ASTM D5352-95(2001)

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

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-Dec-1994
• ICS: 71.080.01 - Organic chemicals in general
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5352-95 - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride Ash-Gravimetric, Test Method C
• Effective Date: 01-Jan-1995
• Replaced By: ASTM D5352-95(2006) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride Ash-Gravimetric, Test Method C
• Effective Date: 01-Apr-2006

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 5352 – 95 (Reapproved 2001)
Standard Test Method for
Determination of Organically Combined Sulfuric Anhydride
Ash-Gravimetric, Test Method C
This standard is issued under the fixed designation D 5352; 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 4.4 Sodium Chloride (NaCl), solid.
4.5 Sodium Sulfate (Na SO ), anhydrous.
1.1 This test method covers the determination of the organi- 2 4
cally combined sulfuric anhydride existing in a sample of
5. Procedure
sulfonated or sulfated oil, or both, by extracting the undecom-
5.1 The procedure consists of isolating and purifying the
posed sulfonated or sulfated fat and other fatty matter over an
fatty matter as it exists in the original oil by dissolving the
acidulated, concentrated salt solution, and ashing the purified
sample in a solvent, acidifying and washing with saturated
extract.This test method is applicable to all types of sulfonated
brine, and ashing the purified extract. If the sample contains
and sulfated oils, including true sulfonic acid oils and those
ammonia, the ammonia shall first be expelled before the
containing sodium acetate or similar partially titratable com-
determination is made on the sample.
pounds. This test method was derived from Test Methods
5.1.1 In the Absence of Ammonia—Proceed as described in
D 500, Sections 25 through 28.
the separation of purified oil (6.1.1 Method B), combining the
1.2 The values stated in SI units are to be regarded as the
ether layers in the first funnel rather than in the decomposition
standard.
flask. Carefully remove any water that may settle and dehy-
1.3 This standard does not purport to address all of the
drate the ether layer as follows: add5gof anhydrous Na SO ,
2 4
safety concerns, if any, associated with its use. It is the
shake vigorously for 5 min, and filter directly into a 150-mL
responsibility of the user of this standard to establish appro-
beaker placed in a bath of warm water.Wash the flask and filter
priate safety and health practices and determine the applica-
with ether until free from fat (absence of oil stains on the filter
bility of regulatory limitations prior to use.
paper after drying) and add the filtrate to the beaker. To avoid
2. Referenced Documents creeping of the oil, the volume in the beaker should at no time
during the filtering and washing exceed 50 mL(one third full).
2.1 ASTM Standards:
Evaporate the ether solution until the volume has been reduced
D 500 Test Methods of Chemical Analysis of Sulfonated
to about 20 mL and transfer the residue to a tared 50-mL
and Sulfated Oils
crucible (high form). Immerse the crucible in a 100-mLbeaker
3. Significance and Use
containing warm water until practically all of the ether has
evaporated. Rinse the beaker with two 10-mL and three 5-mL
3.1 This test method is intended for the determination of
portions of ether, or until all of the oil has been transferred to
organically combined sulfuric anhydride in sulfonated and
the crucible; allow each portion of rinsing ether to evaporate
sulfated fats and oils.
before the next rinsing is made. Burn gently the solvent-free
4. Reagents
residue, and finally ignite at a dull red heat to constant weight.
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