1、Designation: D 2358 89 (Reapproved 2003)Standard Test Method forSeparation of Active Ingredient from Surfactant and SyndetCompositions1This standard is issued under the fixed designation D 2358; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、 from 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
4、-soluble 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 This standard does not purport to address all of thesafety concerns, if any, associated w
5、ith 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 reagents and materials. Reviewthem for hazards prior to usage.
6、2. Referenced Documents2.1 ASTM Standards:D 1681 Test Method for Synthetic Anionic Active Ingredi-ent in Detergents by Cationic Titration Procedure23. Summary of Test Method3.1 The test method involves the extraction of the activeingredient with alcohol. Reprecipitation of the insolubles isspecified
7、 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-soluble matter. An estimation of sodium chloride content ismade so that a corrected total active ingredient level may beob
8、tained. 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 otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalR
9、eagents 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 purity to permit its use without lessening the accuracy ofthe determination.4.2 Unless otherwise indicated, references
10、 to water shall beunderstood to mean distilled water or water of equal purity.SEPARATION OF TOTAL ALCOHOL-SOLUBLEMATTER5. Reagents5.1 Ethyl Alcohol (95 percent)Freshly boiled ethyl alco-hol conforming to Formula No. 3A or No. 30 of the U. S.Bureau of Internal Revenue. The alcohol should not beneutra
11、lized. 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 alcohol conforming to either Formulas No. 3A or No. 30of the U. S. Bureau of Internal Revenue.5.3 Phenolphthalein Indic
12、ator Solution (10 g/L)Dissolve1 g of phenolphthalein in 50 mL of ethyl alcohol (95 %) andthen mix with 50 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 of Soaps and Synthet
13、ic Detergents.Current edition approved May. 26, 1989. Published July 1989. Originallypublished as D 2358 65 T. Last previous edition D 2358 82 (1987).2Annual Book of ASTM Standards, Vol 15.04.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For
14、suggestions 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 Internati
15、onal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.4 Sulfuric Acid (1 + 100)Add 1 mL of concentratedsulfuric acid (H2SO4, sp gr 1.84) to 100 mL of water.6. Safety Precautions6.1 Formulas No. 3A and No. 30 ethyl alcohols are dena-tured alcohols. They are healt
16、h 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 protection. If acid contacts thebody or is splashed in the eyes, flush the affected parts withwater for at lea
17、st 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 beaker. Liquid samples containing highlevels of water should be evaporated to a pasty consistencyafter weighi
18、ng. 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 on a steam bath for approximately 112 to2 h, stirring frequently to disperse the solids and break up anylu
19、mps.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 H2SO4using no more than 1 mL. Samplescontaining high levels of free alkali, requiring more than 1 mLof 1 N
20、 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 solution is acid originally, neutralize thefree acid with alcoholic NaOH solution to the phenolphthaleinend po
21、int. 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 Add 50 mL of hot 95 % alcohol to the residue in thebeaker and bring to boiling on a safety hot plate. Le
22、t 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 theinsolubles in the beaker.7.5 Evaporate the residual alcohol from the residue in thebeaker on a steam bath, s
23、tirring 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 solution.7.6 Dilute the water solution with 200 mL of hot absolutealcohol. Bring to a boil on a steam bath and
24、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 the filterwith several small portions of hot 95 % alcohol.7.7 Evaporate the combined alcoholic filtrate
25、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 flask and evaporateto dryness on a steam bath. Place in an oven maintained at 1056 2C and dry for half-hour p
26、eriods to constant weight.8. Calculation8.1 Calculate the percentage of total alcohol-soluble matteras follows:Total alcohol2soluble matter, % 5 W 2 T!/S#3 100 (1)where:W = weight of dish plus alcohol-soluble matter, g,T = weight of dish, g, andS = grams of sample in aliquot taken.CORRECTION FOR SOD
27、IUM 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 drops of methylorange indicator solution and acidify to the acid color by usingHNO3(1+4). Warm slightly, s
28、tir, and add 50 mL of acetone.Follow the procedure for quantitative determination, startingwith 13.2 of Method D 1681.10. Calculation10.1 Calculate the percentage of sodium chloride (NaCl) asfollows:NaCl, % 5 B 3 N3 0.05845!/S# 3 100 (2)where:B = millilitres of AgNO3solution used,N = normality of th
29、e AgNO3solution, andS = grams of sample in aliquot taken.TOTAL ACTIVE INGREDIENT11. Calculation11.1 Calculate the corrected alcohol-soluble matter, whichis a measure of the total active ingredient, as follows:Alcohol2soluble matter, corrected, % 5 A 2 C (3)where:A = percentage of total alcohol-solub
30、le 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 7Over 80 5D 2358 89 (2003)2PURIFICATION OF TOTAL ALCOHOL-SOLUBLEMATTER12. Reagent12.1 Acetone-Ether M
31、ixture (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 area and protective gloves and garments should be used.13.2 Ether is a skin, brain, and kidney irrita
32、nt 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 garments should be used.NOTE 1See special instructions on manufacturers label for acetoneand ether
33、 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 general-purpose acid-washed filter paper. Collect thefiltrate in a small beaker. Wash the paper with
34、 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 infrared spectropho-tometric or qualitative examination. If the sample size is insufficientforthese purp
35、oses, 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 the validity of any patent rights asserted in connection with any item mentionedin this standard. U
36、sers of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed eve
37、ry five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible techn
38、ical 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 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).D 2358 89 (2003)3
