1、Designation: D800 05 (Reapproved 2014)Standard Test Methods ofChemical Analysis of Industrial Metal CleaningCompositions1This standard is issued under the fixed designation D800; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 These test methods descr
3、ibe the procedures for thechemical analysis of industrial metal cleaning compositions insolid, paste, or liquid form. These cleaning compositions maycontain caustic alkalies, silicates, phosphates, chromates,carbonates, bicarbonates, borates, sulfates, sulfites, nitrates,chlorides, soaps, rosin, sul
4、fonated wetting 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 D500. The examination under
5、 a low power microscopeor magnifying glass, supplemented by a few qualitative tests,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 58Total Fatty Acids (and Rosin) 9 and 10N
6、a2O Combined with Fatty Acids (and Rosin) 11 and 12Anhydrous Soap 13Rosin (McNicoll Test Method):Qualitative 14 and 15Quantitative 1619Total Silica Calculated as SiO22023Phosphates:Qualitative 24 and 25Quantitative 2618Combined Sodium and Potassium Oxides 3437Chlorides 3840Sulfates 4143Water, Distil
7、lation Test Method 4447Carbon Dioxide by Evolution-Absorption Test Method 4852Loss at 105C 53 and 54Total Matter Insoluble in Alcohol 5557Free Alkali 5860Synthetic Detergent or Wetting Agent 61 and 62Volatile Hydrocarbons 6367Loss on Ignition 68 and 69Report 70 and 711.3 The values stated in SI unit
8、s are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport 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 pract
9、ices and determine the applica-bility of regulatory limitations prior to use. Material SafetyData Sheets are available for reagents and materials. Reviewthem for hazards prior to usage. See 6.1 for a specific hazardsstatement.2. Referenced Documents2.1 ASTM Standards:2D500 Test Methods of Chemical A
10、nalysis of Sulfonated andSulfated OilsD841 Specification for Nitration Grade TolueneD843 Specification for Nitration Grade XyleneD1193 Specification for Reagent Water3. Purity of Reagents and Materials3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated
11、, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American 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
12、its use without lessening theaccuracy of the determination.1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and are the direct responsibility of SubcommitteeD12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and theirComponents.Cur
13、rent edition approved Jan. 1, 2014. Published February 2014. Originallyapproved in 1944. Last previous edition approved in 2005 as D800 05. DOI:10.1520/D0800-05R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Boo
14、k 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 suggestions on the testing of reagents notlisted by the American Chemical Society, see An
15、alar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1
16、3.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD1193.4. Preparation of Sample4.1 Samples of metal cleaning compositions shall be wellmixed. Excessive exposure to the air shall be avoided toprevent the sample from absorbing mois
17、ture 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 10.000 g in freshly boiledwater and dilute to 500 mL as the sample for analysis.4.3 Liquid or Paste CleanersIf the clean
18、er 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 for analysis.NOTE 1In order to prepare this sample it is first necessary todetermine the water content (Sections 4447), lo
19、ss at 105C (53 and 54),and volatile hydrocarbons (Sections 6367).TOTAL ALKALINITY AS NA2O5. Reagents5.1 Ethyl Ether.5.2 Hydrochloric Acid, Standard (0.5 N)Prepare and stan-dardize 0.5 N hydrochloric acid (HCl).5.3 Methyl Orange Indicator Solution5.4 Sodium Hydroxide, Standard Solution (0.5 N)Prepare
20、and 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 safety precau-tions and instructions on the manufacturers label or MSDS(Material Safety Data Sheet).7. Procedure7.1 Pipet 50 mL
21、 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 expel carbon dioxide (CO2). Cool, add25 mL of ethyl ether, and titrate the excess HCl with 0.5 NNaOH solution. When the wa
22、ter 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 gelatinous mass which will produce atroublesome emulsion. All the soap will have been decom-posed during the reaction and t
23、he 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 Na2O,%5 A 2 B! 30.0155 3100#/W (1)where:A = millilitres of 0.5 N HCl (1 mL of 0.5 N HCl = 0.0155 gof Na2O),B = millilitres o
24、f 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 from the titration in Section 7, usingadditional ether to wash all the fat or oil into the separatoryfunnel.Allow the two
25、 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 with successive portions of water until theyare no longer acid to methyl orange. Transfer the ether layer toa weighed flas
26、k, 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 fatty acids and rosin acids!,%5 E/W! 3100 (2)where:E = grams of ether residue, andW = grams of sample used.NA2O COMBINED W
27、ITH 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 phenolphthalein indicator solution, and titrate with 0.5 NNaOH solution.12. Calculation12.1 Calculate the percentage of Na2O combined
28、with thefatty acids (and rosin acids) as follows:Na2O combined with fatty acids and rosin acids!, % (3)5 B 30.0155!/W 3100where:B = millilitres of 0.5 N NaOH solution (1 mL of 0.5 NNaOH = 0.0155 g of Na2O), andW = grams of sample used.ANHYDROUS SOAP13. Calculation13.1 Calculate the percentage of anh
29、ydrous soap as follows:H 5 C 30.29 (4)F 5 R 2 HP 5 F1CD800 05 (2014)2where:C = percentage of Na2O combined with fatty acids (androsin acids) (Section 11),F = percentage of fatty acid anhydride,H = percentage of water equivalent,R = percentage of fatty acids (and rosin acids) (Section 10),andP = perc
30、entage of anhydrous soap.ROSIN (McNICOLL TEST METHOD)Qualitative14. Reagents14.1 Acetic Anhydride (99 to 100 %).14.2 Sulfuric Acid (34.7 + 35.7)Prepare by carefully add-ing 34.7 mL of H2SO4(sp gr 1.84) to 35.7 mL of water.15. Procedure15.1 The presence of rosin may be determined qualitativelyby test
31、ing 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 weight of acetic anhydride, and then cool thesolution. Allow several drops of H2SO4to flow slowly into theacetic anhydride-f
32、at 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 testing a sample of fatty acids to which rosin hasbeen added. If the test for rosin is positive the quantitativeproced
33、ure 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 a reflux condenser.16.1.1 Esterification FlaskA 150-mL flask of either theround-bottom or Erlenmeyer type shall be used
34、.16.1.2 Reflux CondenserAny suitable water-cooled, glassreflux condenser may be used.17. Reagents17.1 Naphthalene-Sulfonic Acid SolutionDissolve 40 gof Eastman grade or equivalent reagent in 1 L of absolutemethyl alcohol.17.2 Phenolphthalein Indicator Solution (5 g/L)Dissolve0.5 g of phenolphthalein
35、 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 (KOH) inneutral redistilled alcohol (due to volatility of alcohol, thissolution should be restandardized frequently).17.4 Su
36、lfuric 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 asufficient portion of the sample to give the equivalent of 50 gof dry material in 500 mL of hot water. (If the cleaner to
37、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 ina clear layer. Siphon off the aqueous acid layer, add 300 mL ofhot water, boil gently for a few minutes, and siphon off t
38、heaqueous 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 oxidation ofthe acids.After the last washing, remove the last traces of waterfrom the beaker with a pipet, filter the fatty ac
39、ids 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 present, decant theclear fatty acids into another beaker, and again reheat themmomentarily to 130C. These acids may then
40、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-sulfonic acid solution. Add a few glass beads toensure smooth boiling, attach the reflux condenser, and boil for30 min; also, run a bla
41、nk 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 alcoholic KOH solution.19. Calculation19.1 Calculate the results as follows:R 5 S 2 B! 3 N 30.346 3100#/W (5)R15 R 2 1.0R25 R13
42、 F!/100RS5 R231.064where:R = percentage of rosin acids in fatty acids,R1= corrected percentage of rosin acids in fatty acids (Note2),R2= percentage of rosin on basis of original sample,RS= percentage of rosin soda soap on basis of originalsample,S = millilitres of KOH solution required for titration
43、 of thesample,B = millilitres of KOH solution required for titration of theblank,N = normality of the KOH solution,W = grams of sample used,F = percentage of total fatty acids (and rosin acids) in thecleaner, andA = percentage of total anhydrous soap (Section 13).19.2 If true fatty acid soap is desi
44、red, subtract the rosin soapfrom the total anhydrous soap.NOTE 2Cooperative studies have shown that the McNicoll testmethod gives results approximately 1 % higher than the amount of rosinD800 05 (2014)3present. Consequently, the committee recommends deducting 1 % fromthe percentage of rosin found in
45、 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 of HCl(sp gr 1.19) and water.20.3 Hydrofluoric Acid (sp gr 1.15)Prepare a solution ofhydrofluoric acid (HF) having a sp
46、ecific 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 the cleaner,draw off the water solution from the total alkalinity titration(Section 7) into a porcelain evaporating dish. Add an excess ofH
47、Cl (sp gr 1.19), evaporate the mixture to dryness on a steambath, and carry out the procedure in Section 22. The weight ofthe sample will be 1.000 g.21.2 When Soap is Not PresentIf soap is not present in thecleaner, transfer a 100-mL aliquot of the sample solutionobtained as described in Section 3 t
48、o 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 described in Section 22. Theweight of the sample will be 2.000 g.22. Procedure22.1 Triturate the dehydrated residue, obtained
49、 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 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 pape
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