1、Designation: D 800 05Standard Test Methods ofChemical Analysis of Industrial Metal CleaningCompositions1This standard is issued under the fixed designation D 800; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test methods describe the procedures f
3、or thechemical analysis of industrial metal cleaning compositions insolid, paste, or liquid form. These cleaning compositions maycontain caustic alkalies, silicates, phosphates, chromates, car-bonates, bicarbonates, borates, sulfates, sulfites, nitrates, chlo-rides, soaps, rosin, sulfonated wetting
4、agents, anti-foamingagents, organic bases, organic solvents, organic couplingagents, and sometimes inorganic acid salts or organic acids.Occasionally, such cleaning compositions may contain sul-fonated oils; in such cases, reference should be made toMethod D 500. The examination under a low power mi
5、cro-scope or magnifying glass, supplemented by a few qualitativetests, will often indicate the number of components and theiridentity.1.2 The analytical methods appear in the following order:SectionPreparation of Sample 4Total Alkalinity as Na2O 5-8Total Fatty Acids (and Rosin) 9 and 10Na2O Combined
6、 with Fatty Acids (and Rosin) 11 and 12Anhydrous Soap 13Rosin (McNicoll Test Method):Qualitative 14 and 15Quantitative 16-19Total Silica Calculated as SiO220-23Phosphates:Qualitative 24 and 25Quantitative 26-18Combined Sodium and Potassium Oxides 34-37Chlorides 38-40Sulfates 41-43Water, Distillation
7、 Test Method 44-47Carbon Dioxide by Evolution-Absorption Test Method 48-52Loss at 105C 53 and 54Total Matter Insoluble in Alcohol 55-57Free Alkali 58-60Synthetic Detergent or Wetting Agent 61 and 62Volatile Hydrocarbons 63-67Loss on Ignition 68 and 69Report 70 and 711.3 This standard does not purpor
8、t to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Material SafetyData Sheets are available for re
9、agents and materials. Reviewthem for hazards prior to usage. See 6.1 for a specific hazardsstatement.2. Referenced Documents2.1 ASTM Standards:2D 500 Test Methods of Chemical Analysis of Sulfonatedand Sulfated OilsD 841 Specification for Nitration Grade TolueneD 843 Specification for Nitration Grade
10、 XyleneD 1193 Specification for Reagent Water3. Purity of Reagents and Materials3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the Ame
11、rican Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.3.2 Unless otherwise indicated, references to water shall beun
12、derstood to mean reagent water conforming to SpecificationD 1193.4. Preparation of Sample4.1 Samples of metal cleaning compositions shall be wellmixed. Excessive exposure to the air shall be avoided to1These test methods are under the jurisdiction of ASTM Committee D-12 onSoaps and Other Detergents
13、and are the direct responsibility of SubcommitteeD12.12 on Analysis of Soaps and Synthetic Detergents.Current edition approved May 1, 2005. Published June 2005. Originallyapproved in 1944. Last previous edition approved in 1997 as D 800 91(1997).2For referenced ASTM standards, visit the ASTM website
14、, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggest
15、ions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 1
16、00 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.prevent the sample from absorbing moisture and carbondioxide and, if a volatile solvent is present, to preventevaporation.4.2 Solid CleanersIf the cleaner is a solid and appears tocontain no volatile solvent, dissolve
17、 10.000 g in freshly boiledwater and dilute to 500 mL as the sample for analysis.4.3 Liquid or Paste CleanersIf the cleaner is a paste orliquid dissolve a sufficient portion in freshly boiled water togive the equivalent of 10.000 g of the dry material in solution,and dilute to 500 mL as the sample f
18、or analysis.NOTE 1In order to prepare this sample it is first necessary todetermine the water content (Sections 44-47), loss at 105C (53 and 54),and volatile hydrocarbons (Sections 63-67).TOTAL ALKALINITY AS NA2O5. Reagents5.1 Ethyl Ether.5.2 Hydrochloric Acid, Standard (0.5 N)Prepare and stan-dardi
19、ze 0.5 N hydrochloric acid (HCl).5.3 Methyl Orange Indicator Solution5.4 Sodium Hydroxide, Standard Solution (0.5 N)Prepareand standardize a 0.5 N sodium hydroxide (NaOH) solution.6. Hazards6.1 All reagents and chemicals should be handled with care.Before using any chemical, read and follow all safe
20、ty precau-tions and instructions on the manufacturers label or MSDS(Material Safety Data Sheet).7. Procedure7.1 Pipet 50 mL of the sample (1.000 g) prepared inaccordance with Section 4, into a 250-mL Erlenmeyer flask.Add methyl orange indicator solution and a measured excess of0.5 N HCl, and boil to
21、 expel carbon dioxide (CO2). Cool, add25 mL of ethyl ether, and titrate the excess HCl with 0.5 NNaOH solution. When the water layer is neutral to methylorange, it should be clear unless sodium metasilicate (or othersilicate) is present in large quantities. If silicates are present,they will form a
22、gelatinous mass which will produce atroublesome emulsion. All the soap will have been decom-posed during the reaction and the corresponding fatty acid willbe found in the ether layer.8. Calculation8.1 Calculate the total alkalinity as percentage of sodiumoxide (Na2O) as follows:Total alkalinity as N
23、a2O,%5 A 2 B! 3 0.0155 3 100/W (1)where:A = millilitres of 0.5 N HCl (1 mL of 0.5 N HCl = 0.0155gofNa2O),B = millilitres of 0.5 N NaOH solution, andW = grams of sample used.TOTAL FATTY ACIDS (AND ROSIN ACIDS)9. Procedure9.1 Pour into a separatory funnel the neutral ethyl ether-water mixture obtained
24、 from the titration in Section 7, usingadditional ether to wash all the fat or oil into the separatoryfunnel.Allow the two layers to separate, and draw off the waterlayer into a second separatory funnel. Wash the water layerwith two 10-mL portions of ethyl ether. Combine the etherextracts, and wash
25、with successive portions of water until theyare no longer acid to methyl orange. Transfer the ether layer toa weighed flask, evaporate the ether over a steam bath, andfinally dry to constant weight at 105C.10. Calculation10.1 Calculate the percentage of fatty acids (and rosin acids)as follows:Total
26、fatty acids and rosin acids!,%5 E/W! 3 100 (2)where:E = grams of ether residue, andW = grams of sample used.NA2O COMBINED WITH FATTY ACIDS(AND ROSIN ACIDS)11. Procedure11.1 Dissolve the fatty acid (and rosin acid) residue ob-tained under Section 9 in warm neutral alcohol, add six dropsof phenolphtha
27、lein indicator solution, and titrate with 0.5 NNaOH solution.12. Calculation12.1 Calculate the percentage of Na2O combined with thefatty acids (and rosin acids) as follows:Na2O combined with fatty acids and rosin acids!,%5 B 3 0.0155!/W 3 100 (3)where:B = millilitres of 0.5 N NaOH solution (1 mL of
28、0.5 NNaOH = 0.0155 g of Na2O), andW = grams of sample used.ANHYDROUS SOAP13. Calculation13.1 Calculate the percentage of anhydrous soap as follows:H 5 C 3 0.29 (4)F 5 R 2 HP 5 F 1 Cwhere:C = percentage of Na2O combined with fatty acids (androsin acids) (Section 11),F = percentage of fatty acid anhyd
29、ride,H = percentage of water equivalent,R = percentage of fatty acids (and rosin acids) (Section 10),andP = percentage of anhydrous soap.ROSIN (McNICOLL TEST METHOD)Qualitative14. Reagents14.1 Acetic Anhydride (99 to 100 %).D80005214.2 Sulfuric Acid (34.7 + 35.7)Prepare by carefully add-ing 34.7 mL
30、of H2SO4(sp gr 1.84) to 35.7 mL of water.15. Procedure15.1 The presence of rosin may be determined qualitativelyby testing a portion of the residue obtained under Section 9 bythe Liebermann-Storch reaction as follows:15.1.1 Dissolve a portion of the ether extract by warming inseveral times its weigh
31、t of acetic anhydride, and then cool thesolution. Allow several drops of H2SO4to flow slowly into theacetic anhydride-fat mixture. Rosin is indicated by the devel-opment of a fugitive violet coloration changing to a brownishtinge at the margin of contact of the reagents. The test shouldbe checked by
32、 testing a sample of fatty acids to which rosin hasbeen added. If the test for rosin is positive the quantitativeprocedure should be carried out as described in Sections 16-19.Quantitative16. Apparatus16.1 The apparatus shall consist of a glass flask connected,preferably by a ground-glass joint, to
33、a reflux condenser.16.1.1 Esterification FlaskA 150-mL flask of either theround-bottom or Erlenmeyer type shall be used.16.1.2 Reflux CondenserAny suitable water-cooled, glassreflux condenser may be used.17. Reagents17.1 Naphthalene-b-Sulfonic Acid SolutionDissolve 40 gof Eastman grade or equivalent
34、 reagent in 1 L of absolutemethyl alcohol.17.2 Phenolphthalein Indicator Solution (5 g/L)Dissolve0.5 g of phenolphthalein in 50 mL of neutral redistilled alcoholand then mix with 50 mL of water.17.3 Potassium Hydroxide Solution (0.2 N)Accuratelystandardize a 0.2 N solution of potassium hydroxide (KO
35、H) inneutral redistilled alcohol (due to volatility of alcohol, thissolution should be restandardized frequently).17.4 Sulfuric Acid (1 + 2)Carefully mix 1 volume ofconcentrated sulfuric acid (H2SO4, sp gr 1.84) into 2 volumesof water.18. Procedure18.1 Preparation of Fatty and Rosin AcidsDissolve as
36、ufficient portion of the sample to give the equivalent of 50 gof dry material in 500 mL of hot water. (If the cleaner to betested contains alcohol, the alcohol should be completelyremoved by evaporation from the solution.) Add 100 mL ofH2SO4(1 + 2), and heat gently until the fatty matter collects in
37、a clear layer. Siphon off the aqueous acid layer, add 300 mL ofhot water, boil gently for a few minutes, and siphon off theaqueous acid layer. Wash the acids in this manner three times.Complete this acidification and washing in a very short periodof time, and keep the beaker covered to prevent oxida
38、tion ofthe acids.After the last washing, remove the last traces of waterfrom the beaker with a pipet, filter the fatty acids through oneor two thicknesses of filter paper, and dry at a temperature of105C for 45 to 60 min or heat rapidly to 130C and allow tocool. Do not hold at 130C, but if water is
39、present, decant theclear fatty acids into another beaker, and again reheat themmomentarily to 130C. These acids may then be used for therosin determination.18.2 Esterification and TitrationWeigh about 2 6 0.001 gof the fatty acids into the esterification flask. Add 25 mL ofnaphthalene-b-sulfonic aci
40、d solution. Add a few glass beads toensure smooth boiling, attach the reflux condenser, and boil for30 min; also, run a blank test using 25 mL of the reagent.At theend of the boiling period cool the contents of the flask, add 0.5mL of phenolphthalein indicator, and titrate immediately with0.2 N alco
41、holic KOH solution.19. Calculation19.1 Calculate the results as follows:R 5 S 2 B! 3 N3 0.346 3 100/W (5)R15 R 2 1.0R25 R13 F!/100RS5 R23 1.064where:R = percentage of rosin acids in fatty acids,R1= corrected percentage of rosin acids in fatty acids(Note 2),R2= percentage of rosin on basis of origina
42、l sample,RS= percentage of rosin soda soap on basis of originalsample,S = millilitres of KOH solution required for titration ofthe sample,B = millilitres of KOH solution required for titration ofthe blank,N = normality of the KOH solution,W = grams of sample used,F = percentage of total fatty acids
43、(and rosin acids) in thecleaner, andA = percentage of total anhydrous soap (Section 13).19.2 If true fatty acid soap is desired, subtract the rosin soapfrom the total anhydrous soap.NOTE 2Cooperative studies have shown that the McNicoll testmethod gives results approximately 1 % higher than the amou
44、nt of rosinpresent. Consequently, the committee recommends deducting 1 % fromthe percentage of rosin found in the fatty acids.TOTAL SILICA CALCULATED AS SiO220. Reagents20.1 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl).20.2 Hydrochloric Acid (1 + 1)Mix equal volumes ofHCl (sp
45、gr 1.19) and water.20.3 Hydrofluoric Acid (sp gr 1.15)Prepare a solution ofhydrofluoric acid (HF) having a specific gravity of 1.15.20.4 Sulfuric Acid (sp gr 1.84)Concentrated sulfuric acid(CH2SO4).21. Preparation of Sample21.1 When Soap is PresentIf soap is present in thecleaner, draw off the water
46、 solution from the total alkalinitytitration (Section 7) into a porcelain evaporating dish. Add anexcess of HCl (sp gr 1.19), evaporate the mixture to dryness onD800053a steam bath, and carry out the procedure in Section 22. The weight of the sample will be 1.000 g.21.2 When Soap is Not PresentIf so
47、ap is not present in thecleaner, transfer a 100-mL aliquot of the sample solutionobtained as described in Section 3 to a 400-mL evaporatingdish, neutralize with HCl (sp gr 1.19) using methyl orange asthe indicator, evaporate to apparent dryness on a steam bath,and carry out the procedure as describe
48、d in Section 22. Theweight of the sample will be 2.000 g.22. Procedure22.1 Triturate the dehydrated residue, obtained as describedin 21.1 or 21.2, with the smooth end of a stirring rod, moistenthe residue with 10 mL of HCl (1 + 1), and again evaporate toapparent dryness on the steam bath. Dehydrate
49、at 110C for 1h, take up the residue with 10 mL of HCl (1 + 1) and 20 mL ofwater, and digest a short time on the steam bath to effectsolution of the soluble salts. Filter the silica on a fine-texturepaper by washing the dish with hot water. Scrub the dish witha rubber policeman and again wash thoroughly with hot water.Wash the residue and paper free of acid with hot water andreserve.22.2 Evaporate the filtrate and washings on the steam bathin the porcelain dish used before, moisten the residue with 10mL of HCl (1 + 1), and again evaporate to
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