Designation: A 967 - 05"* Standard Specific: Chemical Passivation Treatments for Stainless Steel Parts‘ ‘Ti stander eed war th co design A 967; heme mec elowng the designation ates Be year of trig adoption ein the cate of vison, he ya flat evion. Ammer m pacers incase year fat eppreval A ‘spencrint epsilon) internets chan Sc the as even a espa, Tits senda hs born eproved fru by gents of he Department of Defense © Nowe Section 6.1.1.1 was editorially comecte in July 2007, 1. Scope* 1.1 This specification covers several different types of chemical passivation treatments for stainless steel parts. It includes recommendations and precautions for descaling, cleaning, and passivation of stainless steel parts. It includes several alternative test, with acceptance criteria, for confirma tion of effectiveness of such treatments for stainless stl parts 1.2 Practices for the mechanical and chemical treatments of siainless stee! surfaces are discussed more thoroughly in Practice A 380, 1.3 Several alternative chemical treatments are defined for passivation of stainless steel parts. Appendix XI gives some ronmandatory information and provides some general guide- lines regarding the sclection of passivation treatment appropri- ate to particular grades of stainless stel. It makes no recom: ‘mendations regarding the suitability of any grade, treatment, or acceptance criteria for any particular application or class of applications, 14 The tests in this specification ae intended to confirm the ‘effectiveness of passivation, particularly with regard to the removal of free iron and other exogenous matter. These tests include the following practices: 14.1 Practice A—Weter Immersion Test, 14.2 Practice B—High Humidity Test, 143 Practice C—Sakt Spray Test, 144 Practice D—Copper Sulfate Test, 14.5 Practice E—Potassium Ferricyanide-Nitric Acid Test, and 1,46 Practice FFree Iron Test. 15 The values stated in inch-pound units are to be regarded as the standard. The ST units given in parentheses are for information only. 16 The following precautionary caveat pertains only to the test method portions, Sections 14 through 18 of this specifica- tion: This standard does not purpors to address all of the safery "hi pecicnon tude he jain of ASTI Connie AU 08 Sel Sines Stel aed Rend Aye ad i a iret exons of Suboomaes ‘ol. eon Setods of Contsen Testing. ‘Cue dion eppoved Sept 1, 205, Poblihed September 200, Originally approved ia 1956 Ls previous eden approved in 2001 at A867 =O" concers, if any, associated with its use. It is the responsiblity of the user ofthis standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2, Referenced Documents 2.1 ASTM Standards: * 'X 380 Practice for Cleaning, Descaling, and Depassivation ‘of Stainless Steel Pats, Equipment, and Systems BB 117 Practice for Operating Salt Spray (Fog) Apporatos 254 Practice for Preparation of and Electroplating. on Stainless Stel 22. Federal Specification? QOP-35C Passivation Treatments for Comosion-Resistant Steels 3. Terminology 3.1 Defnition of Term Specific to This Standard —It is necessary to define which of the several commonly used efinitions of the term passivation will be used in this specification, (See Discussion.) 3.1.1 Discussion—Stainless steels aro autopassivating inthe sense thatthe protective passive film is formed spontaneously fon exposure to air or moisture. The presence of exogenous surface contamination, including dirt, erease, free iron from contact with steel tooling, and so forth, may interfere with the formation of the passive film, The cleaning of these contami nants from the stainless stee! surface will facilitate the spon- tancous passivation by allowing the oxygen uniform access to the surface. The passive film may be augmented by chemical treatments that provide an oxidizing environment for the stainless stee] surface. 3.1.1.1 In this specification, passivation, unless otherwise specified, is defined a5 the chemical treatment of a stainless see] with a mild oxidant, such as a nitric acid solution, for the 2 For refrnca ASTM stata, vis te ASTM webs, works. oat ASTI Cuma Serie a neem og, Pr Annas! Book of ASTH ‘Sandan vlan frst, ee ots andar» Decnnt Sima pags o8 ‘AST webate fice, Washington, DC 20402. "A Summary of Changes section appears atthe end of this standard Corts ASTA tein, 09 BV Dm, FOR 708, Mt Consnotntan, A 1928.2850, ned erfly A967 -05" purpose of the removal of free iron or other foreign matter, but ‘which is generally not effective in removal of heat tint or oxide scale on stainless steel. In the case of stainless steels with additions of sulfur for the purpose of improved machinability, ‘passivation may also include the removal of sulfides from the surface of the metal fr the purpose of maximizing corrosion resistance. 3.1.1.2 The formation of the protective passive film on @ stainless steel, also called passivation in a more general Context, will occur spontaneously in sir or other oxygen- containing environment when the stainless steel surface is free of oxide scale and exogenous matter. 3.1.13 Chemical westments, such a3 sodium dichromate solutions, may facilitate the more rapid formation of the passive film on a stainless stecl surface already free of scale or foreign matter. Such treatments, also sometimes called passi ‘vation in common usage, are designated 2s post-cleaning ‘weatments in this specification in order to distinguish them ‘from chemical treatments capable of removing free iron from stainless steels, 3.1.1.4 The chemical treatments capable of removing heat tint or oxide scale from stainless steel and capable of dissolving the stainless steel itself, typically called pickling, are substan- tially more aggressive than treatments used for passivation, as defined in 3.1.1.1. The surface of stainless steel that has been pickled is free of scale, free iron, and exogenous foreign matter, and does not require a separatc treatment for passive tion as defined in 3.1.1.1. The passivation process defined in 3.1.12 will occur without further chemical treatment but may bbe augmented and improved by the post-clesning treatments defined in 3.1.1.3, 3.1.1.5 Electrochemical weatments, ingluding clectropick- ling and electropolishing capable of removing heat tint or oxide scale from stainless steel and capable of dissolving the stainless steel itself, are substantially more aggressive than treatments used for passivation, as defined in 3.1.1.1. The surface of sainless steel resulting from these treatments is free of scale, free iron, end exogenous foreign matter, and does not require & separate treatment for passivation as defined ia 3.1.1.1. The passivation process defined in 3.1.1.2 will occur without farther chemical treatment, but may be augmented and im- proved by the post-cleaning teatments defined in 3.1.1.3 Statements regarding chemical treatments, unless otherwise specified, are taken to include electrochemical treatments. 4. Ordering Information 4.1 This the responsibilty of the purchaser to specify a test practice appropriate to any particular material ané application. ‘This specification was written for the purpose of providing an alternative to United States Federal Specification QQ-P-35C, Decermination of the suitability of this specification for that purpose is the responsibility of the purchaser. 42 Unless specified by the purchaser, the chemical treat- ment applied to the stainless stel parts shall be selected by the seller from among the listed passivation treatments. 5. Materials and Preparation for Passivation Treatments 5.1 ‘The passivation treatments shall be of one or more of the following types, The effectiveness of a particular treatment for 1 particular grade of stainless steel in a particular application is ‘demonstrated by meeting the specified testing requingnents: 5.1.1 Treatments in nitric acid, 5.1.2 Treatments in citie acid, 5.1.3 Other chemical treatments, including electrochemical treatments, 3.1.4 Neutralization, and 5.1.5 Post-cleaning treatments 5.2 Materials: 5.2.1 The chemicals used for passivation treatments shall produce passivated surfaces that meet the requirements of one ‘or more of the tests of this specification. Attention shall be given to maintaining adequate volume, concentration, putty and temperature control appropriate to the size and amount of stainless stee] to be treated 5.2.2 The processor shall maintain a record with regard to concentration and temperature of the passivation solution sufficient to demonstrate thatthe specified passivation condi- tions were maintained for each Tot of stainless steel parts processed, Such records shall be available for inspection when specified in the purchase order. The processor is not required to reveal the precise composition of proprietary chemical mix- tures but shall maintain a unique identification of the mixture that will ensue its accurate representation for subsequent use. ‘5.2.3 The processor shall be responsible for the safe dis- posal of all material generated by this process. ‘5.3 Preparation for Passivation Treatments 53.1 The pretreatment methods and procedures used prior to the passivation treatment, including mechanical and chemi- cal methods, singly or in combination, for descaling and pickling, shall be in accordance with Practice A 380. When clectrochemical cleaning is required, it shall be performed in accordance with Practice B 254. 5.3.2 The resulting pretreated surface shall be substantially free of ol, grease, rust, scale, and other foreign matter, 5.3.3 When the final pretreatment of a part includes pickling of the entire surface of the part, no further passivation treatment is required prior to testing of the surface unless specified by the purchaser. 6. Treatments in Nitrie Acid Solutions 6.1 Passivation Treatment: 6.1.1 Stainless steel parts shall be treated in one of the following aqueous solutions and maintained within the speci- fied temperature range for the specified time. 6.1.1.1 Niric —The solution shall contain 20 1025 volume percent of nitric acid and 2.5 + 0.5 weight percent of sodium chromate. The parts shall be immersed for a minimum of 20, ‘min at a temperature in the range from 120 t© 130°F (49 10 54°0). 6.1.12 Nitric 2—The solution shall contain 20 to 45 volume percent of nitric acid. The parts shall be immersed for a ‘minimama of 30 min at a temperature in the range from 70 10 90°F (21 to 32°C). 6.1.13. Nitric 3—The solution shall contain 20 to 25 volume ‘percent nitric acid. The pars shall be immereed for @ minimum ff 20 min ata temperature in the range from 120 to 140°F (49 10 60°C).Aly a 967 - 05°" 6.1.14 Nitric 4—The solution shall contain 45 to 55 volume percent of nittic ecid. The parts shall be immersed for @ ‘minimum of 30 min ata temperature in the range from 120 10 130°F (49 to 54°C). 6.1.15 Nitric 5—Other combinations of temperature, time, ‘and concentration of nitric acid, with or without other chemi- cals, including accelerans, inhibitors, or proprietary solutions, ‘capable of producing parts that pass the specified test require ments, 6.2 Wetter Rinse—Immediately after removal from the pas- sivating solution the parts shall be thoroughly rinsed, using stagnant, countercurrent, or spray washes singly or in combi- nation, with or without a separate chemical treatment for neutralization (Gee 9.1) of the passivation media, with a tinal rinse being carried out using water with a maximum total solids ‘content of 200 pra. 17, Treatments in Citric Acid 7.1 Passivation Treatment: 7A Stainless steel pars shall be treated in one of the following aqueous solutions and maintained within the speci- fied temperature range for the specified time, Jalul.l Circ I—The solution shall contain 4 to 10 weight percent of citric acid. The parts shall be immersed for a ‘minimum of 4 min at 2 temperature in the range from 140 t0 160°F (60 t0 71°C). 71.2 Citric 2—The solution shall contain 4 :0 10 weight petcent of citric acid, The parts shall be immersed for a ‘minimum of 10 min at a temperature in the range from 120 t0 140°F (49 to 60°C). T.L.13 Citric 3—The solution shall contain 4 to 10 weight percent of cittic acid. The parts shall be immersed for a ‘minimum of 20 min at a temperature in the range from 70 to 120°F (21 to 49°C). ‘.l.L.d Citric 4—Other combinations of temperature, time, and concentration of citric acid, with or without other chemi- cals to enhance cleaning, including accelerants, inhibitors, oF proprietary solutions capable of producing parts that pass the specified test requirements. 7.115 Citric 5—Other combinations of temperature, time, and concentrations of citric ack, with or without other chemi- cals to enhance cleaning, including accelerants, inhibitors, ot ‘proprietary solutions capable of producing parts that pass the specified test requirements, Immersion beth to be controlled at a pH of 18-22. "1.2. Water Rinse—Immediately after removal from the pas sivating solution, the parts shall be thoroughly rinsed, using stagnant, countercurrent, oF spray washes, singly or in combi- nation, with or without a separate chemical treatment for neutralization of the passivation media (see 9.2), with a final rinse being carried out using water with a maximum total solids content of 200 ppm. ‘8, ‘Treatments in Other Chemical Solutions, Including Electrochemical Treatments 8.1 It is recognized that the purpose of removal of all ‘exogenous matter from 8 stainless steel surface, including the removal of free irom, can be accomplished by different media, with potential for benefits to be gained from use of proprietary skills and art, including proprietary passivation media, Such tueatments may include extemally applying an electrical po tential on the stainless steel parts, as in the case of electropal- ishing. The suitability of such passivation treatments for use in meeting the requisements of this specification shall be deter- rmined by the capability of the processed) parts meeting the specified test requirements 8.2 Stainless steel parts shall be treated in a specified ‘aqueous solution, with or without externally applied electrical potential, and maintained within a specified temperature range for a time sufficient for the processed parts to meet the specified test requirement, 8.3 Wover Rinse—Immediately after removal from the pas- sivating solution, the pars shall be thoroughly rinsed, using stagnant, countercurrent, or spray washes, singly or in combi- nation, with or without a separate chemical weatment for neutralization of the passivation media (see 9.2), with a final rinse being carried out using water with a maximum toval solids ‘content of 200 ppm. 9. Neutralization 9.1 The chemical reactions of the passivating media on the surface of the sinless stel shall be stopped by cinsing of the stainless steel part, with or without a separate neuttalization treatment 9.2 The suitability of # neutralization procedure is deter- mined by the capability of the processed parts meeting the specified test requirements (see Note 1) [Nore 1—The selection of medium and procedures fora neutralization depends of the chemistry of the pessivaion und on eccaomic consider ttlons. An example ofa neuralizing trestment would be immersion of the Dt for mininam of 30 mini a solution of § % NaOH at 160 0 180°F (it 82°C, followed by a water ine 10, Post-Cleaning Treatments 10.1 Although the passive film characteristic of stainless steel will form spontaneously in air or any other oxygen: ‘containing environment, the processor shall, when specified ‘apply a chemical treatment that will accelerate the formation of the passive film on a chemically clean stainless steel surface. ‘An example of a medium that serves to accelerate the forma tion of the passive film hut does not contribute tothe removal Of free ‘von from the stainless steel surface would be an aqueous solution of sodium dichromate. 10.2 When specified, within one hour after the final water rinse a8 required in 6.2, 7.2, or 8.3, all feritic and martensitic stee! parts shall be immersed in an aqueous solution containing 410 6 weight percent of sodium dichromate ata temperature in the range from 140 to 160°F (60 10 71°C) for a minimum of 30 min, followed by a rinse in accordance with 6.2, 7.2, or 83. ‘The parts shall then be thoravghly dried, 303 The purchaser may specify other post-cleaning treat~ ments. 0. Fi 1.1 The passivated parts shall exhibit a chemically clean surface and shall, on visual inspection, show no etching, pitting, or frosting resulting from the passivation procedures.