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ASTM D5351-93(2009)

(Test Method)

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

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

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 extracting the undecomposed sulfated fat and other fatty matter over an acidulated, concentrated salt solution, boiling the residue with sulfuric acid after evaporating the solvent, and titrating the products of reaction. This test method is applicable only to sulfated oils that split off their combined SO3 upon boiling with mineral acids, including samples containing sodium acetate or other 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 20 through 24, and ALCA Method H-43.
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.

General Information

Status
Historical
Publication Date
31-Mar-2009
ICS
71.080.01 - Organic chemicals in general
Technical Committee
D31 - Leather
Drafting Committee
D31.08 - Fats and Oils
Current Stage
Ref Project

Relations

Replaces
ASTM D5351-93(2003) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Extraction Titration, Test Method B
Effective Date
01-Apr-2009
Referred By
ASTM D5353-95(2019) - Standard Test Method for Determination of Total Desulfated Fatty Matter
Effective Date
01-Apr-2009
Referred By
ASTM D5553-95(2019) - Standard Test Method for Determination of the Unsaponifiable Nonvolatile Matter in Sulfated Oils
Effective Date
01-Apr-2009

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ASTM D5351-93(2009) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Extraction Titration, Test Method BASTM D5351-93(2009) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Extraction Titration, Test Method B
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ASTM D5351-93(2009) - Standard Test Method for Determination of Organically Combined Sulfuric Anhydride by Extraction Titration, Test Method B
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5351 − 93 (Reapproved 2009)
Standard Test Method for
Determination of Organically Combined Sulfuric Anhydride
by Extraction Titration, Test Method B
This standard is issued under the fixed designation D5351; 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
1.1 This test method covers the determination of the organi- 3.1 This test method is intended for the determination of
cally combined sulfuric anhydride existing in a sample of organically combined sulfuric anhydride in sulfated oils.
sulfated oil by extracting the undecomposed sulfated fat and
other fatty matter over an acidulated, concentrated salt 4. Apparatus
solution, boiling the residue with sulfuric acid after evaporat-
4.1 The apparatus required consists of a glass flask provided
ing the solvent, and titrating the products of reaction. This test
with a glass stopper and an air condenser. The connection
method is applicable only to sulfated oils that split off their
between the flask and the condenser shall be a ground joint.
combined SO upon boiling with mineral acids, including
Perforated glass beads shall be used to prevent bumping.
samples containing sodium acetate or other compounds that
4.1.1 Flask, an Erlenmeyer flask (Fig. 1) made of borosili-
cannot be accurately titrated in water solution with methyl
cate glass, having a capacity of approximately 300 mL, and
orange as the indicator.This test method was derived fromTest
provided with a glass stopper.
Methods D500, Sections 20 through 24, and ALCA Method
4.1.2 Condenser—The condenser required consists of a
H-43.
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
1.2 The values stated in SI units are to be regarded as the outside diameter. The lower end of the tube shall be flared and
standard. The values given in parentheses are provided for
ground to fit the mouth of the Erlenmeyer flask.
information only. 4.1.3 Glass Beads, perforated glass beads, made of chemi-
cally resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
1.3 This standard does not purport to address all of the
Before using, the glass beads shall be boiled thoroughly in
safety concerns, if any, associated with its use. It is the
several portions of water or until the wash water reacts neutral
responsibility of the user of this standard to establish appro-
to methyl orange indicator.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Reagents
2. Referenced Documents
5.1 Ethyl Ether:
2.1 ASTM Standards:
5.2 Methyl Orange Indicator Solution (1 g/L)—Dissolve 0.1
D500 Test Methods of ChemicalAnalysis of Sulfonated and
g of methyl orange in 100 mL of water.
Sulfated Oils
5.3 Sodium Chloride (NaCl), solid.
2.2 Other Document:
5.4 Sodium Hydroxide, Standard Solution (1 N)—
ALCA Method H-43 Organically Combined Sulfuric Anhy-
Accurately prepare and standardize a 1 N sodium hydroxide
dride Extraction Titration Test (for Sulfated Oils)
(NaOH) solution. Express the strength or concentration of the
solution as milligrams of KOH per millilitre; 1 mL of 1 N
NaOH solution is equivalent to 56.1 mg of KOH.
This test method is under the jurisdiction ofASTM Committee D31 on Leather
5.5 Sodium Hydroxide, Standard Solution (0.5 N)—
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils
Accurately prepare and standardize a 0.5 N NaOH solution.
Current edition approved April 1, 2009. Published July 2009. Originally
approved in 1993. Last previous edition approved in 2003 as D5351 – 93 (2003).
Express the strength of the solution as milligrams of KOH per
DOI: 10.1520/D5351-93R09.
millilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
mg of KOH.
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
5.6 Sulfuric Acid (1 + 19)—Carefully mix one volume of
the ASTM website.
concentrated sulfuric acid (H SO , sp gr 1.84) into 19 volumes
Available fromAmerican Leather ChemistsAssn., Texas Tech University, P.O. 2 4
Box 45
...

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1.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfated oil by extracting the undecomposed sulfated fat and other fatty matter over an acidulated, concentrated salt solution, boiling the residue with sulfuric acid after evaporating the solvent, and titrating the products of reaction. This test method is applicable only to sulfated oils that split off their combined SO3 upon boiling with mineral acids, including samples containing sodium acetate or other 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 20 through 24, and ALCA Method H-43.  
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