ASTM D5351-93(2003)
(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
SIGNIFICANCE AND USE
This test method is intended for the determination of organically combined sulfuric anhydride in sulfated oils.
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 D 500, 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 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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Standards Content (Sample)
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Designation:D5351–93 (Reapproved 2003)
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 4. Apparatus
1.1 This test method covers the determination of the organi- 4.1 The apparatus required consists of a glass flask provided
cally combined sulfuric anhydride existing in a sample of with a glass stopper and an air condenser. The connection
sulfated oil by extracting the undecomposed sulfated fat and between the flask and the condenser shall be a ground joint.
other fatty matter over an acidulated, concentrated salt solu- Perforated glass beads shall be used to prevent bumping.
tion, boiling the residue with sulfuric acid after evaporating the 4.1.1 Flask, an Erlenmeyer flask (Fig. 1) made of borosili-
solvent, and titrating the products of reaction. This test method cate glass, having a capacity of approximately 300 mL, and
is applicable only to sulfated oils that split off their combined provided with a glass stopper.
SO upon boiling with mineral acids, including samples 4.1.2 Condenser—The condenser required consists of a
containing sodium acetate or other compounds that cannot be glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
accurately titrated in water solution with methyl orange as the outside diameter. The lower end of the tube shall be flared and
indicator. This test method was derived from Test Methods ground to fit the mouth of the Erlenmeyer flask.
D 500, Sections 20 through 24, and ALCA Method H-43. 4.1.3 Glass Beads, perforated glass beads, made of chemi-
1.2 The values stated in SI units are to be regarded as the cally resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
standard. The values given in parentheses are provided for Before using, the glass beads shall be boiled thoroughly in
information only. several portions of water or until the wash water reacts neutral
1.3 This standard does not purport to address all of the to methyl orange indicator.
safety concerns, if any, associated with its use. It is the
5. Reagents
responsibility of the user of this standard to establish appro-
5.1 Ethyl Ether:
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 5.2 Methyl Orange Indicator Solution (1 g/L)—Dissolve
0.1 g of methyl orange in 100 mL of water.
2. Referenced Documents
5.3 Sodium Chloride (NaCl), solid.
2.1 ASTM Standards: 5.4 Sodium Hydroxide, Standard Solution (1 N)—
D 500 Test Methods of Chemical Analysis of Sulfonated Accurately prepare and standardize a 1 N sodium hydroxide
and Sulfated Oils (NaOH) solution. Express the strength or concentration of the
2.2 Other Document: solution as milligrams of KOH per millilitre; 1 mL of 1 N
ALCAMethod H-43 Organically Combined SulfuricAnhy- NaOH solution is equivalent to 56.1 mg of KOH.
dride Extraction Titration Test (for Sulfated Oils) 5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
Accurately prepare and standardize a 0.5 N NaOH solution.
3. Significance and Use
Express the strength of the solution as milligrams of KOH per
3.1 This test method is intended for the determination of millilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05
organically combined sulfuric anhydride in sulfated oils.
mg of KOH.
5.6 Sulfuric Acid (1 + 19)—Carefully mix one volume of
1 concentrated sulfuric acid (H SO , sp gr 1.84) into 19 volumes
2 4
This test method is under the jurisdiction ofASTM Committee D31 on Leather
of water while stirring.
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils.
Current edition approved May 10, 2003. Published June 2003. Originally
approved in 1993. Last previous edition approved in 1997 as D 5351 – 93 (1997).
Annual Book of ASTM Standards, Vol 15.04.
Available fromAmerican Leather ChemistsAssn., Texas Tech University, P.O.
Box 453
...
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