ASTM D5350-95(2012)
(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)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5350 − 95 (Reapproved 2012)
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
sulfated oil by boiling the sample with sulfuric acid and cate glass, having a capacity of approximately 300 mL and
determining the acidity of the reaction mixture. This test provided with a glass stopper.
method is applicable only to oils that split off their combined
4.1.2 Condenser—The condenser required consists of a
SO upon boiling with mineral acids and that do not contain
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
compounds that cannot be accurately titrated in water solution
outside diameter. The lower end of the tube shall be flared and
with methyl orange as the indicator. This test method was
ground to fit the mouth of the Erlenmeyer flask.
derived from Test Methods D500, Sections 15 through 19.
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
responsibility of the user of this standard to establish appro-
5. Reagents
priate safety and health practices and determine the applica-
5.1 Ethyl Ether.
bility of regulatory limitations prior to use.
5.2 MethylOrangeIndicatorSolution(1g/L)—Dissolve 0.1
2. Referenced Documents
g of methyl orange in 100 mL of water.
2.1 ASTM Standards:
5.3 Sodium Chloride (NaCl), solid.
D500 Test Methods of ChemicalAnalysis of Sulfonated and
Sulfated Oils
5.4 Sodium Hydroxide, Standard Solution (1 N)—
Accurately prepare and standardize a 1 N sodium hydroxide
3. Significance and Use
(NaOH) solution. Express the strength or concentration of the
3.1 This test method is intended for the determination of
solution as milligrams of KOH per millilitre; 1 mL of 1 N
organically combined sulfuric anhydride in sulfated oils.
NaOH solution is equivalent to 56.1 mg of KOH.
4. Apparatus
5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
4.1 The apparatus required consists of a glass flask provided
Accurately prepare and standardize a 0.5 N NaOH solution.
with a glass stopper and an air condenser. The connection
Express the strength of the solution as milligrams of KOH per
millilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05
mg of KOH.
This test method is under the jurisdiction ofASTM Committee D31 on Leather
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
5.6 SulfuricAcid,Standard(0.5N)—Accuratelyprepareand
method was developed in cooperation with the American Leather Chemists Assn.
standardize a 0.5 N sulfuric acid (H SO ) solution. Express the
(Method H 42–1957). 2 4
Current edition approved April 1, 2012. Published April 2012. Originally strength of the solution as milligrams of KOH per millilitre; 1
approved in 1993. Last previous edition approved in 2006 as D5350 – 95(2006).
mL of 0.5 N H SO is equivalent to 28.05 mg of KOH.
2 4
DOI: 10.1520/D5350-95R12.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.7 Sulfuric Acid (1+19)—Carefully mix one volume of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
concentrated sulfuric acid (H SO , sp gr 1.84) into 19 volumes
2 4
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. of water while stirring.
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D5350 − 95 (2012)
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
vigorously but with very little evaporation taking place.At the
end of the heating peri
...
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