ASTM D5350-95(2006)
(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
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 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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Standards Content (Sample)
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Designation:D5350–95 (Reapproved 2006)
Standard Test Method for
Determination of Organically Combined Sulfuric Anhydride
by Titration, Test Method A
This standard is issued under the fixed designation D5350; 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 (´) 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 boiling the sample with sulfuric acid and
provided with a glass stopper.
determining the acidity of the reaction mixture. This test
4.1.2 Condenser—The condenser required consists of a
method is applicable only to oils that split off their combined
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
SO upon boiling with mineral acids and that do not contain
outside diameter. The lower end of the tube shall be flared and
compounds that cannot be accurately titrated in water solution
ground to fit the mouth of the Erlenmeyer flask.
with methyl orange as the indicator. This test method was
4.1.3 Glass Beads, perforated glass beads, made of chemi-
derived from Test Methods D500, Sections 15 through 19.
cally resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
1.2 The values stated in SI units are to be regarded as the
Before using, the glass beads shall be boiled thoroughly in
standard. The values given in parentheses are provided for
several portions of water or until the wash water reacts neutral
information only.
to methyl orange indicator.
1.3 This standard does not purport to address all of the
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-
5.2 MethylOrangeIndicatorSolution(1g/L)—Dissolve0.1
bility of regulatory limitations prior to use.
g of methyl orange in 100 mL of water.
2. Referenced Documents 5.3 Sodium Chloride (NaCl), solid.
5.4 Sodium Hydroxide, Standard Solution (1 N)—
2.1 ASTM Standards:
Accurately prepare and standardize a 1 N sodium hydroxide
D500 TestMethodsofChemicalAnalysisofSulfonatedand
(NaOH) solution. Express the strength or concentration of the
Sulfated Oils
solution as milligrams of KOH per millilitre; 1 mL of 1 N
3. Significance and Use
NaOH solution is equivalent to 56.1 mg of KOH.
5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
3.1 This test method is intended for the determination of
Accurately prepare and standardize a 0.5 N NaOH solution.
organically combined sulfuric anhydride in sulfated oils.
Express the strength of the solution as milligrams of KOH per
4. Apparatus
millilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05
mg of KOH.
4.1 The apparatus required consists of a glass flask provided
5.6 Sulfuric Acid, Standard (0.5 N)—Accurately prepare
with a glass stopper and an air condenser. The connection
andstandardizea0.5Nsulfuricacid(H SO )solution.Express
2 4
thestrengthofthesolutionasmilligramsofKOHpermillilitre;
This test method is under the jurisdiction ofASTM Committee D31 on Leather
1mLof0.5 N H SO is equivalent to 28.05 mg of KOH.
2 4
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. 5.7 Sulfuric Acid (1+19)—Carefully mix one volume of
(Method H 42–1957).
concentrated sulfuric acid (H SO , sp gr 1.84) into 19 volumes
2 4
Current edition approved April 1, 2006. Published April 2006. Originally
of water while stirring.
approved in 1993. Last previous edition approved in 2001 as D5350 – 95(2001).
DOI: 10.1520/D5350-95R06.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
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D5350–95 (2006)
water layers are perfectly clear, using glass beads to prevent
bumping. The volume of H SO added shall be sufficient to
2 4
neutralize the total alkalinity, A, of the sample plus 25 mL in
excess. Regulate the heating so that the solution boils rather
vigoro
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