ASTM D2358-89(2009)

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 The values stated in SI units are to be regarded as standard. No other units of 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 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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2009
• ICS: 71.100.40 - Surface active agents
• Technical Committee: D12 - Soaps and Other Detergents
• Drafting Committee: D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components

Relations

• Replaces: ASTM D2358-89(2003) - Standard Test Method for Separation of Active Ingredient from Surfactant and Syndet Compositions
• Effective Date: 01-Oct-2009
• Replaced By: ASTM D2358-16 - Standard Test Method for Separation of Active Ingredient from Surfactant and Syndet Compositions
• Effective Date: 01-Jul-2016
• Referred By: ASTM D2959-95(2017) - Standard Test Method for Ethylene Oxide Content of Polyethoxylated Nonionic Surfactants
• Effective Date: 01-Oct-2009
• Referred By: ASTM D820-93(2023) - Standard Test Methods for Chemical Analysis of Soaps Containing Synthetic Detergents
• Effective Date: 01-Oct-2009

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D2358 − 89 (Reapproved2009)
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 of the alcoholic extract to a known volume and the evaporation
of a suitable aliquot permits measurement of total alcohol-
1.1 This test method covers the procedure for the separation
soluble matter. An estimation of sodium chloride content is
and purification of active ingredient from surfactants and
made so that a corrected total active ingredient level may be
syndet compositions. The separated active ingredient may be
obtained. Provision is made for purification of the active
used for qualitative examinations. This test method also
ingredients in Section 14.
permits the estimation of total active ingredient level present in
the sample under test.
4. Reagents
1.2 This test method yields the active ingredient together
4.1 Purity of Reagents:
with other alcohol-soluble materials and therefore is useful
4.1.1 Reagent grade chemicals shall be used in all tests.
only in estimating the actual active ingredient level. Correction
Unless otherwise indicated, it is intended that all reagents shall
for the amount of the most common contaminant, sodium
conform to the specifications of the Committee on Analytical
chloride, is shown by a separate determination.
Reagents of the American Chemical Society, where such
1.3 The values stated in SI units are to be regarded as
specifications are available. Other grades may be used, pro-
standard. No other units of measurement are included in this
vided it is first ascertained that the reagent is of sufficiently
standard.
high purity to permit its use without lessening the accuracy of
the determination.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.2 Unless otherwise indicated, references to water shall be
responsibility of the user of this standard to establish appro-
understood to mean distilled water or water of equal purity.
priate safety and health practices and determine the applica-
SEPARATION OF TOTAL ALCOHOL-SOLUBLE
bility of regulatory limitations prior to use. Material Safety
Data Sheets are available for reagents and materials. Review MATTER
them for hazards prior to usage.
5. Reagents
2. Referenced Documents
5.1 Ethyl Alcohol (95 percent)—Freshlyboiledethylalcohol
2.1 ASTM Standards:
conforming to Formula No. 3A or No. 30 of the U. S. Bureau
D1681 Test Method for SyntheticAnionicActive Ingredient
of Internal Revenue. The alcohol should not be neutralized.
in Detergents by Cationic Titration Procedure
Redistilled alcohol shall be used if alkali absorption 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
1 g of phenolphthalein in 50 mL of ethyl alcohol (95 %) and
This test method is under the jurisdiction of ASTM Committee D12 on Soaps
then mix with 50 mL of water.
and Other Detergents and is the direct responsibility of Subcommittee D12.12 on
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components.
Current edition approved Oct. 1, 2009. Published December 2009. Originally
approved in 1965 as D2358 – 65 T. Last previous edition approved in 2003 as Reagent Chemicals, American Chemical Society Specifications, American
D2358 – 89 (2003). DOI: 10.1520/D2358-89R09. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
For referenced ASTM standards, visit the ASTM website, www.astm.org, or listed by the American Chemical Society, see Analar Standards for Laboratory
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards volume information, refer to the standard’s Document Summary page on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
the ASTM website. MD.
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D2358 − 89 (2009)
5.4 Sulfuric Acid (1 + 100)—Add 1 mL of concentrated a minimum volume of hot water, not to exceed 10 mL, heating
sulfuric acid (H SO , sp gr 1.84) to 100 mL of water. on a steam bath to effect solution.
2 4
7.6 Dilute the water solution with 200 mL of hot absolute
6. Safety Precautions
alcohol. Bring to a boil on a steam bath and filter through the
6.1 Formulas No. 3A and No. 30 ethyl alcohols are dena-
previously used filter, combining the filtrate with the initial
tured alcohols. They are health hazards and flammable liquids.
alcoholic filtrate. Wash the beaker and residue several times
See manufacturer’s label warning as to use, safe handling, and
with hot 95 % alcohol, transferring the insolubles to the filter
disposal.
with several small portions of hot 95 % alcohol.
6.2 Sulfuric acid is corrosive. Use proper protective equip-
7.7 Evaporate the combined alcoholic filtrate and washings
ment including adequate eye protection. If acid contacts the
to approximately 450 mL and transfer to a 500-mL volumetric
body or is splashed in the eyes, flush the affected parts with
flask. Cool to room temperature and dilute to volume with
water for at least 15 min. Obtain medical attention.
95 % alcohol. Mix well.
7.8 Pipet a 100-mL aliquot into a tared flask and evaporate
7. Procedure
to dryness on a steam bath. Place in an oven maintained at 105
7.1 Weigh ou
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