ASTM D2358-89(1995)e1

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
e1
Designation: D 2358 – 89 (Reapproved 1995)
Standard Test Method for
Separation of Active Ingredient from Surfactant and Syndet
Compositions
This standard is issued under the fixed designation D 2358; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Keywords were added editorially in February 1995.
1. Scope ingredients in Section 14.
1.1 This test method covers the procedure for the separation
4. Reagents
and purification of active ingredient from surfactants and
4.1 Purity of Reagents:
syndet compositions. The separated active ingredient may be
4.1.1 Reagent grade chemicals shall be used in all tests.
used for qualitative examinations. This test method also
Unless otherwise indicated, it is intended that all reagents shall
permits the estimation of total active ingredient level present in
conform to the specifications of the Committee on Analytical
the sample under test.
Reagents of the American Chemical Society, where such
1.2 This test method yields the active ingredient together
specifications are available. Other grades may be used, pro-
with other alcohol-soluble materials and therefore is useful
vided it is first ascertained that the reagent is of sufficiently
only in estimating the actual active ingredient level. Correction
high purity to permit its use without lessening the accuracy of
for the amount of the most common contaminant, sodium
the determination.
chloride, is shown by a separate determination.
4.2 Unless otherwise indicated, references to water shall be
1.3 This standard does not purport to address all of the
understood to mean distilled water or water of equal purity.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
SEPARATION OF TOTAL ALCOHOL-SOLUBLE
priate safety and health practices and determine the applica-
MATTER
bility of regulatory limitations prior to use. Material Safety
Data Sheets are available for reagents and materials. Review
5. Reagents
them for hazards prior to usage.
5.1 Ethyl Alcohol (95 percent)—Freshly boiled ethyl alco-
hol conforming to Formula No. 3A or No. 30 of the U. S.
2. Referenced Documents
Bureau of Internal Revenue. The alcohol should not be
2.1 ASTM Standards:
neutralized. Redistilled alcohol shall be used if alkali absorp-
D 1681 Test Method for Synthetic Anionic Active Ingredi-
tion is more than 0.2 mL of 0.1 N NaOH solution/100 mL of
ent in Detergents by Cationic Titration Procedure
alcohol.
5.2 Ethyl Alcohol (Absolute)—Freshly boiled 200-proof
3. Summary of Test Method
ethyl alcohol conforming to either Formulas No. 3A or No. 30
3.1 The test method involves the extraction of the active
of the U. S. Bureau of Internal Revenue.
ingredient with alcohol. Reprecipitation of the insolubles is
5.3 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
specified to remove the last traces of active ingredient. Dilution
1 g of phenolphthalein in 50 mL of ethyl alcohol (95 %) and
of the alcoholic extract to a known volume and the evaporation
then mix with 50 mL of water.
of a suitable aliquot permits measurement of total alcohol-
5.4 Sulfuric Acid (1 + 100)—Add 1 mL of concentrated
soluble matter. An estimation of sodium chloride content is
sulfuric acid (H SO , sp gr 1.84) to 100 mL of water.
2 4
made so that a corrected total active ingredient level may be
obtained. Provision is made for purification of the active
1 3
This test method is under the jurisdiction of ASTM Committee D-12 on Soaps Reagent Chemicals, American Chemical Society Specifications, American
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Analysis of Soaps and Synthetic Detergents. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved May. 26, 1989. Published July 1989. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 2358 – 65 T. Last previous edition D 2358 – 82 (1987). and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.04. MD.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 2358
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.
7.7 Evaporate the combined alcoholic filtrate and washings
See manufacturer’s label warning as to use, safe handling, and
to approximately 450 mL and transfer to a 500-mL volumetric
disposal.
flask. Cool to room temperature and dilute to volume with
6.2 Sulfuric acid is corrosive. Use proper protective equip-
95 % alcohol. Mix well.
ment including adequate eye protection. If acid contacts the
7.8 Pipet a 100-mL aliquot into a tared flask and evaporate
body or is splashed in the eyes, flush the affected parts with
to dryness on a steam bath. Place in an oven maintained at 105
water for at least 15 min. Obtain medical attention.
6 2°C and dry for half-hour periods to constant weight.
7. Procedure
8. Calculation
7.1 Weigh out a sample, to the nearest 0.01 g, to correspond
8.1 Calculate the percentage of total alcohol-soluble matter
with the levels of active ingredient prescribed in Table 1 and
as follows:
transfer to a 600-mL beaker. Liquid samples containing high
levels of water should be evaporated to a pasty consistency Total alcohol2soluble matter, % 5 @~W 2 T!/S#3 100 (1
...