ASTM D2358-89(2003)
(Test Method)Standard Test Method for Separation of Active Ingredient from Surfactant and Syndet Compositions
Standard Test Method for Separation of Active Ingredient from Surfactant and Syndet Compositions
ABSTRACT
This test method covers the procedure for the separation and purification of active ingredient from surfactants and syndet compositions. The separated active ingredient may be used for qualitative examinations. The method also permits the estimation of total active ingredient level present in the sample under test. The method method yields the active ingredient together with other alcohol-soluble materials and therefore is useful only in estimating the actual active ingredient level.
SCOPE
1.1 This test method covers the procedure for the separation and purification of active ingredient from surfactants and syndet compositions. The separated active ingredient may be used for qualitative examinations. This test method also permits the estimation of total active ingredient level present in the sample under test.
1.2 This test method yields the active ingredient together with other alcohol-soluble materials and therefore is useful only in estimating the actual active ingredient level. Correction for the amount of the most common contaminant, sodium chloride, is shown by a separate determination.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.
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Designation:D2358–89(Reapproved 2003)
Standard Test Method for
Separation of Active Ingredient from Surfactant and Syndet
Compositions
This standard is issued under the fixed designation D2358; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope obtained. Provision is made for purification of the active
ingredients in Section 14.
1.1 This test method covers the procedure for the separation
and purification of active ingredient from surfactants and
4. Reagents
syndet compositions. The separated active ingredient may be
4.1 Purity of Reagents:
used for qualitative examinations. This test method also
4.1.1 Reagent grade chemicals shall be used in all tests.
permits the estimation of total active ingredient level present in
Unless otherwise indicated, it is intended that all reagents shall
the sample under test.
conform to the specifications of the Committee on Analytical
1.2 This test method yields the active ingredient together
Reagents of the American Chemical Society, where such
with other alcohol-soluble materials and therefore is useful
specifications are available. Other grades may be used, pro-
only in estimating the actual active ingredient level. Correction
vided it is first ascertained that the reagent is of sufficiently
for the amount of the most common contaminant, sodium
high purity to permit its use without lessening the accuracy of
chloride, is shown by a separate determination.
the determination.
1.3 This standard does not purport to address all of the
4.2 Unless otherwise indicated, references to water shall be
safety concerns, if any, associated with its use. It is the
understood to mean distilled water or water of equal purity.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
SEPARATION OFTOTALALCOHOL-SOLUBLE
bility of regulatory limitations prior to use. Material Safety
MATTER
Data Sheets are available for reagents and materials. Review
them for hazards prior to usage.
5. Reagents
5.1 Ethyl Alcohol (95 percent)—Freshly boiled ethyl alco-
2. Referenced Documents
hol conforming to Formula No. 3A or No. 30 of the U. S.
2.1 ASTM Standards:
Bureau of Internal Revenue. The alcohol should not be
D1681 TestMethodforSyntheticAnionicActiveIngredient
neutralized. Redistilled alcohol shall be used if alkali absorp-
in Detergents by Cationic Titration Procedure
tion is more than 0.2 mL of 0.1 N NaOH solution/100 mL of
alcohol.
3. Summary of Test Method
5.2 Ethyl Alcohol (Absolute)—Freshly boiled 200-proof
3.1 The test method involves the extraction of the active
ethyl alcohol conforming to either Formulas No. 3Aor No. 30
ingredient with alcohol. Reprecipitation of the insolubles is
of the U. S. Bureau of Internal Revenue.
specifiedtoremovethelasttracesofactiveingredient.Dilution
5.3 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
of the alcoholic extract to a known volume and the evaporation
1 g of phenolphthalein in 50 mL of ethyl alcohol (95 %) and
of a suitable aliquot permits measurement of total alcohol-
then mix with 50 mL of water.
soluble matter. An estimation of sodium chloride content is
5.4 Sulfuric Acid (1 + 100)—Add 1 mL of concentrated
made so that a corrected total active ingredient level may be
sulfuric acid (H SO , sp gr 1.84) to 100 mL of water.
2 4
This test method is under the jurisdiction of ASTM Committee D12 on Soaps
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Reagent Chemicals, American Chemical Society Specifications, American
Analysis of Soaps and Synthetic Detergents. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved May. 26, 1989. Published July 1989. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D2358 – 65 T. Last previous edition D2358 – 82 (1987). DOI: Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
10.1520/D2358-89R03. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.04. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2358–89 (2003)
6. Safety Precautions alcoholic filtrate. Wash the beaker and residue several times
with hot 95 % alcohol, transferring the insolubles to the filter
6.1 Formulas No. 3A and No. 30 ethyl alcohols are dena-
with several small portions of hot 95 % alcohol.
tured alcohols. They are health hazards and flammable liquids.
See manufacturer’s label warning as to use, safe handling, and 7.7 Evaporate the combined alcoholic filtrate and washings
disposal.
to approximately 450 mL and transfer to a 500-mL volumetric
6.2 Sulfuric acid is corrosive. Use proper protective equip-
flask. Cool to room temperature and dilute to volume with
ment including adequate eye protection. If acid contacts the
95 % alcohol. Mix well.
body or is splashed in the eyes, flush the affected parts with
7.8 Pipet a 100-mL aliquot into a tared flask and evaporate
water for at least 15 min. Obtain medical attention.
to dryness on a steam bath. Place in an oven maintained at 105
6 2°C and dry for half-hour periods to constant weight.
7. Procedure
7.1 Weigh out a sample, to the nearest 0.01 g, to correspond
8. Calculation
with the levels of active ingredient prescribed in Table 1 and
8.1 Calculate the percentage of total alcohol-soluble matter
transfer to a 600-mL beaker. Liquid samples containing high
as follows:
levels of water should be evaporated to a pasty consistency
after weighing. Samples containing high lev
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