ASTM D5566-95

Standard Test Method for Determination of Inorganic Salt Content of Sulfated and Sulfonated Oils

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 the 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.

General Information

• Status: Historical
• Publication Date: 14-May-1995
• Technical Committee: D31 - Leather
• Drafting Committee: D31.08 - Fats and Oils

Relations

• Replaced By: ASTM D5566-95(2001) - Standard Test Method for Determination of Inorganic Salt Content of Sulfated and Sulfonated Oils
• Effective Date: 15-May-1995

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5566 – 95
Standard Test Method for
Determination of Inorganic Salt Content of Sulfated and
Sulfonated Oils
This standard is issued under the fixed designation D 5566; 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 (e) indicates an editorial change since the last revision or reapproval.
1. 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 the
FIG. 1 Gooch Crucible Assembly for Determination of Inorganic
standard.
Salts
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
the sample and place in a 250-mL beaker, add an approxi-
responsibility of the user of this standard to establish appro-
mately equal amount of oleic acid, and heat the mixture on an
priate safety and health practices and determine the applica-
oil bath, while stirring constantly with a thermometer, at a
bility of regulatory limitations prior to use.
temperature of 105 to 110°C until practically free from water.
Continue the heating until the temperature of the contents
2. Significance and Use
reaches 118 to 120°C and maintain at that temperature for
2.1 This test method is intended to be used for the determi-
about 5 min. If the dehydrated sample upon cooling does not
nation of the inorganic salt content of sulfated and sulfonated
remain liquid, add more oleic acid. Dissolve the dehydrated
fats and oils for the purpose of quality control.
sample in 100 mL of CCl warmed to 50 to 55°C, and filter
through a counterpoised filter paper or a Gooch crucible. Pass
3. Apparatus
75 mL of CCl through the crucible and again ignite, cool in a
3.1 Gooch Crucible or Filter Paper—Either may be used
desiccator, and weigh. Repeat the process of washing with
for filtering. Ignite the Gooch crucible in a larger crucible,
CCl until there is no further loss in weight. Wash the residue
supported by a ring and assembled as shown in Fig. 1. If filter
with three 15-mL portions of a solution of oleic acid in
paper is used, it may be a 9-cm general purpose ashless filter
CCl (2 %), then with six 15-mL portions of hot CCl , and
4 4
paper.
finally with two 15-mL portions of ether or until the residue is
3.2 Thermometer.
free from oil. Take care that the top of the filter is thoroughly
washed. Transfer the last traces of the residue to the filter by
4. Reagents
allowing the solvent to evaporate when the salts become free
4.1 Carbon Tetrachloride (CCl ).
flowing. Dry the residue at 125 to 130°C for 45 min, cool in a
4.2 Ethyl Ether.
desiccator, and weigh. Ignite the residue at a dull red heat for
4.3 Oleic Acid.
15 min, weigh, and repeat the ignition until constant weight is
obtained.
5. Procedure
5.1.2 In the Presence of Ammonium Salts—Proceed as
5.1 The procedure consists of dehydrating the sample,
described in 6.1.1 for the determination of inorganic salts in the
dissolving in a solvent, filtering, igniting, and weighing the
absence of ammonium salts with the following exceptions: (1)
residue. In the presence of ammonium salts, the residue is not
in preparing the Gooch crucible, do not ignite but heat it at 105
ignit
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