ASTM D5352-95(2006)

Standard Test Method for Determination of Organically Combined Sulfuric Anhydride Ash-Gravimetric, Test Method C

SIGNIFICANCE AND USE
This test method is intended for the determination of organically combined sulfuric anhydride in sulfonated and sulfated fats and oils.
SCOPE
1.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfonated or sulfated oil, or both, by extracting the undecomposed sulfonated or sulfated fat and other fatty matter over an acidulated, concentrated salt solution, and ashing the purified extract. This test method is applicable to all types of sulfonated and sulfated oils, including true sulfonic acid oils and those containing sodium acetate or similar partially titratable compounds. This test method was derived from Test Methods D500, Sections 25 through 28.  
1.2 The values stated in SI units are to be regarded as the standard.  
1.3 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.

General Information

• Status: Historical
• Publication Date: 31-Mar-2006
• ICS: 71.080.01 - Organic chemicals in general
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5352-95(2001) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride Ash-Gravimetric, Test Method C
• Effective Date: 01-Apr-2006
• Replaced By: ASTM D5352-95(2012) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride Ash-Gravimetric, Test Method C
• Effective Date: 01-Apr-2012

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5352 – 95 (Reapproved 2006)
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 4.2 Hydrogen Peroxide (30 %)—Concentrated hydrogen
peroxide (H O ).
1.1 This test method covers the determination of the organi- 2 2
4.3 MethylOrangeIndicatorSolution(1g/L)—Dissolve0.1
cally combined sulfuric anhydride existing in a sample of
g of methyl orange in 100 mL of water.
sulfonated or sulfated oil, or both, by extracting the undecom-
4.4 Sodium Chloride (NaCl), solid.
posed sulfonated or sulfated fat and other fatty matter over an
4.5 Sodium Sulfate (Na SO ), anhydrous.
acidulated, concentrated salt solution, and ashing the purified 2 4
extract.This test method is applicable to all types of sulfonated
5. Procedure
and sulfated oils, including true sulfonic acid oils and those
5.1 The procedure consists of isolating and purifying the
containing sodium acetate or similar partially titratable com-
fatty matter as it exists in the original oil by dissolving the
pounds. This test method was derived from Test Methods
sample in a solvent, acidifying and washing with saturated
D500, Sections 25 through 28.
brine, and ashing the purified extract. If the sample contains
1.2 The values stated in SI units are to be regarded as the
ammonia, the ammonia shall first be expelled before the
standard.
determination is made on the sample.
1.3 This standard does not purport to address all of the
5.1.1 In the Absence of Ammonia—Proceed as described in
safety concerns, if any, associated with its use. It is the
the separation of purified oil (6.1.1 Method B), combining the
responsibility of the user of this standard to establish appro-
ether layers in the first funnel rather than in the decomposition
priate safety and health practices and determine the applica-
flask. Carefully remove any water that may settle and dehy-
bility of regulatory limitations prior to use.
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
beaker placed in a bath of warm water.Wash the flask and filter
2.1 ASTM Standards:
with ether until free from fat (absence of oil stains on the filter
D500 TestMethodsofChemicalAnalysisofSulfonatedand
paper after drying) and add the filtrate to the beaker. To avoid
Sulfated Oils
creeping of the oil, the volume in the beaker should at no time
3. Significance and Use
during the filtering and washing exceed 50 mL(one third full).
Evaporate the ether solution until the volume has been reduced
3.1 This test method is intended for the determination of
to about 20 mL and transfer the residue to a tared 50-mL
organically combined sulfuric anhydride in sulfonated and
crucible (high form). Immerse the crucible in a 100-mLbeaker
sulfated fats and oils.
containing warm water until practically all of the ether has
4. Reagents
evaporated. Rinse the beaker with two 10-mL and three 5-mL
portions of ether, or until all of the oil has been transferred to
4.1 Ethyl Ether.
the crucible; allow each portion of rinsing ether to evaporate
before the next rinsing is made. Burn gently the solvent-free
residue, and finally ignite
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