ASTM D5350-95(2001)
(Test Method)Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Titration, Test Method A
Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Titration, Test Method A
SCOPE
1.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfated oil by boiling the sample with sulfuric acid and determining the acidity of the reaction mixture. This test method is applicable only to oils that split off their combined SO3 upon boiling with mineral acids and that do not contain 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 15 through 19.
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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Designation:D5350–95 (Reapproved 2001)
Standard Test Method for
Determination of Organically Combined Sulfuric Anhydride
by Titration, Test Method A
This standard is issued under the fixed designation D 5350; 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 4.1.1 Flask, an Erlenmeyer flask (Fig. 1) made of borosili-
cate glass, having a capacity of approximately 300 mL and
1.1 This test method covers the determination of the organi-
provided with a glass stopper.
cally combined sulfuric anhydride existing in a sample of
4.1.2 Condenser—The condenser required consists of a
sulfated oil by boiling the sample with sulfuric acid and
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
determining the acidity of the reaction mixture. This test
outside diameter. The lower end of the tube shall be flared and
method is applicable only to oils that split off their combined
ground to fit the mouth of the Erlenmeyer flask.
SO upon boiling with mineral acids and that do not contain
4.1.3 Glass Beads, perforated glass beads, made of chemi-
compounds that cannot be accurately titrated in water solution
cally resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
with methyl orange as the indicator. This test method was
Before using, the glass beads shall be boiled thoroughly in
derived from Test Methods D 500, Sections 15 through 19.
several portions of water or until the wash water reacts neutral
1.2 The values stated in SI units are to be regarded as the
to methyl orange indicator.
standard. The values given in parentheses are provided for
information only.
5. Reagents
1.3 This standard does not purport to address all of the
5.1 Ethyl Ether.
safety concerns, if any, associated with its use. It is the
5.2 Methyl Orange Indicator Solution (1 g/L)—Dissolve
responsibility of the user of this standard to establish appro-
0.1 g of methyl orange in 100 mL of water.
priate safety and health practices and determine the applica-
5.3 Sodium Chloride (NaCl), solid.
bility of regulatory limitations prior to use.
5.4 Sodium Hydroxide, Standard Solution (1 N)—
2. Referenced Documents Accurately prepare and standardize a 1 N sodium hydroxide
(NaOH) solution. Express the strength or concentration of the
2.1 ASTM Standards:
solution as milligrams of KOH per millilitre; 1 mL of 1 N
D 500 Test Methods of Chemical Analysis of Sulfonated
NaOH solution is equivalent to 56.1 mg of KOH.
and Sulfated Oils
5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
3. Significance and Use
Accurately prepare and standardize a 0.5 N NaOH solution.
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.
4. Apparatus
5.6 Sulfuric Acid, Standard (0.5 N)—Accurately prepare
andstandardizea0.5Nsulfuricacid(H SO )solution.Express
4.1 The apparatus required consists of a glass flask provided 2 4
thestrengthofthesolutionasmilligramsofKOHpermillilitre;
with a glass stopper and an air condenser. The connection
1mLof0.5 N H SO is equivalent to 28.05 mg of KOH.
between the flask and the condenser shall be a ground joint. 2 4
5.7 Sulfuric Acid (1+19)—Carefully mix one volume of
Perforated glass beads shall be used to prevent bumping.
concentrated sulfuric acid (H SO , sp gr 1.84) into 19 volumes
2 4
of water while stirring.
This test method is under the jurisdiction ofASTM Committee D31 on Leather
6. Procedure
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
method was developed in cooperation with the American Leather Chemists Assn.
6.1 The procedure consists of two determinations: namely,
(Method H 42–1957).
(1) the alkalinity of the sample, designated as A, and (2) the
Current edition approved May 15, 1995. Published July 1995. Originally
increase in acidity after boiling the sample with sulfuric acid,
published as D 5350 – 93. Last previous edition D 5350 – 93.
Annual Book of ASTM Standards, Vol 15.04. designated as F.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5350–95 (2001)
excess. Regulate the heating so that the solution boils rather
vigorously but with very little evaporation taking place.At the
end of the heating period all
...
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