ASTM D5350-95
(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: D 5350 – 95
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
1.1 This test method covers the determination of the organi-
cally 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
SO 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 D 500, 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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
FIG. 1 Apparatus for Determination of Organically Combined
Sulfuric Anhydride, Test Method A
2. Referenced Documents
2.1 ASTM Standards:
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
D 500 Test Methods of Chemical Analysis of Sulfonated
outside diameter. The lower end of the tube shall be flared and
and Sulfated Oils
ground to fit the mouth of the Erlenmeyer flask.
4.1.3 Glass Beads, perforated glass beads, made of chemi-
3. Significance and Use
cally resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
3.1 This test method is intended for the determination of
Before using, the glass beads shall be boiled thoroughly in
organically combined sulfuric anhydride in sulfated oils.
several portions of water or until the wash water reacts neutral
to methyl orange indicator.
4. Apparatus
4.1 The apparatus required consists of a glass flask provided
5. Reagents
with a glass stopper and an air condenser. The connection
5.1 Ethyl Ether.
between the flask and the condenser shall be a ground joint.
5.2 Methyl Orange Indicator Solution (1 g/L)—Dissolve
Perforated glass beads shall be used to prevent bumping.
0.1 g of methyl orange in 100 mL of water.
4.1.1 Flask, an Erlenmeyer flask (Fig. 1) made of borosili-
5.3 Sodium Chloride (NaCl), solid.
cate glass, having a capacity of approximately 300 mL and
5.4 Sodium Hydroxide, Standard Solution (1 N)—
provided with a glass stopper.
Accurately prepare and standardize a 1 N sodium hydroxide
4.1.2 Condenser—The condenser required consists of a
(NaOH) solution. Express the strength or concentration of the
solution as milligrams of KOH per millilitre; 1 mL of 1 N
1 NaOH solution is equivalent to 56.1 mg of KOH.
This test method is under the jurisdiction of ASTM Committee D-31 on Leather
5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
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.
Accurately prepare and standardize a 0.5 N NaOH solution.
(Method H 42–1957).
Express the strength of the solution as milligrams of KOH per
Current edition approved May 15, 1995. Published July 1995. Originally
millilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05
published as D 5350 – 93. Last previous edition D 5350 – 93.
Annual Book of ASTM Standards, Vol 15.04. mg of KOH.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5350
5.6 Sulfuric Acid, Standard (0.5 N)—Accurately prepare condenser with a spray of water from a wash bottle, and
and standardize a 0.5 N sulfuric acid (H SO ) solution. Express disconnect the condenser. Add 30 g of NaCl, 25 mL of ether, 50
2 4
the strength of the solution as milligrams of KOH per millilitre; mL of water, and five drops of indicator solution and titrate the
1mL of0.5 N H SO is equivalent to 28.05 mg of KOH. solution with 1 N NaOH solution to the same end point as in
2 4
the total alkalinity titration, 6.1.1. During the titration stopper
5.7 Sulfuric Acid (1+19)—Carefully mix one volume of
concentrated sulfuric acid (H SO , sp gr 1.84) into 19 volumes
...
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