ASTM D6174-01
(Test Method)Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration
Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration
SCOPE
1.1 This test method describes a potentiometric titration procedure for determining the inorganic sulfate content of surfactants. It is intended for the analysis of α olefin sulfonates, alkane sulfonates, alcohol sulfates, alcohol ether sulfates, alkylbenzenesulfonates, and the like.
1.2 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: D 6174 – 01
Standard Test Method for
Inorganic Sulfate in Surfactants by Potentiometric Lead
1
Titration
This standard is issued under the fixed designation D 6174; 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.
1. Scope forusedependsontheirpurity.Sulfatecontent,asmeasuredby
this test method, can be used to estimate the purity of an
1.1 This test method describes a potentiometric titration
anionic surfactant under test.
procedure for determining the inorganic sulfate content of
surfactants. It is intended for the analysis of a-olefin sul-
6. Apparatus
fonates, alkane sulfonates, alcohol sulfates, alcohol ether
6.1 Potentiometric Titration Assembly, consisting of an
sulfates, alkylbenzenesulfonates, and the like.
automatic titrator fitted with a lead ion-selective electrode, a
1.2 This standard does not purport to address all of the
double-junction reference electrode, and a 10-mL buret. The
safety concerns, if any, associated with its use. It is the
reference electrode should be filled with the standard inner and
responsibility of the user of this standard to establish appro-
outer filling solutions supplied with it. A TFE-fluorocarbon-
priate safety and health practices and determine the applica-
coated magnetic stirring bar should be used for mixing during
bility of regulatory limitations prior to use. Material Safety
titration, with a separate magnetic stirring motor if the autoti-
Data Sheets are available for reagents and materials. Review
trator is not so equipped.
them for hazards prior to usage.
NOTE 1—Proper care of the lead-selective electrode is essential for
2. Referenced Documents
obtaining high-quality titration curves. Follow manufacturer’s instruc-
tions.
2.1 ASTM Standards:
2
D 1193 Specification for Reagent Water
7. Reagents
3. Terminology
7.1 Glacial Acetic Acid.
7.2 Lead Nitrate, reagent grade.
3.1 Definitions of Terms Specific to This Standard:
7.3 Sodium Sulfate, anhydrous, reagent grade.
3.1.1 inorganic sulfate, n—sulfate species present as sulfu-
7.4 Sodium Perchlorate, reagent grade.
ric acid, ionic salts of this acid, or mixtures of these.
7.5 Ethanol, denatured, formula 3A.
4. Summary of Test Method
7.6 Water, Type III reagent water conforming to Specifica-
3
tion D 1193.
4.1 A surfactant sample containing inorganic sulfate is
titrated in ethanolic medium with a standard lead solution.
8. Preparation of Standard Solutions
Lead sulfate precipitate is formed during the titration. Ethanol
8.1 10 % Acetic Acid—Dilute glacial acetic acid 1/10 with
and sodium perchlorate are present to decrease the solubility of
water.
lead sulfate, thus sharpening the endpoint.Acetic acid is added
8.2 Lead Titrant, 0.05 M—Dissolve 16.6 g lead nitrate in
to remove possible interference from carbonate. The endpoint
300 mL water. Pour into a 1-L bottle and fill with 3A ethanol.
is signaled by an increase in lead ion activity, as measured by
Mix well. Standardize according to 9.1.
a lead-selective electrode.
8.3 Sulfate Standard, 0.05 M—Dry 5 g anhydrous sodium
5. Significance and Use
sulfate at 110°C for 1 h. Accurately weigh about 3.5 g into a
500-mLvolumetric flask, dilute to volume with water, and mix
5.1 Anionic surfactants, such as those listed in 1.1, com-
to dissolve. Calculate the exact concentration as follows:
monly are used in detergent formulations. Their acceptability
1 3
This test method is under the jurisdiction of ASTM Committee D12 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 Aug. 10, 2001. Published October 2001. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 6174-97. Last previous edition D 6174-97. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
2
Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D 6174
G
10.2 Transfer a portion of test surfactant, equivalent to
5 Molarity (1)
142.02! 0.500!
~ ~
30–50 mg sodium sulfate, to a 50-mL beaker. For example, if
a surfactant is expected to contain 1 % sodium sulfate, weigh
where:
3–5 g to analytical precision into the beaker, or an equivalent
G
...
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