities: processing techniques may be required.. etc.. water-washable methods ANNEXES (Mandatory Information) A1. so the actual maximum acceptable impurity level must NOTE 21—Caution: Developers should be removed prior to vapor be decided between supplier and user on a case by case basis. 08/09/2005 09:01:58 MDT . degreasing. NAS-410. particularly in the presence of moisture or 10.. or MIL-STD- may contain impurities which are not volatile and may react 410. but must be noncorrosive to the item being specific cleaning requirements of the purchaser.. or be put into a small degreaser or ultrasonic cleaner).``.`.```.1. It is recommended that if developer removal is NOTE 22—Some current standards indicate that impurity levels of necessary. and sulfate. Any such evaluation should also include consideration of 10.1.3 Nondestructive Testing Agency Qualification—If a lowed by Test Method D 516. 11. 1. may decrease the effectiveness of the penetrant examination by ferred method of removing oil or grease-type soils from the smearing or peening over metal surfaces and filling disconti- surface of parts and from open discontinuities. and in Metal-removing processes such as filing.). A1.2 Post Cleaning cleaning efficiency and decrease cleaning time. cleaners that can be effectively utilized to dissolve such soils as A1.3 Vapor Degreasing—Vapor degreasing is a pre. Wet developer coatings can organic solvent if the soil to be removed is organic (grease and be removed effectively by water rinsing or water rinsing with oily films. oz/gal (60 to 120 kg/m3) of water at 180 to 200°F (82 to 93°C). After baking. the part should be baked at a suitable examination process (part temperature at the time of penetrant temperature for an appropriate time to remove the hydrogen before further --``. Because of the short contact time. including abrasives such as glass beads. corrosion products.1. paint.2—Whenever there is a possibility of hydrogen embrittlement of cleaner and thoroughly dried by heat prior to the penetrant as a result of acid solution/etching. waxes and sealants.). produce a desired cosmetic effect on the part. etchants should be used in accordance with the manufacturers’ ing. scraping. thus preparing them to absorb the ambient temperatures. Caution: alkaline solutions are also used for rust removal and descaling NOTE A1. but may not reach to the removing moisture or light organic soil or both.1. A1.1 Removal of Developer—Dry powder developer can used with water and detergent if the soil to be removed is be effectively removed with an air blow-off (free of oil) or it inorganic (rust.`--- processing. These processes A1. Caution: Parts cleaned fluorescence of fluorescent materials. the removal of rust and scale.. paints.. it is surface of the metal. using concen. and with can be removed with water rinsing. In most (15 min minimum). degreasing may not solutions) are routinely used for descaling part surfaces. Acids and chromates can adversely affect the the manufacturers’ recommendations. inorganic soils. rust and flammable and can be toxic. and aluminum. grinding. high-viscosity thickened type for spray or brush application or The actual time required in the vapor degreaser and solvent can be of low viscosity two-layer type for dip-tank application.1—Etched parts and materials must be rinsed completely free to remove oxide scale which can mask surface discontinuities. 125°F (52°C) before applying penetrants. drilling. and in sand. Cleaning time should average 10 to 15 min at 170° are water-soluble powder compounds generally used at 8 to 16 to 200°F (77° to 93°C) with moderate agitation. It will not nuities open to the surface. and a subsequent solvent soak temperature that will not cause degradation of the properties of is recommended.. organic matter. A1. as received.1.6 Paint Removal—Paint films can be effectively A1.1. before application of penetrant.1. corrosion..1. and saponifying various types of soils.`. and degreasing solvent. general. and foundry adhering sands.9 Air Firing of Ceramics—Heating of a ceramic part large.1. Hot recommendations. titanium. then cooled to at least brushing.`.```. completely clean out deep discontinuities and a subsequent Descaling is necessary to remove oxide scale. After paint removal. ings simply dissolve off of the part with a water rinse. welding flux and spatter. After ultrasonic cleaning. reaming. It will remove inorganic soils and many in a clean. general. salts. buffing.1.2. It should be A1. the ceramic should be used.. mechanical milling. soak will depend on the nature of the part and should be Both types of solvent paint removers are generally used at determined experimentally. parts should be detergent either by hand or with a mechanical assist (scrub heated to remove the cleaning fluid.2. washing machine. of etchants.1. by the alkaline cleaning process must be rinsed completely free NOTE A1. E 165 surface and void areas. especially when used as a hand-wipe solvent or as a dip-tank sanding.2 Solvent Cleaning—There are a variety of solvent thoroughly dried.2 Residual penetrant may be removed through solvent removed by bond release solvent paint remover or action. Copyright ASTM International 11 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale.``.. metallic shot.1. Solvent cleaners are not recommended for abrasive blasting. penetrat. (b) Steam cleaning is a modification of the hot-tank alkaline cleaning method.``. Vapor degreasing (10 min minimum). remove all contamination from the void openings and then A1. surface discontinuities and prevent penetrant from entering.5 Ultrasonic Cleaning—This method adds ultra- sonic agitation to solvent or detergent cleaning to improve A1. The maximum bottom of deep discontinuities. etc. The soluble developer coat- 125°F (52°C).). These solvents should be residue-free... and ultrasonic solvent cleaning (3 min cases.). Observe all manufacturers’ scale. Such containing specially selected detergents for wetting. solvent soaking disintegrating-type hot-tank alkaline paint strippers. etc. oxidizing atmosphere is an effective way of organic soils from the surface of parts.`. may not remove resinous soils (plastic coatings. trations (generally 6 to 8 oz/gal or 45 to 60 kg/m3) recom. are often used to remove such soils as carbon.).7 Mechanical Cleaning and Surface Conditioning— grease and oily films. liquid honing. as well as to deburr or instructions and precautionary notes. the surface neutralized and thoroughly dried by heat prior to Alkaline cleaner compounds must be used in accordance with application of penetrants. dirt.1.`. etc. salts..4 Alkaline Cleaning: Acid solutions/etchants are also used routinely to remove (a) Alkaline cleaners are nonflammable water solutions smeared metal that peens over surface discontinuities.8 Acid Etching—Inhibited acid solutions (pickling etc.1.1. ligno-cellulose pellets. aluminum oxide. and beryllium alloy. magnesium. etc. then follow with a solvent soak.. especially for soft metals such as remove inorganic-type soils (dirt. tumble or vibratory deburring. varnish. 08/09/2005 09:01:58 MDT . which can be used for preparation of A1.. the parts must be thoroughly rinsed to mended by the manufacturer of the cleaning compound. which can mask solvent soak is recommended. lathe cutting.`. the part shall be cooled to a temperature below application shall not exceed 125°F (52°C).-`-`. unwieldy parts.. the paint film must be completely removed to expose the minimum) techniques are recommended.``. Caution: Some cleaning solvents are etc. A1.1. Solvent-type paint removers can be of the desirable to vapor degrease..1. In some cases. emulsifying. Hot-tank alkaline strippers penetrant. `. they should be scrubbed out with fine. add it to the sample cup height of 19 mm.5.4.`. It is A2. Chromate A2.5. A2..`. The method is applicable only to materials that are conform to the specifications of the Committee on Analytical totally combustible.1 Reagents and Materials: prescribed hereinafter ensures against explosive rupture of the A2. Dorset. 20 mg of chlorine may cause corrosion of the bomb. platinum. and a 5-mL capacity (Note 1). soaked in hot water for 1 h.``.05 MPa). wide-form with an outside diameter of 29 mm at the top. capable of supplying and National Formulary. 08/09/2005 09:01:58 MDT ..5. 24 mm in outside diameter at sample weight should not exceed 0. Washington. shall be resistant to heat and chemical action. or nickel by means of a dropper at this time (Caution. BDH Ltd. American Chemical Society Specifications. or Cotton Wicking. Copyright ASTM International 12 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale.1 Bomb. 12 mm in content is 2. and shall not holder.1.2 Summary of Methods specifications are available.4 Purity of Reagents amount of these elements will not be reported.3—After repeated use of the bomb for chlorine determination.`. A2. a If white oil will be used (Note A2.1 Reagent grade chemicals shall be used in all tests.3. This dullness should be longer-lasting than platinum..5 g of Na2CO3· 2O) steel plate at least 1⁄2 in.1. bromine or iodine will not be present.1—Fused silica crucibles are much more economical and a film may be noticed on the inner surface. they will be detected and reported as chlorine.``. wet emery cloth. The procedures assume that A2.. top diameter of 28 mm.4 g if the expected chlorine the bottom. 0. liquid or solid.2. alternative titrimetric procedures. The full A2. it is intended that all reagents shall points.3. to Specification D 1193.3).2. Pharmaceutical Convention. 9 Reagent Chemicals. Reagents of the American Chemical Society..2 Procedure: A2. see A2.4.2.`. refined.2 Sample Cup.S.1. METHODS FOR MEASURING TOTAL CHLORINE CONTENT IN COMBUSTIBLE LIQUID PENETRANT MATERIALS A2. (USPC).1 The sample is oxidized by combustion in a bomb vided it is first ascertained that the reagent is of sufficiently containing oxygen under pressure (Caution. U. Use 0. E 165 A2. DC..5.5.2.1. place the sample-filled sample cup in the terminal tion.3. and that section (about 20 mm) and attach the free ends to the terminals. references to water shall determined titrimetrically either against silver nitrate with the be understood to mean referee grade reagent water conforming end point detected potentiometrically (Method A) or coulo.1 Oxygen. where such A2. --``.. After each use. Materials used in the s to distribute the solution over the inside of the bomb.3 Firing Wire.3 White Oil. except when held in closed position by the range of applicability is 0. Place 5 mL of Na2CO3 solution in the bomb (Note of stainless steel or any other material that will not be affected A2. approximately No. If the sample is solid.2 g should be used... Chemicals. then dried and stored in a desiccator before reuse. free of combustible material and halogen bomb. interferes with the procedures. heated to dull red heat over a burner. the bomb.001 to 5 % using either of the operator.5 Decomposition (Method B). and 5-mL capacity.-`-`. protection be provided against unforeseeable contingencies. Use of a sample weight containing over liquid in the bomb.5. so firing wire approximately 100 mm in length. white.2). not more than height outside and weighing 10 to 11 g. or equivalent or 135 g of Na2CO3·10H2O in water and dilute to 1 L.3.2 Sodium Carbonate Solution (50 g Na2CO3/L)— desirable.2 Unless otherwise indicated. (12. provided the bomb is of proper design compounds..1. quantitative recovery of the liquids from the bomb may be Arrange the coil so that it will be above and to one side of the readily achieved. carbonate solution and the amount of chloride present is A2. and construction and in good mechanical condition. U. The high purity to permit its use without lessening the accuracy of chlorine compounds thus liberated are absorbed in a sodium the determination. height. place the cover on the bomb and vigorously shake for 15 by the combustion process or products. see Analar Standards for Laboratory gage.9 Other grades may be used pro- A2.```.. American A2. that the bomb be enclosed in a shield of Dissolve 50 g of anhydrous Na2CO3 or 58. 26 B & S Chemical Society. such as the head gasket and leadwire insula.4).. metrically with the end point detected by current flow increase A2.3 Apparatus A2. Its type that remains open. The inner surface of the bomb may be made sample cup.1. available at a pressure of 40 atm (4. or a blow-out. and the United States Pharmacopeia A2.4 Ignition Circuit (Note A2.1). see Note A2.1 These methods cover the determination of chlorine NOTE A2.1 Safety—Strict adherence to all of the provisions A2.8 g of white oil with solid samples.7 mm) thick.1 Scope and Application without melting the wire. having a capacity of not less than 300 mL.1 Preparation of Bomb and Sample—Cut a piece of A2. opaque fused silica. sufficient current to ignite the nylon thread or cotton wicking MD.. The A2.`--- A2.5 Nylon Sewing Thread.3.2—Caution: The switch in the ignition circuit shall be of a in combustible liquid penetrant materials. Open bomb assembly. causing low or nonexistent end Unless otherwise indicated. however. Coil the middle constructed that it will not leak during the test.5 % or above. NOTE A2. platinum. 15 mm in Note A2. For suggestions on the testing of reagents not listed by the American Chemical Society..6). NOTE A2. 27 mm in outside diameter at the top. Poole.K. Inc.5 and (Kawin capsule form).``. A2. Rockville. If these elements are present. and insert a short length of thread between the firing undergo any reaction that will affect the chlorine content of the wire and the sample. .``. pH measurement type.85) 40 (4.00282 N AgNO3 solution may A2. A satisfactory method for NOTE A2. Add methanol to make the end dips into the sample.6 Analysis. 0. the test on the Wash down the walls of the bomb shell with a fine stream of low-chlorine sample should be repeated and one or both of the low values methanol from a wash bottle.6. making two or A The minimum pressures are specified to provide sufficient oxygen for com. This dilute reagent should not be used with large samples or where chlorine content may be over 0.7910 6 0. Assemble the bomb and tighten 100 mL. chlorine has preceded one low in chlorine content. making If traces of unburned oil or sooty deposits are found. and plot the differential on a chart. Bombs with porous or pitted surfaces should never be used A2.8 g. E 165 removed by periodic polishing of the bomb.5 Blank—Make blank determinations with the amount 300 to 350 38 (3.`.2 Glass Electrode.24) normally require only 0. and clear of white Na2CO3 precipitate). Gage Pressure. be used with the automatic titrator. Close the buret.6..05-mL graduations. Connect the terminals to the open electrical circuit. Admit oxygen (Caution.84) with 2 volumes of in chlorine content should be avoided whenever possible.3 Collection of Chlorine Solution—Remove the been observed in a number of laboratories. Finally. Potentiometric Titration differential is the end point. 08/09/2005 09:01:58 MDT . If titration is manual.2.6. measure the potential difference.1 Silver Billet Electrode.3 and A2.0005 g of the dried NaCl.1 mL of AgNO3 solution from bath. and pour the washings into the thus obtained should be considered suspect if they do not agree within the beaker.04) 32 (3. (Liquid samples 350 to 400 35 (3.) Follow normal procedure. NOTE A2.2. the combined weight of sample and grams of sodium chloride (NaCl) for 2 h at 130 to 150°C. repeatability for the test.6. dropped.``.`. A2.4 Sodium Chloride Solution (0. and dilute to 1 L.2 Addition of Oxygen—Place the sample cup in and outside of the sample crucible into the beaker. Note A2.6.1..1.1 Acetone. Place the electrodes in the solution. uniform rate such that the operation requires and the amount of difference between the present reading and not less than 1 min.2..6.6. cover and terminals into the beaker. start the stirrer (if NOTE A2. Rinse any residue into the beaker.94) require 0.6.2 Reagents and Materials: with soap and water to remove oil or paste left from the polishing A2.6.6.74) 29 (2.```. 25-mL capacity.0282 N)—Dry a few place of white oil.`--- Copyright ASTM International 13 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. Repeatability and sensitivity of the method inside surface with Grit No.6.6. calculate the differential.2.75) 400 to 450 30 (3. gr 1. Open the bomb and examine the contents.55) 37 (3. sp.`. Continue adding 0.4—If the sample is not readily miscible with white oil. rinse the last traces of chlorine from the walls of the bomb and the tendency for residual chlorine to carry over from sample to sample has A2.2. chlorine-free.1. 2/0 or equivalent paper coated with a light are much enhanced by the automatic equipment while much tedious effort machine oil to prevent cutting. a layer of white oil. atm (MPa) to avoid exceeding the 10-mL water dilution limit.6.1 % since A2. chlorine-free combustible diluent may be employed in A2. the last reading.2 Methanol. oxide and water. However. When a sample high in sample cup with clean forceps and place in a 400-mL beaker. it should be washed A2. some other nonvolatile.8 g or larger. add titrant. three test runs to be sure the results are within the limits of plete combustion and the maximum pressures present a safety requirement. Allow a few seconds stirring. dilute to 1 L.. This procedure will remove all but very deep pits and put a high polish on the surface. set the pH meter on the expanded millivolt scale and A2.``.4 Millivolt Meter. Next.6) slowly A2. Subtract the second reading from the first. Remove the bomb from the millivolt reading. and thoroughly clean the bomb before again maximum difference between readings is obtained. Before using the bomb. nonvolatile diluent shall not exceed 1 g. or tilted. 0.. then record the new the circuit to ignite the sample.1.0282 N)—Dissolve Caution: Do not use more than 1 g total of sample and white oil or other 4. A2. Release the Continue the titration.-`-`. mechanical stirrer is to be used)..6—Caution: Do not add oxygen or ignite the sample if the bomb has been jarred. mL minA max A2. A2.1 Gage Pressures 1 % in samples of 0. but may be satisfactorily burned when covered with water.5. Washings position and arrange the nylon thread.7—An automatic titrator is highly recommended in place of doing this is to rotate the bomb in a lathe at about 300 rpm and polish the items A2. chlorine-free.`. The total putting it in use (Note A2..1. Automatic titrators continuously Procedure stir the sample.282 N AgNO3 solution will be required Capacity of Bomb.25 g of white oil while solids 450 to 500 27 (2.3 Buret.2. or wisp of cotton so that should equal but not exceed 100 mL.5—The practice of running alternately samples high and low trated sulfuric acid (H2SO4. making the end point very difficult to detect. 0. or expanded scale pH meter ca- these tests will cause end points of 10 mL or higher. rinse the bomb limits of repeatability of this method. amount of AgNO3 solution required to produce this maximum A2.3). dissolve in relatively insoluble.1-mL increments.5. discard readings and determining differences between readings until a the determination. bath after immersion for at least ten minutes.0005 g of silver nitrate (AgNO3) in water and chlorine-free combustible material. The large amount of pable of measuring 0 to 220 mV. Add 100 mL of acetone.3 Silver Nitrate Solution (0. the cover securely.. It is difficult to water. and begin titration.6480 6 0. water used in such titrations reduces the differential between readings. and then with a paste of grit-free chromic is avoided. rinse both inside A2.`.7 to 0. A2. Some solid additives are weigh out 1. Add exactly 0.1. For chlorine contents over TABLE A2.05) of white oil used but omitting the sample. NOTE A2.4. noting each amount of AgNO3 solution pressure at a slow.1. operation. Method A.4 Determination of Chlorine—Add 5 mL of H2SO4 (to avoid blowing the sample from the cup) until a pressure is (1:2) to acidify the solution (solution should be acid to litmus reached as indicated in Table A2.. A2..6.6.2.3 Combustion—Immerse the bomb in a cold-water note the reading.6. Repeat this blank procedure whenever --``..15 to 0. because of the tendency to retain chlorine from sample to sample.1 Apparatus: The maximum differential is taken as the end point.8—For maximum sensitivity.5 Sulfuric Acid (1 + 2)—Mix 1 volume of concen- NOTE A2. A2.7.545 mL of gelatin solution and 5. (A typical mixture is 2.7. whichever wash bottle.4 Mix enough gelatin solution and of acetic acid- sample as follows: nitric acid mixture for one titration.7.2.7.7. two.7.2 Reproducibility—Results by different laborato.006 % or 10. A2. and hot water to liquefy the gelatin.6.1 g of thymol blue. A2.7..1.7. Calculate the normality approximately 1 L of hot distilled or deionized water to the 6.2) mixture. ries should not be considered suspect unless they differ by Wash down the sides of the bomb shell with water. acetone.8.1 Apparatus: acid mixture.1 Repeatability—Results by the same analyst A2. A B A2..013 % or 21. This is done by titration of a known A2.8.6.`.8. Gently heat with continuous mixing 5. and according to the operating manual of the titrator.6.4.2.7. A2. dissolve in water. Dry a A2. Coulometric Titration A2. the is 86 % to 89 % of the actual amount present. Weigh out 5. rinse the under side. This modified process eliminates the interference and does not alter the quality of the titration. and that introduced by contamination. Copyright ASTM International 14 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale.3 Empty the bomb shell into the 100-mL beaker.7 Analysis. crystal.10—The solution may be premixed in a larger quantity for where: convenience.7. but do not NNaCl = normality of the NaCl solution. erably with 11⁄2 in.2.) Keep the remainder in a refrigerator.1 g and record the weight of the acceptability of results: the 100-mL beaker. or gelatin mix-acetic acid-nitric A2. 08/09/2005 09:01:58 MDT .0 mL of 0. Prepare and titrate a similar mixture of all the chemicals except the NaCl solution.6 Standardization—Silver nitrate solutions are not quantity of NaCl for 2 h at 130 to 150°C. Method B. sample.0 3 NNaCl NAgNO3 5 V 2 V (A2.4.. A2.2.3. cal ratio is 12. so the true activity should be checked 0. A2.3 Glacial Acetic Acid-Nitric Acid Solution—A typi- titration of the reagents only. Glacial.5 ~VS 2 VB! 3 N 3 3. When ready to use. platinum wire.```.4 Titration: A2.. weight % 5 W (A2.3.1 Acetic Acid. but may not be useable after 24 h.5 parts CH3COOH to 1 part HNO3). --``.5 % of the value determined.``.1 Gelatin Solution—A typical preparation is: Add thus obtaining a reagent blank reading..1 Coulometric Chloride Titrator. A2. VB = millilitres of AgNO3 solution used by the blank. 0.-`-`.7.1 The following criteria should be used for judging A2. 10 the blank run is to measure the chlorine in the white oil.5 to 1 (12.. whichever is bottle.1) until the gelatin is completely dissolved. and.`.0282-N the bomb. using a more than 0.1.8 Precision and Accuracy: mineral oil.7. and changed. and. immerse the day’s aliquot in titration including the NaCl solution.6.-outside diameter bottom). 10 May be purchased from the equipment supplier. E 165 new batches of reagents or white oil are used.. the A2. A2.9—The normal reagent preparation process has been slightly the chemicals (Na2CO3 solution. using a wash than 0. VB = millilitres of AgNO3 solution used for the A2.1.2 Reagents: 6 g of gelatin powder.1 Weigh to the nearest 0. H2SO4 solution.4.6.0005 g of dried NaCl in a closed container.3. due to the interference from the 50 mL of water required to wash methanol) specified for the test. A2. The purpose of A2. (Thirty millilitres is enough for approximately eleven NAgNO3 = normality of the AgNO3 solution.7.5 Add specified amounts of gelatin mixture and acetic acid-nitric acid mixture. freeze.3 Refrigerator. when the solution is first made up and then periodically during and dilute to 1 L.4.2 Beakers.1 g of thymol. 100-mL. A2.`. The total amount of washings should be 50 6 1 g. 100-mL beaker.`. Determine W = grams of sample used.2 of the AgNO3 solution as follows: g of dry gelatin mixture contained in one vial supplied by the equipment manufacturer.`--- VS = millilitres of AgNO3 solution used by the sample. is higher.7.``.8.4 Sodium Chloride Solution—100 meq C/1. using the wash bottle. if this was premixed.3 % of the value detected. titrations.3 Nitric Acid.3 Accuracy—The average recovery of the method bly support.. contains the 50 g of washings including the decomposed A2.3.6... and the terminals into the same 100-mL beaker.5 Run at least three blank values and take an average N = normality of the AgNO3 solution.2 Divide into aliquots each sufficient for one day’s where: analyses.`. into the 100-mL beaker that A2. reagent grade.4. NaCl solution and titrate to the end point.7. water-soluble. A typical mixture consists of A2.2 Remove the sample crucible from the cover as- should not be considered suspect unless they differ by more sembly support ring using a clean forceps. and 0..7.7 Calculation—Calculate the chlorine content of the A2.) NOTE A2. or glazed crucibles (pref.1. the life of the solution.8440 6 permanently stable..3 Reagent Preparation: NaCl solution as follows: Prepare a mixture of the amounts of NOTE A2.7.3. Pipet in 5.7. The solution will keep for about 6 months in the VA = millilitres of AgNO3 solution used for the refrigerator.1. A2.7.1. A2.6.4 Remove the cover assembly from the cover assem- A2.7. rinse both the inside and the outside with water into the higher.``.2 Dry Gelatin Mixture.4 mL of acetic-nitric acid Chlorine.7. reagents. separate blanks for both 5 drops of mineral oil and 20 drops of A2. The inner surface of the bomb may be made be used in all tests.11 Fluoride Specific Ion Electrode and suitable refer- they are present in sufficient concentration to exceed the ence electrode.6. A3.2 Summary of Method and weighing 10 to 11 g. metals forming precipitates with fluoride ion will interfere if A3. 08/09/2005 09:01:58 MDT .1 Safety—Strict adherence to all of the provisions type that remains open.. 26 B & S containing oxygen under pressure (Caution. provided the bomb is of proper design A3. polypropylene (Note A3.`. solubility of their respective fluorides.4. desirable. according to A2. weight % 5 W (A2. E 165 A2. This is dependent on the 0.2—Glassware should never be used to handle a fluoride solution as it will remove fluoride ions from solution or on subsequent use A3.1 Scope and Application by the combustion process or products.2. polypropylene.1 mV. expected to exhibit the following relative standard deviations: tion in the sample as follows: Approximate % Chlorine RSD. 0. that do tion.12 Millivolt Meter capable of measuring to 0. polypropylene.10 Magnetic Stirrer and TFE-coated magnetic stirring A3. If iodine is present.2). 12 mm in height.2). however.1.4. and that A3..4.7.3 If bromine is present.4. A2. 20. Fluorine will not be detected.4.1.4. aluminum.``. NOTE A3.. bomb. 27 mm in outside diameter at the top.`--- Copyright ASTM International 15 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale.2 The method can be expected to report values that B = average counter reading obtained with average of the vary from the true value by the following amounts: three blank readings. in height..2.1 Bomb.4.8 Beaker.0 and above 0.7. and shall not not contain appreciable amounts of interfering elements. 24 mm in outside diameter at the bottom. white. It is A3. 150-mL (Note A3.3. A3.5 0. combustion will entrain fluorine even if otherwise soluble.6 Precision and Accuracy: operating manual procedure.```.1 % chlorine and above 62% M = standardization constant.1 Duplicate results by the same operator can be A2.1—Caution: The switch in the ignition circuit shall be of a A3. or undergo any reaction that will affect the fluorine content of the have any insoluble residue after combustion.`.`. A3. instrument range setting in use and the reading obtained with a known amount of the 100 meq of Cl A2. (12.`. A3. sufficient current to ignite the nylon thread or cotton wicking mined potentiometrically through the use of a fluoride selective without melting the wire.003 5.6.7.4. platinum. such as the head gasket and leadwire insula- combustible liquid penetrant materials.4 Ignition Circuit (Note A3.. Its range of liquid in the bomb....1 Purity of Reagents—Reagent grade chemicals shall readily achieved.1). A3.4. % ~P 2 B! 3 M Chlorine.3 Firing Wire. so constructed that it will not leak during the test. 28 mm in outside diameter at the top.7 Volumetric Flask. METHOD FOR MEASURING TOTAL FLUORINE CONTENT IN COMBUSTIBLE LIQUID PENETRANT MATERIALS A3.9 Pipet. approximately No. calcium.2). see A3.``. it is intended of stainless steel or any other material that will not be affected that all reagents shall conform to the specifications of the --``.6 Titrate using a coulometric titrimeter.9 where: P = counter reading obtained with the sample. nickel. A3. 36. or equivalent A3. NOTE A3. ion electrode. A3.6 Funnel.5. 20 mm in outside diameter at A3. magnesium. and construction and in good mechanical condition.3) 1. except when held in closed position by the prescribed hereinafter ensures against explosive rupture of the operator. or a blow-out.1.1).2 Sample Cup. 100-mL (Note steel plate at least 1⁄2 in.5 Calculations—Calculate the chloride ion concentra.5 Nylon Sewing Thread.2 The measure of the fluorine content employs the the bottom. A2.`.01 % chlorine 69%. or platinum. will be reported. capable of supplying citrate solution and the amount of fluorine present is deter. Materials used in the A3. Eppendorf-type (Note A3. protection be provided against unforeseeable contingencies.7. The gage.1 Silicon.4 Apparatus carry fluoride ion from a concentrated solution to one more dilute. and other bar. Unless otherwise indicated. Insoluble residue after A3.1.2).. and 16 mm fluoride selective ion electrode..2.4. that the bomb be enclosed in a shield of A3.1 This method covers the determination of fluorine in bomb assembly. fluorine compounds thus liberated are absorbed in a sodium A3.10 0.``. applicability is 1 to 200 000 ppm.6.7.5 % of the true amount per litre of solution.. shall be resistant to heat and chemical action. g.5 Reagents quantitative recovery of the liquids from the bomb may be A3. having a capacity of not less than 300 mL..7.7 mm) thick.001 to 0.-`-`.3 Interferences A3. and will be reported.7 % of the true amount W = weight of sample used.1 2. 100-µL.1 The sample is oxidized by combustion in a bomb A3.4. liquid or solid. A3.4. or Cotton Wicking.4. 05 MPa).5. 32.1 0.9 Other grades Gage Pressure atm (MPa) Capacity of Bomb..6 Sodium Hydroxide Solution (5 N)—Dissolve 200 g determination.5.15 g of sodium chloride.1 Repeatability—The results of two determinations by --``.6.4 Add 100 µL of stock fluoride solution and obtain the reading after the same length of time necessary for A3. concentration) of the electrode as described by the manufac- Arrange the coil so that it will be above and to one side of the turer..1 Gage Pressures Society.1 Calculate the fluorine content of the sample as Chlorine Sample White Oil follows: Content.. Release the pressure compounds. If traces citrate dihydrate in water and dilute to 1 L..5.6. or wisp of cotton so that the 100 µL of the stock fluoride solution..) oil at this time to ensure ignition of the sample.2 0..6. then A3.4 Fluorine.4) slowly (to and avoid blowing the sample from the cup) until a pressure is W = grams of sample. A3.5 Sodium Citrate Solution—Dissolve 27 g of sodium than 1 min. and insert a short length of thread between the firing condition of the electrode determines the length of time wire and the sample.6. A3. and thoroughly clean the bomb before again of sodium hydroxide (NaOH) pellets in water and dilute to 1 L. putting it in use. Finally. available at a pressure of 40 atm (4. plete combustion and the maximum pressures present a safety requirement. Rinse the walls of the bomb of glacial acetic acid. and shell with a fine stream of wash solution from a wash bottle. Open A3.9 Precision and Bias bomb has been jarred. g 0. Remove the bomb from the A3. Admit oxygen (Caution. uniform rate such that the operation requires not less A3.7. solution to bring the contents of the flask to the line. A3. 350 to 400 35 37 A3. discard the A3. add 32 mL into a 100-mL volumetric flask. cover securely.``. and terminals into the volumetric flask. NOTE A3.1. refined. NOTE A3. provided it is first ascertained that the reagent is minA max of sufficiently high purity to permit its use without lessening 300 to 350 38 40 the accuracy of the determination.-`-`.1) 20 to 50 0. of unburned oil or sooty deposits are found. 15 s to distribute the solution over the inside of the bomb.. Cool and dilute to 1 L. rinse the bomb cover pH to 5. or tilted.7.`--- Copyright ASTM International 16 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale.0005 g of predried (at 130 to 150°C for 1 h.42006 0. Place 10 mL of sodium citrate solution in the A3.3 Immerse the fluoride and reference electrodes in the bomb.``..7 Procedure A3. Note A3.6 g of sodium citrate dihydrate.5.1.2 Purity of Water—Unless otherwise indicated.6 Decomposition Procedure A3.`. place the sample-filled sample cup in the terminal solutions and obtain the equilibrium reading to 0. Close dilute to 1 L.. 6.4—Caution: Do not add oxygen or ignite the sample if the A3.``.7 (A3.```.2 Addition of Oxygen—Place the sample cup in posi- D E2 = millivolt change in blank solution on addition of tion and arrange the nylon thread. end dips into the sample. A3.`.5.3. the sample weight be based on the following table: A3.6 W 10 to 20 0. A3.4 Oxygen.. Next.8. and vigorously shake for without a sample.5. A3. To avoid this it is recommended that for A3. (The holder. place the cover on the bomb.1 mV.7 Caution: Do not use more than 1 g total of sample and white where: D E1 = millivolt change in sample solution on addition of oil or other fluorine-free combustible material.7. Stir to dissolve and then adjust the and add the washings to the flask. Total Ionic Strength sample cup with clean forceps and rinse with wash solution Adjustment Buffer)—To 300 mL of distilled water.7. This may be as little as 5 min exceed 1 g. Connect the terminals to the open electrical circuit..9. ppm 5 2 3 1024 F 10DE1/S 2 1 2 2 3 1024 10DE2/S 2 1 G 3 106 5 to 10 0.3 Combustion—Immerse the bomb in a cold-water cooled in a desiccator) sodium fluoride in distilled water and bath.3 using 5 N NaOH solution. The sample weight used should not necessary to reach equilibrium. reached as indicated in Table A3. mL may be used.7 Wash Solution (Modified TISAB. sample cup.3 Fluoride Solution.4 weight.7. store in a polyethylene container.. add a few drops of white or as much as 20 min. Assemble the bomb and tighten the S = slope of fluoride electrode as determined in A3. 100 µL of stock fluoride solution. the circuit to ignite the sample.2 Obtain a blank solution by performing the procedure bomb.3—Use of sample weights containing over 20 mg of chlorine may cause corrosion of the bomb.1 Preparation of Bomb and Sample—Cut a piece of firing wire approximately 100 mm in length.8 Calculation samples containing over 2 % chlorine. dropped.05 0. all 400 to 450 30 32 450 to 500 27 29 references to water shall be understood to mean Type I reagent A The minimum pressures are specified to provide sufficient oxygen for com- water conforming to Specification D 1193.`.4 Collection of Fluorine Solution—Remove the A3.`. g 0.`. at a slow.1 Ascertain the slope (millivolts per ten-fold change in section (about 20 mm) and attach the free ends to the terminals. 08/09/2005 09:01:58 MDT . add wash A3. free of combustible material and halogen bath after immersion for at least 10 min. Coil the middle A3. Open the bomb and examine the contents. If the sample is a solid.7. % 2 to 5 weight. Stock (2000 ppm)—Dissolve 4.5.8 White Oil. where such specifications are available. E 165 Committee on Analytical Reagents of the American Chemical TABLE A3. to protect separator column from fouling by a 100-µL sample loop and a 10-µmho full-scale setting on the particulates or organics. PO43−.00011 %) or 8. and SO42− with 4 3 50 mm. height.. and a strip chart recorder capable of full-scale additions. conductivity detector. amount detected.7 ppm or 129. NO3−. a dilution overcomes many interferences. guard.`.1 Scope and Application a higher scale setting and an electronic integrator. and weighing 10 to 11 g. 27 mm in outside diameter at the top.1 The material must be put in the form of an aqueous bomb assembly.`--- A4.1).2—Caution: The switch in the ignition circuit shall be of a type that remains open. The anions of interest are separated (Kawin capsule form). they should be scrubbed out exchanger (suppressor column) where they are converted to with fine. or nickel series of ion exchangers. detectable concentrations are in the range of 0. The ion chromatograph shall be capable of delivering Because small sample volumes are used. Cl−.`. a similar fashion.3. and a 5-mL capacity (Note A4.5 Nylon Sewing Thread. The inner surface of the bomb may be made of stainless steel or any other material that will not be affected A4.1.. To resolve uncertain.4 Ignition Circuit (Note A4. optional. An electronic peak integrator is reagent water. glassware.``.. divinylbenzene-based low-capacity pellicular anion-exchange mum detectable concentration of an anion is a function of resin capable of resolving Br−.. NO2−. fluoride. A high concentration of any one A4. whichever is greater.8 Guard Column. relatively high concentrations of low- molecular-weight organic acids interfere with the determina.3.2 Reproducibility—The results of two determinations 64 % of the amount actually present although 83 to 85 % by different laboratories should not be considered suspect recoveries can be expected with proper technique.1 Bomb. The sample is tion. 4 3 250 mm. top diameter of 28 mm.3. 24 mm in outside diameter at washed from the bomb.2. conductivity... readily achieved.9. For example.`. NO2−. Similar values may be achieved by using A4. and 5-mL capacity. The separated anions in their acid form are measured by S gage. --``. heated to dull red heat over a burner. DETERMINATION OF ANIONS BY ION CHROMATOGRAPHY WITH CONDUCTIVITY MEASUREMENT A4. white.``. and that ment of common anions such as bromide. They are identified on the basis of retention time A4. and shall not oxidized by combustion in a bomb containing oxygen under undergo any reaction that will affect the chlorine content of the pressure.3. minimum and SO42−. Spurious peaks may result from contaminants in response of 2 s or less. After each use.9. 26 B and acid. separator. sequential measure.1. quantitative recovery of the liquids from the bomb may be nitrate.2 Summary of Method by the combustion process or products.3 Apparatus detrimental substances in organic based materials. having a capacity of not less than 300 mL.1—Fused silica crucibles are much more economical and The separated anions are directed onto a strongly acidic cation longer lasting than platinum.3. 15 mm in on the basis of their relative affinities for a low capacity. a stream of carbonate-bicarbonate eluant and passed through a height of 19 mm.3. a ion also interferes with the resolution of others. or Cotton Wicking. The products liberated are absorbed in the eluant liquid in the bomb. contamination. soaked their highly conductive acid form and the carbonate. Quantitation is by measurement of sufficient current to ignite the nylon thread or cotton wicking peak area or peak height. chloride. present in the bomb at the time of ignition.3. Blanks are prepared and analyzed in without melting the wire. capable of supplying as compared to standards. constructed that it will not leak during the test. It provides a A4. height outside..2). opaque fused silica. including an injection valve. NO3−. 08/09/2005 09:01:58 MDT . A4.3 Minimum Detectable Concentration—The mini. filtered. tion of chloride and fluoride. scrupulously avoid 2 to 5 mL eluant/min at a pressure of 1400 to 6900 kPa.3 Firing Wire. A4. A3. sample size and conductivity scale used. phosphate. NOTE A4. high-capacity cation-exchange Copyright ASTM International 17 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. A4.``. bicarbonate eluant is converted to weakly conductive carbonic A4. strongly basic anion exchanger (guard and separator column). with styrene A4. F−. shall be resistant to heat and chemical action. platinum.9 Suppressor Column..0 % of the detected. Sample sample loop.0 % of the amount differ by more than 1. such as the head gasket and leadwire insula- solution before analysis can be attempted.05 mg/L for F− A4.1 mg/L for Br−. platinum.`. wet emery cloth.1 ppm (0. or sample processing apparatus.3.2 Interferences—Any substance that has a retention NOTE A4. E 165 the same analyst should not be considered suspect unless they unless they differ by 6..-`-`. A4. interfere. 12 mm in volume. and sulfate. temperature-compensated small-volume conductivity cell (6 ties of identification or quantitation use the method of known µL or less). Materials used in the A4.2..2.. nitrite.```.3. and suppressor columns.1 This method is condensed from ASTM procedures and APHA Method 429 and optimized for the analysis of A4.7 Anion Separator Column. so single instrumental technique for rapid.6 Ion Chromatograph. Generally. and diluted to a known the bottom. whichever is greater. This solution is A4.1 A filtered aliquot of sample is injected into a wide-form with an outside diameter of 29 mm at the top. in hot water for 1 h then dried and stored in a desiccator before reuse. identical to separator column except and 0..2.3 Bias—The average recovery of the method is 62 to A3. Cl−.`.2 Sample Cup. except when held in closed position by the time coinciding with that of any anion to be determined will operator. A4. approximately No. PO43−. H2SO4. the flask. place the sample-filled sample cup in the terminal be used in all tests. and 100 mg wash bottle.4—Caution: Do not add oxygen or ignite the sample if the stable for at least one month. If traces PO43− KH2PO4 1. Remove the bomb from the F− NaF 2. NO2−. % weight.. tion and arrange the nylon thread.6 NaHCO3 and 1. or tilted. fluorine-free combustible material. and (IC) analysis. Unless otherwise indicated..1 Preparation of Bomb and Sample—Cut a piece of plete combustion and the maximum pressures present a safety requirement. or wisp of cotton so that the sor system.9 Alternative Combined Working Standard Gage Pressures. where such specifications are available. Range—Dilute 100 mL combined working standard solution.3 Combustion—Immerse the bomb in a cold-water g/L bath.10 Syringe.0024M Na2CO3: dissolve 1.7 A4. 08/09/2005 09:01:58 MDT . mL.5.4. Low washings through the filter into the volumetric flask. add a few drops of white Society. Finally. mL mmA max ion concentration to be determined.``. bomb has been jarred.3707 at a slow.`. free from interferences following: at the minimum detection limit of each constituent and filtered Chlorine Sample White Oil through a 0.4330 of unburned oil or sooty deposits are found..-`-`. A4. minimum capacity of 2 mL and equipped Arrange the coil so that it will be above and to one side of the with a male pressure fitting. 0. Prepare fresh daily. 0.5 Decomposition Procedure A The minimum pressures are specified to provide sufficient oxygen for com- A4. Release the pressure Br− NaBr 1.4 0. add deionized water to bring the contents of the flask to the high range.4 Regenerant Solution 1. Range—Combine 10 mL of the Cl−.5 Regenerant Solution 2.4 Reagents 15 s to distribute the solution over the inside of the bomb.2 0. 400 to 450 30 32 450 to 500 27 29 A4. Anion Salt Amount. and store in washings into a 100-mL volumetric flask.3—Use of sample weights containing over 20 mg of chlorine sufficiently high purity to permit its use without lessening the may cause corrosion of the bomb.5. content..4. and add the washings through the filter paper to SO42−/L.8 mL conc H2SO4 to 4 L or 100 mL regenerant solution 1 to 4 L.8 Combined Working Standard Solution.2 Addition of Oxygen—Place the sample cup in posi- Use this regenerant with continuous regeneration fiber suppres. and 100 mL with clean forceps and rinse with deionized water and filter the of the SO42− standard solutions.2876 NO3− NaNO3 1. discard the SO42− K2SO4 1.. Open the bomb and examine the contents..``. F−. dilute to 1000 mL. contains 10 mg/L each of the bomb shell with a fine stream of deionized water from a Cl−.4 Collection of Solution—Remove the sample cup PO43− standard anion solutions. NO3−. E 165 resin capable of converting eluant and separated anions to their firing wire approximately 100 mm in length.. 0. To avoid this it is recommended that for accuracy of the determination. Rinse the walls of a plastic bottle protected from light.2-µm membrane filter to avoid plugging columns. Coil the middle acid forms.4. PO43−. Prepare fresh daily. Capacity of Bomb. A4.`--- Committee on Analytical Reagents of the American Chemical exceed 1 g.4. The sample weight used should not --``. NO2−. these solutions are NOTE A4. A4.1 mg Br−/L. it is intended holder. atm Solutions—Prepare appropriate combinations according to an. and thoroughly clean the bomb before again A4.5. F−.8141 determination.3 Eluant Solution. 1000 mg/L.2 Deionized or Distilled Water.. If NO2− and PO43− are not included. NO3−. Note A4.003M NaHCO3− 0. samples containing over 2 % chlorine. 10 to 20 0.`. Connect the terminals to the open electrical circuit.4. rinse the bomb cover and terminals and add the A4. Admit oxygen (Caution.05 0. If the sample is a solid. dilute 2.4998 than 1 min..4. H2SO4. contains 1. and PO43−.1 0. TABLE A4. Open A4. F−. Use aliquots of this solution for the ion chromatography from light.9 Other grades oil at this time to ensure ignition of the sample. g weight. NO2−. NO3−.0176 g Na2CO3 in water and dilute to 4 L.4 bonate. 1 mg Br−/L. 1 N.1. dried to a constant weight at 105°C. Place 5 mL of Na2CO3/NaHCO3 solution in the bomb.4. the sample weight be based on the A4.`.4. end dips into the sample.2100 bath after immersion for at least 10 min.7 Combined Working Standard Solution.`. Copyright ASTM International 18 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale.3.4.7 CAUTION: Do not use more than 1 g total of sample and white oil or other erant when suppressor is not a continuously regenerated one. the combined working standard is stable for one 300 to 350 38 40 350 to 400 35 37 month. Store in plastic bottles in a refrigerator.025 N. uniform rate such that the operation requires not less NO2− NaNO2 1. and vigorously shake for A4. A4. sample cup. and A4. may be used provided it is first ascertained that the reagent has NOTE A4. g A4.1 Gage Pressures A4.```..`.4) slowly (to series of standard anion solutions by weighing the indicated avoid blowing the sample from the cup) until a pressure is amount of salt.6 Standard Anion Solutions. to 1000 reached as indicated in Table A4.1 Purity of Reagents—Reagent grade chemicals shall the bomb. section (about 20 mm) and attach the free ends to the terminals. High putting it in use.008 g 5 to 10 0. Close Cl− NaCl 1.0 mg/L each Cl−. sodium bicarbonate-sodium car- 2 to 5 0.``. and insert a short length of thread between the firing that all reagents shall conform to the specifications of the wire and the sample. Assemble the bomb and tighten the A4. use this regen.. prepare a cover securely. and 10 mg SO42−/L. to 1000 mL and store in a plastic bottle protected line. dropped. place the cover on the bomb. 20 to 50 0..5. Next. 1 mL of the Br−.6485 the circuit to ignite the sample. .7 43.2 Calibration—Inject standards containing a single returned to base line.03 Yes.1 mL sample loop inject at least 1 mL..03 No NO3− 15. After the the manufacturer’s instructions..49 0. and adjust eluant flow rate to approximate the separation A4.1 Typical Anion Profile --``.`. With a when the response is shown to be linear.1 If linearity is established for a given detector TABLE A4..05 0.15 0.86 0.16 0.6.. Br−. mg/L Found.15 0.03 No SO42− 43. Bias 95 % Added.46 No Cl 0.38 0.``. Single- Overall Significant Amount Amount Operator Anion Precision. retention always is in the turer’s instructions when the conductivity base line exceeds order F−.82 0..5 2.. 08/09/2005 09:01:58 MDT . by height or area against concentration on linear graph paper. chromatograph from load to inject mode and record peak A4. Adjust detector to necessary. Adjust detector offset to zero-out standard.9 No SO42− 0.5 to 3 mL/min.1 Set up the ion chromatograph in accordance with heights and retention times on strip chart recorder.64 0.`.4) may shift slightly during suppressor exhaustion and with C = mg anion/L.1 System Equilibration—Turn on ion chromatograph calculation of the calibration factor.4 1.1 Samples of reagent water to which were added the common anions were analyzed in 15 laboratories with the NOTE A4.6.52 0. Inject at 300 µmho when the suppressor column is on line. PO43−. Switch ion eration flow rate to maintain stability.2. If sample adjustments are made.7. a fast run column this may lead to slight interference for F− or H = peak height or area.6 No PO43− 0. A4.52 0. Cl−.. Alternatively.2.17 Yes.43 No Cl 455 471 46 13 No NO2 0. Inject enough sample to flush sample loop several eluant conductivity.84 4. last peak (SO42−) has appeared and the conductivity signal has A4. neg Br− 0.2 Precision and Accuracy Observed for Anions at Various Concentration Levels in Reagent Water setting. Using a prewashed syringe of 1 to 10 mL equilibrium (15 to 20 min).6.48 0.45 0. make this determination only when the suppressor is at the same C5H3F3D (A4. Recalibrate whenever the detector setting is changed.18 0. and diluting the sample with eluant or by adding concentrated D = dilution factor for those samples requiring dilution.. A stable base line indicates capacity equipped with a male luer fitting inject sample or equilibrium conditions.50 0.07 0.1.6.04 0. least three different concentrations for each anion to be A4. it is acceptable to calibrate with a single standard.8 Precision and Bias tration as in the eluant.8 1. A4.`. A4.`. E 165 A4.34 0. with the fiber suppressor adjust the regen. Cl−. referring to the appropriate calibration curve.0 0. neg PO43− 0.2 0.7 Calculation measured and construct a calibration curve by plotting peak A4. if achieved in Fig. A4.``.49 0.76 0.5 2.-`-`.9 1. by filtering through a prewashed 0.6.9 1.09 0.03 No F− 4. In this type of system the water dip (see NoteNote where: A4. To eliminate this interference.25 0.25 0.8.11 No Cl− 17 17. neg NO2 21. mg/L Precision. another sample can be injected.51 0.09 0.3 Yes.``.1 (2 to 3 mL/min). eluant to the sample to give the same HCO3−/CO32− concen- A4. mg/L Level mg/L F− 0.33 0.2 No FIG.04 Yes. NO3−.4 Regeneration—For systems without fiber suppressor Observed times vary with conditions but if standard eluant and regenerate with 1 N H2SO4 in accordance with the manufac- anion separator column are used.7 12.`--- Copyright ASTM International 19 Reproduced by IHS under license with ASTM Licensee=YPF/5915794100 No reproduction or networking permitted without license from IHS Not for Resale. in mg/L.. neg NO3− 0.2-µm-pore-diam desired setting (usually 10 µmho) and let system come to membrane filter. A4. adjust standards and blanks identically. usually 2..06 0. NO2− interaction equation: with the suppressor may lead to erroneous NO2− results.`. and SO42−. NO2−.3 Sample Analysis—Remove sample particulates.5—Water dip occurs because water conductivity in sample is results shown in Table A4..6. F. use the following system requiring suppressor regeneration. anion or a mixture and determine approximate retention times. less than eluant conductivity (eluant is diluted by water).1) stage of exhaustion as during standardization or recalibrate frequently.1 Calculate concentration of each anion. times: for 0.```.10 0.8 19.6 Procedure Record the peak height or area and retention time to permit A4. analyze standards that F = response factor − concentration of standard/height (or bracket the expected result or eliminate the water dip by area) of standard.1 14.02 No Br− 13. ..-`-`..``.. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised.. 610-832-9555 (fax). at the address shown below... E 165 ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard. and the risk of infringement of such rights.`.. 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