ASTM D5553-95(2012)
(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 standard. No other units of measurement are included in this 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5553 −95 (Reapproved 2012)
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
4.1 Saponification Flask—The apparatus required for the
unsaponifiable, 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
alcohol and dilute to 1 L.
standard. No other units of measurement are included in this
4.4 Potassium Hydroxide Aqueous Solution (28 g/L)—
standard.
Dissolve 28 g of potassium hydroxide (KOH) in water and
1.3 This standard does not purport to address all of the
dilute to 1 L.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Procedure
priate safety and health practices and determine the applica-
5.1 The procedure consists of decomposing the sample with
bility of regulatory limitations prior to use.
mineralacid,extractingthedesulfatedfattymatter,saponifying
the latter, and extracting the unsaponifiable matter from the
2. Referenced Documents
soap solution with ethyl ether.
2.1 ASTM Standards:
5.1.1 Desulfated Fatty Matter—Determine the desulfated
D5350 Test Method for Determination of Organically Com-
fatty matter as described in the determination of total desul-
bined Sulfuric Anhydride by Titration, Test Method A
fated fatty matter. See Test Methods D5350, D5351, and
D5351 Test Method for Determination of Organically Com-
D5353.
bined Sulfuric Anhydride by Extraction Titration, Test
5.1.2 Saponification—Accurately weigh 2 to 2.5 g of the
Method B
desulfated fatty matter in the flask, add 25 mL of the alcoholic
D5353 Test Method for Determination of Total Desulfated
KOH solution, and simmer the contents (without loss of
Fatty Matter
alcohol) for 1 h with occasional swirling, over an electric hot
plate or other source of heat.
3. Significance and Use
5.1.3 Extraction—Transfer the content of the flask to a
3.1 This test method is intended for use in the determination
250-mL separatory funnel and wash the flask several times
of the unsaponifiable, nonvolatile matter contained in sulfated
with a total of 50 mL of water, pouring it into the separatory
oils for the purpose of quality assurance.
funnel. Extract the solution while still warm (about 30°C) with
50 mL of ether (rinse the saponification flask with the ether
before adding it to the separatory funnel), shaking vigorously
1 for about 1 min, and allow the layers to settle and clear. Draw
This test method is under the jurisdiction ofASTM Committee D31 on Leather
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
off the lower layer in a second 250-mL separatory funnel and
method was developed in cooperation with the American Leather Chemists Assn.
extract in a similar manner with two 50-mL portions of ether.
(Method H 47–1957).
5.1.4 Preliminary Water Washing—Add 20 mL of water to
Current edition approved April 1, 2012. Published April 2012. Originally
the combined ether layer, turn the separatory funnel and
approved in 1994. Last previous edition approved in 2006 as D5553 – 95(2006).
DOI: 10.1520/D5553-95R12.
contents over gently about six times, and allow the layers to
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
settle and clear. Draw off the lower layer and discard.Wash the
contact ASTM Customer Service at service@as
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