ASTM D3049-89(2016)
(Test Method)Standard Test Method for Synthetic Anionic Ingredient by Cationic Titration
Standard Test Method for Synthetic Anionic Ingredient by Cationic Titration
SIGNIFICANCE AND USE
4.1 This test method offers a means of determining anionic detergents commonly found in laundry, dishwashing, and other cleaning materials. Accurate determination of the anionic active substance is highly important in assessing the cost and effectiveness of such cleaning substances.
4.2 This test method is not affected by low molecular weight sulfonates, such as those of toluene and xylene commonly found in detergent formulations, when these substances are present up to 15 weight % of active material.
SCOPE
1.1 This test method covers the determination of the amount of synthetic anionic ingredient in a surfactant by direct titration with a standardized cationic reagent. The test method is a simple and convenient means for the quantitative estimation of the anionic material. The end point is detected by the transfer of a colored complex from an organic solvent phase to an aqueous phase. The colored complex is formed by the addition of a solution of dye to a solution of the anionic surfactant. This complex is soluble in the organic-solvent phase and insoluble in the aqueous phase. When this solution is titrated with a standardized solution of a cationic reagent, the dye is displaced from the colored complex and, being water-soluble, migrates to the aqueous phase. Therefore, a cationic titrating solution that has been standardized against a characterized anionic agent can be used to analyze for other anionics of known molecular mass.
1.2 This test method is applicable to alkylaryl sulfonates, alkyl sulfonates, alkyl sulfates and hydroxy-sulfates, alkylphenol- and fatty alcohol ethoxy-sulfates and dialkylsulfosuccinates. It applies to active materials containing one hydrophilic group per molecule.
1.3 The analytical procedures appear in the following order:
Sections
Reagents
6
Primary Standard
8
Purity
8.2
Alcohols
8.3
Free Acid or Alkali
8.4
Preparation of Mixed Indicator Solution
9
Preparation of Hyamine Solution
10
Standardization of Hyamine Solution
11
General Procedure for Anionic-Active Material
12
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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. A precautionary statement appears in Section 7. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.
General Information
Relations
Standards Content (Sample)
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.
Designation: D3049 − 89 (Reapproved 2016)
Standard Test Method for
1
Synthetic Anionic Ingredient by Cationic Titration
This standard is issued under the fixed designation D3049; 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 responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 Thistestmethodcoversthedeterminationoftheamount
bility of regulatory limitations prior to use. A precautionary
ofsyntheticanionicingredientinasurfactantbydirecttitration
statementappearsinSection7.MaterialSafetyDataSheetsare
with a standardized cationic reagent. The test method is a
available for reagents and materials. Review them for hazards
simple and convenient means for the quantitative estimation of
prior to usage.
the anionic material. The end point is detected by the transfer
of a colored complex from an organic solvent phase to an
2. Referenced Documents
aqueous phase. The colored complex is formed by the addition
2.1 ASTM Standards:
of a solution of dye to a solution of the anionic surfactant.This
2
complex is soluble in the organic-solvent phase and insoluble D1193 Specification for Reagent Water
in the aqueous phase. When this solution is titrated with a
3. Summary of Test Method
standardized solution of a cationic reagent, the dye is displaced
fromthecoloredcomplexand,beingwater-soluble,migratesto
3.1 An aqueous solution of an anionic-type detergent, to
the aqueous phase. Therefore, a cationic titrating solution that
which is added a small amount of mixed indicator (dimidium
hasbeenstandardizedagainstacharacterizedanionicagentcan
bromideanddisulphineblue),isshakenwithaqueousHyamine
beusedtoanalyzeforotheranionicsofknownmolecularmass.
solutionandchloroform.Thepinkcomplexwhichisformedby
thereactionbetweentheanionicdetergentandthecationicdye,
1.2 This test method is applicable to alkylaryl sulfonates,
dimidium bromide, is extracted into the chloroform. Incre-
alkyl sulfonates, alkyl sulfates and hydroxy-sulfates,
ments of additional Hyamine solution are added with a
alkylphenol- and fatty alcohol ethoxy-sulfates and dialkylsul-
thorough mixing after each addition.At first the reaction takes
fosuccinates. It applies to active materials containing one
place between the Hyamine and the excess anionic-type
hydrophilic group per molecule.
detergent, during which there is no noticeable change in the
1.3 The analytical procedures appear in the following order:
color (pink) of the chloroform phase.As the equivalence point
Sections
between the anionic and cationic materials is approached, the
Reagents 6
dimidium bromide portion of the anionic detergent active-
Primary Standard 8
Purity 8.2
dimidium bromide complex (pink) is gradually released and
Alcohols 8.3
transferred to the aqueous layer.As excess Hyamine is added it
Free Acid or Alkali 8.4
reacts with the anionic dye, disulphine blue, to form a
Preparation of Mixed Indicator Solution 9
Preparation of Hyamine Solution 10
chloroform-soluble blue complex. During the transition at the
Standardization of Hyamine Solution 11
end point the chloroform layer, therefore, changes from pink to
General Procedure for Anionic-Active Material 12
gray, to blue. The gray color is taken as the end point.
1.4 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Significance and Use
standard.The values stated in SI units are to be regarded as
4.1 This test method offers a means of determining anionic
standard. No other units of measurement are included in this
detergents commonly found in laundry, dishwashing, and other
standard.
cleaning materials. Accurate determination of the anionic
1.5 This standard does not purport to address all of the
active substance is highly important in assessing the cost and
safety concerns, if any, associated with its use. It is the
effectiveness of such cleaning substances.
1
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
2
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2016. Published August 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1972 as D3049– 72 T. La
...
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