ASTM D5351-93(1997)
(Test Method)Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Extraction Titration, Test Method B
Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Extraction Titration, Test Method B
SCOPE
1.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfated oil by extracting the undecomposed sulfated fat and other fatty matter over an acidulated, concentrated salt solution, boiling the residue with sulfuric acid after evaporating the solvent, and titrating the products of reaction. This test method is applicable only to sulfated oils that split off their combined SO3 upon boiling with mineral acids, including samples containing sodium acetate or other compounds that cannot be accurately titrated in water solution with methyl orange as the indicator. This test method was derived from Test Methods D500, Sections 20 through 24, and ALCA Method H-43.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information only.
1.3 This standard does not purport to address all of the safety problems, 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 5351 – 93 (Reapproved 1997)
Standard Test Method for
Determination of Organically Combined Sulfuric Anhydride
by Extraction Titration, Test Method B
This standard is issued under the fixed designation D 5351; 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 between the flask and the condenser shall be a ground joint.
Perforated glass beads shall be used to prevent bumping.
1.1 This test method covers the determination of the organi-
4.1.1 Flask, an Erlenmeyer flask (Fig. 1) made of borosili-
cally combined sulfuric anhydride existing in a sample of
cate glass, having a capacity of approximately 300 mL, and
sulfated oil by extracting the undecomposed sulfated fat and
provided with a glass stopper.
other fatty matter over an acidulated, concentrated salt solu-
4.1.2 Condenser—The condenser required consists of a
tion, boiling the residue with sulfuric acid after evaporating the
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
solvent, and titrating the products of reaction. This test method
outside diameter. The lower end of the tube shall be flared and
is applicable only to sulfated oils that split off their combined
ground to fit the mouth of the Erlenmeyer flask.
SO upon boiling with mineral acids, including samples
4.1.3 Glass Beads, perforated glass beads, made of chemi-
containing sodium acetate or other compounds that cannot be
cally resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
accurately titrated in water solution with methyl orange as the
Before using, the glass beads shall be boiled thoroughly in
indicator. This test method was derived from Test Methods
several portions of water or until the wash water reacts neutral
D 500, Sections 20 through 24, and ALCA Method H-43.
to methyl orange indicator.
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are provided for
5. Reagents
information only.
5.1 Ethyl Ether:
1.3 This standard does not purport to address all of the
5.2 Methyl Orange Indicator Solution (1 g/L)—Dissolve
safety concerns, if any, associated with its use. It is the
0.1 g of methyl orange in 100 mL of water.
responsibility of the user of this standard to establish appro-
5.3 Sodium Chloride (NaCl), solid.
priate safety and health practices and determine the applica-
5.4 Sodium Hydroxide, Standard Solution (1 N)—
bility of regulatory limitations prior to use.
Accurately prepare and standardize a 1 N sodium hydroxide
2. Referenced Documents (NaOH) solution. Express the strength or concentration of the
solution as milligrams of KOH per millilitre; 1 mL of 1 N
2.1 ASTM Standards:
NaOH solution is equivalent to 56.1 mg of KOH.
D 500 Test Methods of Chemical Analysis of Sulfonated
5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
and Sulfated Oils
Accurately prepare and standardize a 0.5 N NaOH solution.
2.2 Other Document:
Express the strength of the solution as milligrams of KOH per
ALCA Method H-43 Organically Combined Sulfuric Anhy-
millilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05
dride Extraction Titration Test (for Sulfated Oils)
mg of KOH.
3. Significance and Use
5.6 Sulfuric Acid (1 + 19)—Carefully mix one volume of
concentrated sulfuric acid (H SO , sp gr 1.84) into 19 volumes
3.1 This test method is intended for the determination of 2 4
of water while stirring.
organically combined sulfuric anhydride in sulfated oils.
5.7 Sulfuric Acid Standard (0.5 N)—Accurately prepare
4. Apparatus
and standardize as 0.5 N sulfuric acid (H SO ) solution.
2 4
Express the strength of the solution as milligrams of KOH per
4.1 The apparatus required consists of a glass flask provided
millilitre; 1 mL of 0.5 N H SO is equivalent to 28.05 mg of
with a glass stopper and an air condenser. The connection 2 4
KOH.
This test method is under the jurisdiction of ASTM Committee D-31 on Leather 6. Procedure
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils.
6.1 The procedure consists of isolating and purifying the
Current e
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