ASTM D5553-95(2019)
(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
3.1 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:D5553 −95 (Reapproved 2019)
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 3. Significance and Use
1.1 This test method covers the determination of the
3.1 This test method is intended for use in the determination
unsaponifiable, nonvolatile (above 80°C) matter existing in a
of the unsaponifiable, nonvolatile matter contained in sulfated
sample of sulfated oil by saponifying the desulfated fatty
oils for the purpose of quality assurance.
matter and extracting the unsaponifiable matter, and extracting
the unsaponifiable matter from the soap solution with ethyl
4. Apparatus and Reagents
ether.
4.1 Saponification Flask—The apparatus required for the
1.2 The values stated in SI units are to be regarded as
saponification consists of a glass flask provided with an air
standard. No other units of measurement are included in this
condenser.
standard.
4.2 Ethyl Ether.
1.3 This standard does not purport to address all of the
4.3 Potassium Hydroxide, Alcoholic Solution (28 g/L)—
safety concerns, if any, associated with its use. It is the
Dissolveapproximately,butnotlessthan,28gofKOHinethyl
responsibility of the user of this standard to establish appro-
alcohol and dilute to 1 L.
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4.4 Potassium Hydroxide Aqueous Solution (28 g/L)—
1.4 This international standard was developed in accor-
Dissolve 28 g of potassium hydroxide (KOH) in water and
dance with internationally recognized principles on standard-
dilute to 1 L.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5. Procedure
mendations issued by the World Trade Organization Technical
5.1 The procedure consists of decomposing the sample with
Barriers to Trade (TBT) Committee.
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.
1 5.1.3 Extraction—Transfer the content of the flask to a
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
250-mL separatory funnel and wash the flask several times
method was developed in cooperation with the American Leather Chemists Assn.
with a total of 50 mL of water, pouring it into the separatory
(Method H 47–1957).
funnel. Extract the solution while still warm (about 30°C) with
Current edition approved April 1, 2019. Published April 2019. Originally
50 mL of ether (rinse the saponification flask with the ether
approved in 1994. Last previous edition approved in 2012 as D5553 – 95(2012).
DOI: 10.1520/D5553-95R19.
before adding it to the separatory funnel), shaking vigorously
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
for about 1 min, and allow the layers to settle and clear. Draw
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
off the lower layer in a second 250-mL separatory funnel and
Standards volume information, refer to the standard’
...
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