ASTM D5553-95

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.

General Information

• Status: Historical
• Publication Date: 14-May-1995
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaced By: ASTM D5553-95(2001) - Standard Test Method for Determination of the Unsaponifiable Nonvolatile Matter in Sulfated Oils
• Effective Date: 15-May-1995
• Referred By: ASTM D5560-95(2018) - Standard Test Method for Determination of Neutral Fatty Matter Contained in Fats and Oils
• Effective Date: 15-May-1995

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5553 – 95
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 Dissolve approximately, but not less than, 28 g of KOH in ethyl
alcohol and dilute to 1 L.
1.1 This test method covers the determination of the unsa-
4.4 Potassium Hydroxide Aqueous Solution (28 g/L)—
ponifiable, nonvolatile (above 80°C) matter existing in a
Dissolve 28 g of potassium hydroxide (KOH) in water and
sample of sulfated oil by saponifying the desulfated fatty
dilute to 1 L.
matter and extracting the unsaponifiable matter, and extracting
the unsaponifiable matter from the soap solution with ethyl
5. Procedure
ether.
5.1 The procedure consists of decomposing the sample with
1.2 The values stated in SI units are to be regarded as the
mineral acid, extracting the desulfated fatty matter, saponifying
standard.
the latter, and extracting the unsaponifiable matter from the
1.3 This standard does not purport to address all of the
soap solution with ethyl ether.
safety concerns, if any, associated with its use. It is the
5.1.1 Desulfated Fatty Matter—Determine the desulfated
responsibility of the user of this standard to establish appro-
fatty matter as described in the determination of total des-
priate safety and health practices and determine the applica-
ulfated fatty matter. See Test Methods D 5350, D 5351, and
bility of regulatory limitations prior to use.
D 5353.
2. Referenced Documents 5.1.2 Saponification—Accurately weigh 2 to 2.5 g of the
desulfated fatty matter in the flask, add 25 mL of the alcoholic
2.1 ASTM Standards:
KOH solution, and simmer the contents (without loss of
D 5350 Test Method for Determination of Organically
alcohol) for 1 h with occasional swirling, over an electric hot
Combined Sulfuric Anhydride by Titration, Test Method
plate or other source of heat.
A
5.1.3 Extraction—Transfer the content of the flask to a
D 5351 Test Method for Determination of Organically
250-mL separatory funnel and wash the flask several times
Combined Sulfuric Anhydride by Extraction Titration, Test
2 with a total of 50 mL of water, pouring it into the separatory
Method B
funnel. Extract the solution while still warm (about 30°C) with
D 5353 Test Method for Determination of Total Desulfated
2 50 mL of ether (rinse the saponification flask with the ether
Fatty Matter
before adding it to the separatory funnel), shaking vigorously
3. Significance and Use for about 1 min, and allow the layers to settle and clear. Draw
off the lower layer in a second 250-mL separatory funnel and
3.1 This test method is intended for use in the determination
extract in a similar manner with two 50-mL portions of ether.
of the unsaponifiable, nonvolatile matter contained in sulfated
5.1.4 Preliminary Water Washing—Add 20 mL of water to
oils for the purpose of quality assurance.
the combined ether layer, turn the separatory funnel and
4. Apparatus and Reagents
contents over gently about six times, and allow the layers to
settle and clear. Draw off the lower layer and discard. Wash the
4.1 Saponification Flask—The apparatus required for the
ether layer twice more with 20-mL portions of water, shaking
saponification consists of a glass flask provided with an air
vigorously after each addition.
condenser.
5.1.5 Alkali and Water Washing—Add 20 mL of aqueous
4.2 Ethyl Ether.
KOH solution to the washed ether layer, turn the separatory
4.3 Potassium Hydroxide, Alcoholic Solution (28 g/L)—
funnel and contents over gently about six times, and allow the
layers to settle and clear. Draw off the lower layer and discard.
This test method is under the jurisdiction of ASTM Committee D-31 o
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