Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Titration, Test Method A

SIGNIFICANCE AND USE
3.1 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 standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
31-Mar-2019
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM D5350-95(2019) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Titration, Test Method A
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5350 − 95 (Reapproved 2019)
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 3. Significance and Use
3.1 This test method is intended for the determination of
1.1 This test method covers the determination of the organi-
organically combined sulfuric anhydride in sulfated oils.
cally combined sulfuric anhydride existing in a sample of
sulfated oil by boiling the sample with sulfuric acid and
4. Apparatus
determining the acidity of the reaction mixture. This test
4.1 The apparatus required consists of a glass flask provided
method is applicable only to oils that split off their combined
with a glass stopper and an air condenser. The connection
SO upon boiling with mineral acids and that do not contain
between the flask and the condenser shall be a ground joint.
compounds that cannot be accurately titrated in water solution
Perforated glass beads shall be used to prevent bumping.
with methyl orange as the indicator. This test method was
4.1.1 Flask, an Erlenmeyer flask (Fig. 1) made of borosili-
derived from Test Methods D500, Sections 15 through 19.
cate glass, having a capacity of approximately 300 mL and
1.2 The values stated in SI units are to be regarded as provided with a glass stopper.
standard. The values given in parentheses after SI units are 4.1.2 Condenser—The condenser required consists of a
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
provided for information only and are not considered standard.
outside diameter. The lower end of the tube shall be flared and
1.3 This standard does not purport to address all of the
ground to fit the mouth of the Erlenmeyer flask.
safety concerns, if any, associated with its use. It is the
4.1.3 Glass Beads, perforated glass beads, made of chemi-
responsibility of the user of this standard to establish appro-
cally resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
priate safety, health, and environmental practices and deter-
Before using, the glass beads shall be boiled thoroughly in
mine the applicability of regulatory limitations prior to use.
several portions of water or until the wash water reacts neutral
1.4 This international standard was developed in accor-
to methyl orange indicator.
dance with internationally recognized principles on standard-
5. Reagents
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
5.1 Ethyl Ether.
mendations issued by the World Trade Organization Technical
5.2 MethylOrangeIndicatorSolution(1g/L)—Dissolve 0.1
Barriers to Trade (TBT) Committee.
g of methyl orange in 100 mL of water.
5.3 Sodium Chloride (NaCl), solid.
2. Referenced Documents
5.4 Sodium Hydroxide, Standard Solution (1 N)—
2.1 ASTM Standards:
Accurately prepare and standardize a 1 N sodium hydroxide
D500 Test Methods of ChemicalAnalysis of Sulfonated and
(NaOH) solution. Express the strength or concentration of the
Sulfated Oils
solution as milligrams of KOH per millilitre; 1 mL of 1 N
NaOH solution is equivalent to 56.1 mg of KOH.
5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
This test method is under the jurisdiction ofASTM Committee D31 on Leather
Accurately prepare and standardize a 0.5 N NaOH solution.
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test
Express the strength of the solution as milligrams of KOH per
method was developed in cooperation with the American Leather Chemists Assn.
(Method H 42–1957).
millilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05
Current edition approved April 1, 2019. Published April 2019. Originally
mg of KOH.
approved in 1993. Last previous edition approved in 2012 as D5350 – 95(2012).
DOI: 10.1520/D5350-95R19.
5.6 SulfuricAcid,Standard(0.5N)—Accuratelyprepareand
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
standardize a 0.5N sulfuric acid (H SO ) solution. Express the
2 4
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
strength of the solution as milligrams of KOH per millilitre; 1
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. mL of 0.5 N H SO is equivalent to 28.05 mg of KOH.
2 4
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5350 − 95 (2019)
6.1.2 Increase in Acidity upon Boiling, F—Weigh 10 g of
the sample into the Erlenmeyer flask and boil under the air
condenserwithH SO (1+19)for1 ⁄2horuntilboththeoiland
2 4
water layers are perfectly clear,
...

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