ASTM D5352-95

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
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaced By: ASTM D5352-95(2001) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride Ash-Gravimetric, Test Method C
• Effective Date: 01-Jan-1995

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.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