1、Designation: D2358 89 (Reapproved 2009) D2358 16Standard 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
2、 case of 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 separation and purification of active ing
3、redient from surfactants and syndetcompositions. The separated active ingredient may be used for qualitative examinations. This test method also permits theestimation of total active ingredient level present in the sample under test.1.2 This test method yields the active ingredient together with oth
4、er alcohol-soluble materials and therefore is useful only inestimating the actual active ingredient level. Correction for the amount of the most common contaminant, sodium chloride, isshown by a separate determination.1.3 The values stated in SI units are to be regarded as standard. No other units o
5、f measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulato
6、rylimitations prior to use. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior tousage.2. Referenced Documents2.1 ASTM Standards:2D1681 Test Method for Synthetic Anionic Active Ingredient in Detergents by Cationic Titration Procedure3. Summary of Test
7、 Method3.1 The test method involves the extraction of the active ingredient with alcohol. Reprecipitation of the insolubles is specifiedto remove the last traces of active ingredient. Dilution of the alcoholic extract to a known volume and the evaporation of a suitablealiquot permits measurement of
8、total alcohol-soluble matter. An estimation of sodium chloride content is made so that a correctedtotal active ingredient level may be obtained. Provision is made for purification of the active ingredients in Section 1413.3.2 Purity of Reagents:1 This test method is under the jurisdiction of ASTM Co
9、mmittee D12 on Soaps and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Analysisand Specifications of Soaps, Synthetics, Detergents and their Components.Current edition approved Oct. 1, 2009July 1, 2016. Published December 2009August 2016. Originally approved in 1965 as
10、D2358 65 T. Last previous edition approvedin 20032009 as D2358 89 (2003).89 (2009). DOI: 10.1520/D2358-89R09.10.1520/D2358-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information,
11、refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all
12、 changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-295
13、9. United States13.2.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.3 Other grades m
14、ay be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.3.3 Unless otherwise indicated, references to water shall be understood to mean distilled water or water of equal purity.4. Reagents4.1 Pu
15、rity of Reagents:4.1.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.3 Other grades m
16、ay be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.4.2 Unless otherwise indicated, references to water shall be understood to mean distilled water or water of equal purity.SEPARATION OF TOT
17、ALALCOHOL-SOLUBLE MATTERSEPARATION OF TOTALALCOHOL-SOLUBLE MATTER4. Reagents4.1 Ethyl Alcohol (95 percent)Freshly boiled ethyl alcohol conforming to Formula No. 3A or No. 30 of the U. S. Bureau ofInternal Revenue. The alcohol should not be neutralized. Redistilled alcohol shall be used if alkali abs
18、orption is more than 0.2 mLof 0.1 N NaOH solution/100 mL of alcohol.4.2 Ethyl Alcohol (Absolute)Freshly boiled 200-proof ethyl alcohol conforming to either Formulas No. 3A or No. 30 of theU. S. Bureau of Internal Revenue.4.3 Phenolphthalein Indicator Solution (10 g/L)Dissolve 1 g of phenolphthalein
19、in 50 mL of ethyl alcohol (95 %) and thenmix with 50 mL of water.4.4 Sulfuric Acid (1 + 100)Add 1 mL of concentrated sulfuric acid (H2SO4, sp gr 1.84) to 100 mL of water.5. Safety Precautions5.1 Formulas No. 3A and No. 30 ethyl alcohols are denatured alcohols. They are health hazards and flammable l
20、iquids. Seemanufacturers label warning as to use, safe handling, and disposal.5.2 Sulfuric acid is corrosive. Use proper protective equipment including adequate eye protection. If acid contacts the body oris splashed in the eyes, flush the affected parts with water for at least 15 min. Obtain medica
21、l attention.6. Procedure6.1 Weigh out a sample, to the nearest 0.01 g, to correspond with the levels of active ingredient prescribed in Table 1 andtransfer to a 600-mL beaker. Liquid samples containing high levels of water should be evaporated to a pasty consistency afterweighing. Samples containing
22、 high levels of hydrated alkaline salts should be dried in an oven at 105C for 1 h after weighing.6.2 Add 300 to 350 mL of hot 95 % alcohol. Cover with a watch glass and heat on a steam bath for approximately 112 to 2 h,stirring frequently to disperse the solids and break up any lumps.6.3 Remove the
23、 beaker from the steam bath and permit the insolubles to settle for a few minutes.Add 2 drops of phenolphthaleinindicator solution. If the solution is pink, neutralize with 1 N H2SO4 using no more than 1 mL. Samples containing high levelsof free alkali, requiring more than 1 mL of 1 N H2SO4, should
24、be neutralized with H2SO4 of higher concentration to limit theamount added to less than 1 mL. Before proceeding, make the solution just alkaline with 0.1 N NaOH solution. If the solution is3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For s
25、uggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Active Ingredien
26、t Level ExpectedActive Ingredient Level Expected, % Weight of Sample, g10 to 25 2025 to 40 1540 to 60 1060 to 80 7Over 80 5D2358 162acid originally, neutralize the free acid with alcoholic NaOH solution to the phenolphthalein end point. Decant the alcoholicsolution through a suitable filter, retaini
27、ng as much as possible of the insoluble matter in the beaker. Collect the clear filtrate ina suitable filter flask or beaker.6.4 Add 50 mL of hot 95 % alcohol to the residue in the beaker and bring to boiling on a safety hot plate. Let the insolublessettle and decant the alcoholic solution through t
28、he filter as before. Repeat the extraction of the insolubles with an additional 50mL of 95 % alcohol, retaining the bulk of the insolubles in the beaker.6.5 Evaporate the residual alcohol from the residue in the beaker on a steam bath, stirring at intervals to permit completeevaporation of the solve
29、nt. Dissolve the residue in the beaker in a minimum volume of hot water, not to exceed 10 mL, heatingon a steam bath to effect solution.6.6 Dilute the water solution with 200 mL of hot absolute alcohol. Bring to a boil on a steam bath and filter through thepreviously used filter, combining the filtr
30、ate with the initial alcoholic filtrate. Wash the beaker and residue several times with hot95 % alcohol, transferring the insolubles to the filter with several small portions of hot 95 % alcohol.6.7 Evaporate the combined alcoholic filtrate and washings to approximately 450 mLand transfer to a 500-m
31、Lvolumetric flask.Cool to room temperature and dilute to volume with 95 % alcohol. Mix well.6.8 Pipet a 100-mL aliquot into a tared flask and evaporate to dryness on a steam bath. Place in an oven maintained at 105 62C and dry for half-hour periods to constant weight.7. Calculation7.1 Calculate the
32、percentage of total alcohol-soluble matter as follows:Total alcohol2soluble matter,%5W 2T!/S# 3100 (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 SODIUM CHLORIDE CONTENT8. Procedure8.1 Pipet a suitable aliquot
33、from the solution as prepared in 7.76.7 into a 400-mL beaker. Evaporate to a volume of about 30mL and dilute to 100 mL with water.Add 2 drops of methyl orange indicator solution and acidify to the acid color by using HNO3(1+4). Warm slightly, stir, and add 50 mL of acetone. Follow the procedure for
34、quantitative determination, starting with 13.2 ofMethod D1681.9. Calculation9.1 Calculate the percentage of sodium chloride (NaCl) as follows:NaCl,%5B 3N 30.05845!/S# 3100 (2)where:B = millilitres of AgNO3 solution used,N = normality of the AgNO3 solution, andS = grams of sample in aliquot taken.TOT
35、ALACTIVE INGREDIENT10. Calculation10.1 Calculate the corrected alcohol-soluble matter, which is a measure of the total active ingredient, as follows:Alcohol2soluble matter,corrected,%5A 2C (3)where:A = percentage of total alcohol-soluble matter (Section 8), andC = percentage of NaCl (Section 10.).A
36、= percentage of total alcohol-soluble matter (Section 7), andC = percentage of NaCl (Section 9.).D2358 163PURIFICATION OF TOTALALCOHOL-SOLUBLE MATTER11. Reagent11.1 Acetone-Ether Mixture (1+1)Mix 1 part of acetone with 1 part of ether.12. Safety Precautions12.1 Acetone is a flammable solvent and a h
37、ealth hazard.This test should be performed in a well-ventilated explosion-proof areaand protective gloves and garments should be used.12.2 Ether is a skin, brain, and kidney irritant and an extreme fire and explosion hazard. All precautions should be taken toproceed with this test only in a special
38、explosion-proof area and under a special explosion-proof hood. Protective gloves andgarments should be used.NOTE 1See special instructions on manufacturers label for acetone and ether warning and disposal.13. Procedure13.1 To the dried residue from 7.86.8 add 50 mL of acetoneether mixture and warm o
39、n a steam bath.13.2 Agitate with a glass stirring rod and filter while warm through a general-purpose acid-washed filter paper. Collect thefiltrate in a small beaker. Wash the paper with a few small volumes of acetone-ether mixture.13.3 Evaporate the combined filtrate and washings on a steam bath. D
40、ry the residue in an oven at 105 6 2C.NOTE 2The evaporated fraction may be used for infrared spectrophotometric or qualitative examination. If the sample size is insufficientfor thesepurposes, a larger aliquot may be taken for evaporation.14. Keywords14.1 active ingredient; alcohol extraction; surfa
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