ASTM D5553-95(2001)
(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
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.
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Designation: D 5553 – 95 (Reapproved 2001)
Standard Test Method for
Determination of the Unsaponifiable Nonvolatile Matter in
Sulfated Oils
This standard is issued under the fixed designation D 5553; 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 4.3 Potassium Hydroxide, Alcoholic Solution (28 g/L)—
Dissolveapproximately,butnotlessthan,28gofKOHinethyl
1.1 This test method covers the determination of the unsa-
alcohol and dilute to 1 L.
ponifiable, nonvolatile (above 80°C) matter existing in a
4.4 Potassium Hydroxide Aqueous Solution (28 g/L)—
sample of sulfated oil by saponifying the desulfated fatty
Dissolve 28 g of potassium hydroxide (KOH) in water and
matter and extracting the unsaponifiable matter, and extracting
dilute to 1 L.
the unsaponifiable matter from the soap solution with ethyl
ether.
5. Procedure
1.2 The values stated in SI units are to be regarded as the
5.1 The procedure consists of decomposing the sample with
standard.
mineralacid,extractingthedesulfatedfattymatter,saponifying
1.3 This standard does not purport to address all of the
the latter, and extracting the unsaponifiable matter from the
safety concerns, if any, associated with its use. It is the
soap solution with ethyl ether.
responsibility of the user of this standard to establish appro-
5.1.1 Desulfated Fatty Matter—Determine the desulfated
priate safety and health practices and determine the applica-
fatty matter as described in the determination of total des-
bility of regulatory limitations prior to use.
ulfated fatty matter. See Test Methods D 5350, D 5351, and
2. Referenced Documents D 5353.
5.1.2 Saponification—Accurately weigh 2 to 2.5 g of the
2.1 ASTM Standards:
desulfated fatty matter in the flask, add 25 mL of the alcoholic
D 5350 Test Method for Determination of Organically
KOH solution, and simmer the contents (without loss of
Combined Sulfuric Anhydride by Titration, Test Method
alcohol) for 1 h with occasional swirling, over an electric hot
A
plate or other source of heat.
D 5351 Test Method for Determination of Organically
5.1.3 Extraction—Transfer the content of the flask to a
CombinedSulfuricAnhydridebyExtractionTitration,Test
250-mL separatory funnel and wash the flask several times
Method B
with a total of 50 mL of water, pouring it into the separatory
D 5353 Test Method for Determination of Total Desulfated
funnel. Extract the solution while still warm (about 30°C) with
Fatty Matter
50 mL of ether (rinse the saponification flask with the ether
3. Significance and Use before adding it to the separatory funnel), shaking vigorously
for about 1 min, and allow the layers to settle and clear. Draw
3.1 This test method is intended for use in the determination
off the lower layer in a second 250-mL separatory funnel and
of the unsaponifiable, nonvolatile matter contained in sulfated
extract in a similar manner with two 50-mL portions of ether.
oils for the purpose of quality assurance.
5.1.4 Preliminary Water Washing—Add 20 mL of water to
4. Apparatus and Reagents
the combined ether layer, turn the separatory funnel and
contents over gently about six times, and allow the layers to
4.1 Saponification Flask—The apparatus required for the
settle and clear. Draw off the lower layer and discard.Wash the
saponification consists of a glass flask provided with an air
ether layer twice more with 20-mL portions of water, shaking
condenser.
vigorously after each addition.
4.2 Ethyl Ether.
5.1.5 Alkali and Water Washing—Add 20 mL of aqueous
KOH solution to the washed ether layer, turn the separatory
This test method is under the jurisdiction ofASTM Committee D31 on Leather
funnel and contents over gently about six times, and allow the
and is the direct responsibility of Subcommitt
...
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