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ASTM D6174-97

(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.

General Information

Status
Historical
Publication Date
09-Aug-2001
ICS
71.040.40 - Chemical analysis
Technical Committee
D12 - Soaps and Other Detergents
Drafting Committee
D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components
Current Stage
Ref Project

Relations

Replaced By
ASTM D6174-01 - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration
Effective Date
10-Aug-2001

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ASTM D6174-97 - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead TitrationASTM D6174-97 - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration
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ASTM D6174-97 - Standard Test Method for Inorganic Sulfate in Surfactants by Potentiometric Lead Titration
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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: D 6174 – 97
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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 6. Apparatus
1.1 This test method describes a potentiometric titration 6.1 Potentiometric Titration Assembly, consisting of an
procedure for determining the inorganic sulfate content of automatic titrator fitted with a lead ion-selective electrode, a
surfactants. It is intended for the analysis of a-olefin sul- double-junction reference electrode, and a 10-mL buret. The
fonates, alcohol sulfates, alcohol ether sulfates, alkylbenzene- reference electrode should be filled with the standard inner and
sulfonates, and the like. outer filling solutions supplied with it. A TFE-fluorocarbon-
1.2 This standard does not purport to address all of the coated magnetic stirring bar should be used for mixing during
safety concerns, if any, associated with its use. It is the titration, with a separate magnetic stirring motor if the autoti-
responsibility of the user of this standard to establish appro- trator is not so equipped.
priate safety and health practices and determine the applica-
NOTE 1—Proper care of the lead-selective electrode is essential for
bility of regulatory limitations prior to use. Material Safety
obtaining high-quality titration curves. Follow manufacturer’s instruc-
Data Sheets are available for reagents and materials. Review
tions.
them for hazards prior to usage.
7. Reagents
2. Referenced Documents
7.1 Glacial Acetic Acid.
2.1 ASTM Standards:
7.2 Lead Nitrate, reagent grade.
2
D 1193 Specification for Reagent Water
7.3 Sodium Sulfate, anhydrous, reagent grade.
7.4 Sodium Perchlorate, reagent grade.
3. Terminology
7.5 Ethanol, denatured, formula 3A.
3.1 Definitions of Terms Specific to This Standard:
7.6 Water, Type III reagent water conforming to Specifica-
3.1.1 inorganic sulfate, n—sulfate species present as sulfu- 3
tion D 1193.
ric acid, ionic salts of this acid, or mixtures of these.
8. Preparation of Standard Solutions
4. Summary of Test Method
8.1 10 % Acetic Acid—Dilute glacial acetic acid 1/10 with
4.1 A surfactant sample containing inorganic sulfate is
water.
titrated in ethanolic medium with a standard lead solution.
8.2 Lead Titrant, 0.05 M—Dissolve 16.6 g lead nitrate in
Lead sulfate precipitate is formed during the titration. Ethanol
300 mL water. Pour into a 1-L bottle and fill with 3A ethanol.
and sodium perchlorate are present to decrease the solubility of
Mix well. Standardize according to 9.1.
lead sulfate, thus sharpening the endpoint. Acetic acid is added
8.3 Sulfate Standard, 0.05 M—Dry 5 g anhydrous sodium
to remove possible interference from carbonate. The endpoint
sulfate at 110°C for 1 h. Accurately weigh about 3.5 g into a
is signaled by an increase in lead ion activity, as measured by
500-mL volumetric flask, dilute to volume with water, and mix
a lead-selective electrode.
to dissolve. Calculate the exact concentration as follows:
5. Significance and Use G
5 Molarity (1)
~142.02!~0.500!
5.1 Anionic surfactants, such as those listed in 1.1, com-
monly are used in detergent formulations. Their acceptability
where:
for use depends on their purity. Sulfate content, as measured by
this test method, can be used to estimate the purity of an
anionic surfactant under test.
3
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
1
This test method is under the jurisdiction of ASTM Committee D12 on Soaps listed by the American Chemical Society, see Analar Standards for Laboratory
and Detergents and is the direct responsibility of Subcommittee D12.12 on Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Current edition approved Sept. 10, 1997. Published April 1998. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
2
Annual Book of ASTM Standards, Vol 11.01. MD.
1

---------------------- Page: 1 ----------------------
D 6174
sodium perchlorate and approximately 1 mL 10 % acetic acid.
G 5 weight in grams of Na SO dissolved in the 500 mL
2 4
Prepare the autotitrator for operation, immerse the electrodes in
and 142.02 is its gram molecular weight.
the titration solution, and titrate to the potentiometric endpoint
8.4 Ethanolic Sodium Perchlorate, 0.05
...

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1.2 The values stated in SI units are to be regarded as standard.  
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5.2 As stated in 1.2, this test method uses a weaker acid to titrate the base than Test Method D2896, and the titration solvents are also different. Test Method D2896 uses a stronger acid and a more polar solvent system than Test Method D4739. As a result, Test Method D2896 will titrate salts of weak acids (soaps), basic salts of polyacidic bases, and weak alkaline salts of some metals. They do not protect the oil from acidic components due to the degradation of the oil. This test method may produce a falsely exaggerated base number. Test Method D4739 will probably not titrate these weak bases but, if so, will titrate them to a lesser degree of completion. It measures only the basic components of the additive package that neutralizes acids. On the other hand, if the additive package contains weak basic components that do not play a role in neutralizing the acidic components of the degrading oil, then the Test Method D4739 result may be falsely understated.  
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1.4 This test method was developed as an alternative for the former base numb...

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1.2 This test method can be used to indicate relative changes that occur in an oil during use under oxidizing conditions. Although the test is performed under closely specified conditions with standardized reagents, the test method does not measure an absolute basic property that can be used to predict performance of an oil under service conditions. No general relationship between bearing corrosion and base number is known.  
1.3 The values stated in SI units are to be regarded as the standard.  
1.3.1 Exception—The values given in parentheses are for information only.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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