ASTM D5553-95(2006)
(Test Method)Standard Test Method for Determination of the Unsaponifiable Nonvolatile Matter in Sulfated Oils
Standard Test Method for Determination of the Unsaponifiable Nonvolatile Matter in Sulfated Oils
SIGNIFICANCE AND USE
This test method is intended for use in the determination of the unsaponifiable, nonvolatile matter contained in sulfated oils for the purpose of quality assurance.
SCOPE
1.1 This test method covers the determination of the unsaponifiable, nonvolatile (above 80°C) matter existing in a sample of sulfated oil by saponifying the desulfated fatty matter and extracting the unsaponifiable matter, and extracting the unsaponifiable matter from the soap solution with ethyl ether.
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
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5553 – 95 (Reapproved 2006)
Standard Test Method for
Determination of the Unsaponifiable Nonvolatile Matter in
Sulfated Oils
This standard is issued under the fixed designation D5553; 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. Apparatus and Reagents
1.1 This test method covers the determination of the unsa- 4.1 Saponification Flask—The apparatus required for the
ponifiable, nonvolatile (above 80°C) matter existing in a saponification consists of a glass flask provided with an air
sample of sulfated oil by saponifying the desulfated fatty condenser.
matter and extracting the unsaponifiable matter, and extracting 4.2 Ethyl Ether.
the unsaponifiable matter from the soap solution with ethyl 4.3 Potassium Hydroxide, Alcoholic Solution (28 g/L)—
ether. Dissolveapproximately,butnotlessthan,28gofKOHinethyl
1.2 The values stated in SI units are to be regarded as the alcohol and dilute to 1 L.
standard. 4.4 Potassium Hydroxide Aqueous Solution (28 g/L)—
1.3 This standard does not purport to address all of the Dissolve 28 g of potassium hydroxide (KOH) in water and
safety concerns, if any, associated with its use. It is the dilute to 1 L.
responsibility of the user of this standard to establish appro-
5. Procedure
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 5.1 The procedure consists of decomposing the sample with
mineralacid,extractingthedesulfatedfattymatter,saponifying
2. Referenced Documents
the latter, and extracting the unsaponifiable matter from the
2.1 ASTM Standards: soap solution with ethyl ether.
D5350 Test Method for Determination of Organically Com- 5.1.1 Desulfated Fatty Matter—Determine the desulfated
bined Sulfuric Anhydride by Titration, Test Method A fatty matter as described in the determination of total desul-
D5351 Test Method for Determination of Organically Com- fated fatty matter. See Test Methods D5350, D5351, and
bined Sulfuric Anhydride by Extraction Titration, Test D5353.
Method B 5.1.2 Saponification—Accurately weigh 2 to 2.5 g of the
D5353 Test Method for Determination of Total Desulfated desulfated fatty matter in the flask, add 25 mL of the alcoholic
Fatty Matter KOH solution, and simmer the contents (without loss of
alcohol) for 1 h with occasional swirling, over an electric hot
3. Significance and Use
plate or other source of heat.
3.1 This test method is intended for use in the determination
5.1.3 Extraction—Transfer the content of the flask to a
of the unsaponifiable, nonvolatile matter contained in sulfated 250-mL separatory funnel and wash the flask several times
oils for the purpose of quality assurance.
with a total of 50 mL of water, pouring it into the separatory
funnel. Extract the solution while still warm (about 30°C) with
50 mL of ether (rinse the saponification flask with the ether
This test method is under the jurisdiction ofASTM Committee D31 on Leather
before adding it to the separatory funnel), shaking vigorously
and is the direct responsibility of Subcommittee D31.08 on Fats and OilsThis test
method was developed in cooperation with the American Leather Chemists Assn.
for about 1 min, and allow the layers to settle and clear. Draw
(Method H 47–1957).
off the lower layer in a second 250-mL separatory funnel and
Current edition approved April 1, 2006. Published April 2006. Originally
extract in a similar manner with two 50-mL portions of ether.
approved in 1994. Last previous edition approved in 2001 as D5553 – 95(2001).
DOI: 10.1520/D5553-95R06. 5.1.4 Preliminary Water Washing—Add 20 mL of water to
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the combined ether layer, turn the separatory funnel and
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
contents over gently about six times, and allow the layers to
Standards volume information, refer to the standard’s Document Summar
...
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