ASTM D5566-95(2011)

Standard Test Method for Determination of Inorganic Salt Content of Sulfated and Sulfonated Oils (Withdrawn 2020)

SIGNIFICANCE AND USE
This test method is intended to be used for the determination of the inorganic salt content of sulfated and sulfonated fats and oils for the purpose of quality control.
SCOPE
1.1 This test method covers the determination of a sample of sulfonated or sulfated oil, or both, the inorganic sulfates, chlorides, and all other salts that are insoluble in a mixture of oleic acid and carbon tetrachloride.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this 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 and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method covers the determination of a sample of sulfonated or sulfated oil, or both, the inorganic sulfates, chlorides, and all other salts that are insoluble in a mixture of oleic acid and carbon tetrachloride.
Formerly under the jurisdiction of Committee D31 on Leather, this test method was withdrawn in January 2020 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-2010
• Withdrawal Date: 09-Jan-2020
• ICS: 67.200.10 - Animal and vegetable fats and oils
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaces: ASTM D5566-95(2006) - Standard Test Method for Determination of Inorganic Salt Content of Sulfated and Sulfonated Oils
• Effective Date: 01-Jan-2011

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D5566 − 95 (Reapproved 2011)
Standard Test Method for
Determination of Inorganic Salt Content of Sulfated and
Sulfonated Oils
This standard is issued under the fixed designation D5566; 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 5. Procedure
1.1 Thistestmethodcoversthedeterminationofasampleof
5.1 The procedure consists of dehydrating the sample,
sulfonated or sulfated oil, or both, the inorganic sulfates,
dissolving in a solvent, filtering, igniting, and weighing the
chlorides, and all other salts that are insoluble in a mixture of
residue. In the presence of ammonium salts, the residue is not
oleic acid and carbon tetrachloride.
ignited but only dried to constant weight. The presence of
sodium acetate does not interfere with this test method.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 5.1.1 In theAbsence ofAmmonium Salts—Weigh3to5gof
standard. the sample and place in a 250-mL beaker, add an approxi-
mately equal amount of oleic acid, and heat the mixture on an
1.3 This standard does not purport to address all of the
oil bath, while stirring constantly with a thermometer, at a
safety concerns, if any, associated with its use. It is the
temperature of 105 to 110°C until practically free from water.
responsibility of the user of this standard to establish appro-
Continue the heating until the temperature of the contents
priate safety and health practices and determine the applica-
reaches 118 to 120°C and maintain at that temperature for
bility of regulatory limitations prior to use.
about 5 min. If the dehydrated sample upon cooling does not
remain liquid, add more oleic acid. Dissolve the dehydrated
2. Significance and Use
sample in 100 mL of CCl warmed to 50 to 55°C, and filter
2.1 This test method is intended to be used for the determi-
through a counterpoised filter paper or a Gooch crucible. Pass
nation of the inorganic salt content of sulfated and sulfonated
75 mL of CCl through the crucible and again ignite, cool in a
fats and oils for the purpose of quality control.
desiccator, and weigh. Repeat the process of washing with
CCl until there is no further loss in weight. Wash the residue
3. Apparatus
with three 15-mL portions of a solution of oleic acid in CCl
(2 %), then with six 15-mL portions of hot CCl , and finally
3.1 Gooch Crucible or Filter Paper—Either may be used
with two 15-mL portions of ether or until the residue is free
for filtering. Ignite the Gooch crucible in a larger crucible,
from oil. Take care that the top of the filter is thoroughly
supported by a ring and assembled as shown in Fig. 1. If filter
paper is used, it may be a 9-cm general purpose ashless filter washed. Transfer the last traces of the residue to the filter by
allowing the solvent to evaporate when the salts become free
paper.
flowing. Dry the residue at 125 to 130°C for 45 min, cool in a
3.2 Thermometer.
desiccator, and weigh. Ignite the residue at a dull red heat for
15 min, weigh, and repeat the ignition until constant weight is
4. Reagents
obtained.
4.1 Carbon Tetrachloride (CCl ).
5.1.2 In the Presence of Ammonium Salts—Proceed as
describedin6.1.1forthedeterminationofinorganicsaltsinthe
4.2 Ethyl Ether.
absence of ammonium salts with the following exceptions: (1)
4.3 Oleic Acid.
in preparing the Gooch crucible, do not ignite but heat it at
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