ASTM D5352-95(2012)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5352 − 95 (Reapproved 2012)
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 ).
2 2
1.1 This test method covers the determination of the organi-
cally combined sulfuric anhydride existing in a sample of
4.3 MethylOrangeIndicatorSolution(1g/L)—Dissolve 0.1
sulfonated or sulfated oil, or both, by extracting the undecom-
g of methyl orange in 100 mL of water.
posed sulfonated or sulfated fat and other fatty matter over an
4.4 Sodium Chloride (NaCl), solid.
acidulated, concentrated salt solution, and ashing the purified
extract.This test method is applicable to all types of sulfonated 4.5 Sodium Sulfate (Na SO ), anhydrous.
2 4
and sulfated oils, including true sulfonic acid oils and those
containing sodium acetate or similar partially titratable com- 5. Procedure
pounds. This test method was derived from Test Methods
5.1 The procedure consists of isolating and purifying the
D500, Sections 25 through 28.
fatty matter as it exists in the original oil by dissolving the
1.2 The values stated in SI units are to be regarded as
sample in a solvent, acidifying and washing with saturated
standard. No other units of measurement are included in this
brine, and ashing the purified extract. If the sample contains
standard.
ammonia, the ammonia shall first be expelled before the
determination is made on the sample.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 5.1.1 In the Absence of Ammonia—Proceed as described in
the separation of purified oil (6.1.1 Method B), combining the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- ether layers in the first funnel rather than in the decomposition
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
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
3. Significance and Use
during the filtering and washing exceed 50 mL(one third full).
3.1 This test method is intended for the determination of Evaporate the ether solution until the volume has been reduced
organically combined sulfuric anhydride in sulfonated and
to about 20 mL and transfer the residue to a tared 50-mL
sulfated fats and oils. crucible (high form). Immerse the crucible in a 100-mLbeaker
containing warm water until practically all of the ether has
4. Reagents
evaporated. Rinse the beaker with two 10-mL and three 5-mL
4.1 Ethyl Ether. portions of ether, or until all of the oil has been transferred to
the crucible; allow each portion of rinsing ether to evaporate
1 before the next rinsing is made. Burn gently the solvent-free
This test method is under the jurisdiction ofAST
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