1、Designation: D2358 89 (Reapproved 2009)Standard Test Method forSeparation of Active Ingredient from Surfactant and SyndetCompositions1This standard is issued under the fixed designation D2358; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, the 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.1. Scope1.1 This test method covers the procedure for the separationand purification of active ingredient fr
3、om surfactants andsyndet compositions. The separated active ingredient may beused for qualitative examinations. This test method alsopermits the estimation of total active ingredient level present inthe sample under test.1.2 This test method yields the active ingredient togetherwith other alcohol-so
4、luble materials and therefore is usefulonly in estimating the actual active ingredient level. Correctionfor the amount of the most common contaminant, sodiumchloride, is shown by a separate determination.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement a
5、re 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 practices and determine the applica-bility of regulatory limitations
6、prior to use. Material SafetyData Sheets are available for reagents and materials. Reviewthem for hazards prior to usage.2. Referenced Documents2.1 ASTM Standards:2D1681 Test Method for SyntheticAnionicActive Ingredientin Detergents by Cationic Titration Procedure3. Summary of Test Method3.1 The tes
7、t method involves the extraction of the activeingredient with alcohol. Reprecipitation of the insolubles isspecified to remove the last traces of active ingredient. Dilutionof the alcoholic extract to a known volume and the evaporationof a suitable aliquot permits measurement of total alcohol-solubl
8、e matter. An estimation of sodium chloride content ismade so that a corrected total active ingredient level may beobtained. Provision is made for purification of the activeingredients in Section 14.4. Reagents4.1 Purity of Reagents:4.1.1 Reagent grade chemicals shall be used in all tests.Unless othe
9、rwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society, where suchspecifications are available.3Other grades may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh pu
10、rity to permit its use without lessening the accuracy ofthe determination.4.2 Unless otherwise indicated, references to water shall beunderstood to mean distilled water or water of equal purity.SEPARATION OF TOTALALCOHOL-SOLUBLEMATTER5. Reagents5.1 Ethyl Alcohol (95 percent)Freshly boiled ethyl alco
11、-hol conforming to Formula No. 3A or No. 30 of the U. S.Bureau of Internal Revenue. The alcohol should not beneutralized. Redistilled alcohol shall be used if alkali absorp-tion is more than 0.2 mL of 0.1 N NaOH solution/100 mL ofalcohol.5.2 Ethyl Alcohol (Absolute)Freshly boiled 200-proofethyl alco
12、hol conforming to either Formulas No. 3A or No. 30of the U. S. Bureau of Internal Revenue.5.3 Phenolphthalein Indicator Solution (10 g/L)Dissolve1 g of phenolphthalein in 50 mL of ethyl alcohol (95 %) andthen mix with 50 mL of water.5.4 Sulfuric Acid (1 + 100)Add 1 mL of concentratedsulfuric acid (H
13、2SO4, sp gr 1.84) to 100 mL of water.1This test method is under the jurisdiction of ASTM Committee D12 on Soapsand Other Detergents and is the direct responsibility of Subcommittee D12.12 onAnalysis and Specifications of Soaps, Synthetics, Detergents and their Components.Current edition approved Oct
14、. 1, 2009. Published December 2009. Originallyapproved in 1965 as D2358 65 T. Last previous edition approved in 2003 asD2358 89 (2003). DOI: 10.1520/D2358-89R09.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book o
15、f 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 Anal
16、ar 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, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6
17、. Safety Precautions6.1 Formulas No. 3A and No. 30 ethyl alcohols are dena-tured alcohols. They are health hazards and flammable liquids.See manufacturers label warning as to use, safe handling, anddisposal.6.2 Sulfuric acid is corrosive. Use proper protective equip-ment including adequate eye prote
18、ction. If acid contacts thebody or is splashed in the eyes, flush the affected parts withwater for at least 15 min. Obtain medical attention.7. Procedure7.1 Weigh out a sample, to the nearest 0.01 g, to correspondwith the levels of active ingredient prescribed in Table 1 andtransfer to a 600-mL beak
19、er. Liquid samples containing highlevels of water should be evaporated to a pasty consistencyafter weighing. Samples containing high levels of hydratedalkaline salts should be dried in an oven at 105C for 1 h afterweighing.7.2 Add 300 to 350 mL of hot 95 % alcohol. Cover with awatch glass and heat o
20、n a steam bath for approximately 112 to2 h, stirring frequently to disperse the solids and break up anylumps.7.3 Remove the beaker from the steam bath and permit theinsolubles to settle for a few minutes. Add 2 drops ofphenolphthalein indicator solution. If the solution is pink,neutralize with 1 N H
21、2SO4using no more than 1 mL. Samplescontaining high levels of free alkali, requiring more than 1 mLof 1 N H2SO4, should be neutralized with H2SO4of higherconcentration to limit the amount added to less than 1 mL.Before proceeding, make the solution just alkaline with 0.1 NNaOH solution. If the solut
22、ion is acid originally, neutralize thefree acid with alcoholic NaOH solution to the phenolphthaleinend point. Decant the alcoholic solution through a suitablefilter, retaining as much as possible of the insoluble matter inthe beaker. Collect the clear filtrate in a suitable filter flask orbeaker.7.4
23、 Add 50 mL of hot 95 % alcohol to the residue in thebeaker and bring to boiling on a safety hot plate. Let theinsolubles settle and decant the alcoholic solution through thefilter as before. Repeat the extraction of the insolubles with anadditional 50 mL of 95 % alcohol, retaining the bulk of theins
24、olubles in the beaker.7.5 Evaporate the residual alcohol from the residue in thebeaker on a steam bath, stirring at intervals to permit completeevaporation of the solvent. Dissolve the residue in the beaker ina minimum volume of hot water, not to exceed 10 mL, heatingon a steam bath to effect soluti
25、on.7.6 Dilute the water solution with 200 mL of hot absolutealcohol. Bring to a boil on a steam bath and filter through thepreviously used filter, combining the filtrate with the initialalcoholic filtrate. Wash the beaker and residue several timeswith hot 95 % alcohol, transferring the insolubles to
26、 the filterwith several small portions of hot 95 % alcohol.7.7 Evaporate the combined alcoholic filtrate and washingsto approximately 450 mL and transfer to a 500-mL volumetricflask. Cool to room temperature and dilute to volume with95 % alcohol. Mix well.7.8 Pipet a 100-mL aliquot into a tared flas
27、k and evaporateto dryness on a steam bath. Place in an oven maintained at 1056 2C and dry for half-hour periods to constant weight.8. Calculation8.1 Calculate the percentage of total alcohol-soluble matteras follows:Total alcohol2soluble matter, % 5 W 2 T!/S3 100 (1)where:W = weight of dish plus alc
28、ohol-soluble matter, g,T = weight of dish, g, andS = grams of sample in aliquot taken.CORRECTION FOR SODIUM CHLORIDE CONTENT9. Procedure9.1 Pipet a suitable aliquot from the solution as prepared in7.7 into a 400-mL beaker. Evaporate to a volume of about 30mL and dilute to 100 mL with water. Add 2 dr
29、ops of methylorange indicator solution and acidify to the acid color by usingHNO3(1+4). Warm slightly, stir, and add 50 mL of acetone.Follow the procedure for quantitative determination, startingwith 13.2 of Method D1681.10. Calculation10.1 Calculate the percentage of sodium chloride (NaCl) asfollow
30、s:NaCl, % 5 B 3 N3 0.05845!/S 3 100 (2)where:B = millilitres of AgNO3solution used,N = normality of the AgNO3solution, andS = grams of sample in aliquot taken.TOTALACTIVE INGREDIENT11. Calculation11.1 Calculate the corrected alcohol-soluble matter, whichis a measure of the total active ingredient, a
31、s follows:Alcohol2soluble matter, corrected, % 5 A 2 C (3)where:A = percentage of total alcohol-soluble matter (Section 8),andC = percentage of NaCl (Section 10.).TABLE 1 Active Ingredient Level ExpectedActive Ingredient Level Expected, % Weight of Sample, g10 to 25 2025 to 40 1540 to 60 1060 to 80
32、7Over 80 5D2358 89 (2009)2PURIFICATION OF TOTALALCOHOL-SOLUBLEMATTER12. Reagent12.1 Acetone-Ether Mixture (1+1)Mix 1 part of acetonewith 1 part of ether.13. Safety Precautions13.1 Acetone is a flammable solvent and a health hazard.This test should be performed in a well-ventilated explosion-proof ar
33、ea and protective gloves and garments should be used.13.2 Ether is a skin, brain, and kidney irritant and anextreme fire and explosion hazard. All precautions should betaken to proceed with this test only in a special explosion-proofarea and under a special explosion-proof hood. Protectivegloves and
34、 garments should be used.NOTE 1See special instructions on manufacturers label for acetoneand ether warning and disposal.14. Procedure14.1 To the dried residue from 7.8 add 50 mL of ac-etoneether mixture and warm on a steam bath.14.2 Agitate with a glass stirring rod and filter while warmthrough a g
35、eneral-purpose acid-washed filter paper. Collect thefiltrate in a small beaker. Wash the paper with a few smallvolumes of acetone-ether mixture.14.3 Evaporate the combined filtrate and washings on asteam bath. Dry the residue in an oven at 105 6 2C.NOTE 2The evaporated fraction may be used for infra
36、red spectropho-tometric or qualitative examination. If the sample size is insufficientforthese purposes, a larger aliquot may be taken for evaporation.15. Keywords15.1 active ingredient; alcohol extraction; surfactant com-positions; syndet compositionsASTM International takes no position respecting
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39、Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This
40、 standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D2358 89 (2009)3
