ASTM D5352-95(2019)

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: D5352 − 95 (Reapproved 2019)
Standard Test Method for
Determination of Organically Combined Sulfuric Anhydride
Ash-Gravimetric, Test Method C
This standard is issued under the fixed designation D5352; 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 3. Significance and Use
3.1 This test method is intended for the determination of
1.1 This test method covers the determination of the organi-
organically combined sulfuric anhydride in sulfonated and
cally combined sulfuric anhydride existing in a sample of
sulfated fats and oils.
sulfonated or sulfated oil, or both, by extracting the undecom-
posed sulfonated or sulfated fat and other fatty matter over an
4. Reagents
acidulated, concentrated salt solution, and ashing the purified
extract.This test method is applicable to all types of sulfonated 4.1 Ethyl Ether.
and sulfated oils, including true sulfonic acid oils and those
4.2 Hydrogen Peroxide (30 %)—Concentrated hydrogen
containing sodium acetate or similar partially titratable com-
peroxide (H O ).
2 2
pounds. This test method was derived from Test Methods
4.3 MethylOrangeIndicatorSolution(1g/L)—Dissolve 0.1
D500, Sections 25 through 28.
g of methyl orange in 100 mL of water.
1.2 The values stated in SI units are to be regarded as
4.4 Sodium Chloride (NaCl), solid.
standard. No other units of measurement are included in this
standard. 4.5 Sodium Sulfate (Na SO ), anhydrous.
2 4
1.3 This standard does not purport to address all of the
5. Procedure
safety concerns, if any, associated with its use. It is the
5.1 The procedure consists of isolating and purifying the
responsibility of the user of this standard to establish appro-
fatty matter as it exists in the original oil by dissolving the
priate safety, health, and environmental practices and deter-
sample in a solvent, acidifying and washing with saturated
mine the applicability of regulatory limitations prior to use.
brine, and ashing the purified extract. If the sample contains
1.4 This international standard was developed in accor-
ammonia, the ammonia shall first be expelled before the
dance with internationally recognized principles on standard-
determination is made on the sample.
ization established in the Decision on Principles for the
5.1.1 In the Absence of Ammonia—Proceed as described in
Development of International Standards, Guides and Recom-
the separation of purified oil (6.1.1 Method B), combining the
mendations issued by the World Trade Organization Technical
ether layers in the first funnel rather than in the decomposition
Barriers to Trade (TBT) Committee.
flask. Carefully remove any water that may settle and dehy-
drate the ether layer as follows: add5gof anhydrous Na SO ,
2 4
2. Referenced Documents
shake vigorously for 5 min, and filter directly into a 150-mL
2.1 ASTM Standards:
beaker placed in a bath of warm water.Wash the flask and filter
D500 Test Methods of ChemicalAnalysis of Sulfonated and
with ether until free from fat (absence of oil stains on the filter
Sulfated Oils
paper after drying) and add the filtrate to the beaker. To avoid
creeping of the oil, the volume in the beaker should at no time
during the filtering and washing exceed 50 mL(one third full).
1 Evaporate the ether solution until the volume has been reduced
This test method is under the jurisdiction ofASTM Committee D31 on Leather
and is the direct responsibility of Subcommittee D31.08 on Fats and OilsThis test
to about 20 mL and transfer the residue to a tared 50-mL
method was developed in cooperation with the Ameri
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