ASTM D5566-95(2001)

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
• 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 - Standard Test Method for Determination of Inorganic Salt Content of Sulfated and Sulfonated Oils
• Effective Date: 15-May-1995
• Replaced By: ASTM D5566-95(2006) - Standard Test Method for Determination of Inorganic Salt Content of Sulfated and Sulfonated Oils
• Effective Date: 01-Apr-2006

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2001)
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 Thistestmethodcoversthedeterminationofasampleof
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
ignited but only dried to constant weight. The presence of
responsibility of the user of this standard to establish appro-
sodium acetate does not interfere with this test method.
priate safety and health practices and determine the applica-
5.1.1 In theAbsence ofAmmonium Salts—Weigh3to5gof
bility of regulatory limitations prior to use.
the sample and place in a 250-mL beaker, add an approxi-
mately equal amount of oleic acid, and heat the mixture on an
2. Significance and Use
oil bath, while stirring constantly with a thermometer, at a
2.1 This test method is intended to be used for the determi-
temperature of 105 to 110°C until practically free from water.
nation of the inorganic salt content of sulfated and sulfonated
Continue the heating until the temperature of the contents
fats and oils for the purpose of quality control.
reaches 118 to 120°C and maintain at that temperature for
3. Apparatus about 5 min. If the dehydrated sample upon cooling does not
remain liquid, add more oleic acid. Dissolve the dehydrated
3.1 Gooch Crucible or Filter Paper—Either may be used
sample in 100 mL of CCl warmed to 50 to 55°C, and filter
for filtering. Ignite the Gooch crucible in a larger crucible,
through a counterpoised filter paper or a Gooch crucible. Pass
supported by a ring and assembled as shown in Fig. 1. If filter
75 mL of CCl through the crucible and again ignite, cool in a
paper is used, it may be a 9-cm general purpose ashless filter 4
desiccator, and weigh. Repeat the process of washing with
paper.
CCl until there is no further loss in weight. Wash the residue
3.2 Thermometer. 4
with three 15-mL portions of a solution of oleic acid in
4. Reagents CCl (2 %), then with six 15-mL portions of hot CCl , and
4 4
finally with two 15-mL portions of ether or until the residue is
4.1 Carbon Tetrachloride (CCl ).
free from oil. Take care that the top of the filter is thoroughly
4.2 Ethyl Ether.
washed. Transfer the last traces of the residue to the filter by
4.3 Oleic Acid.
allowing the solvent to evaporate when the salts become free
5. Procedure
flowing. Dry the residue at 125 to 130°C for 45 min, cool in a
desiccator, and weigh. Ignite the residue at a dull red heat for
5.1 The procedure consists of dehydrating the sample,
15 min, weigh, and repeat the ignition until constant weight is
dissolving in a solvent, filtering, igniting, and weighing the
obtained.
residue. In the presence of ammonium salts, the residue is not
5.1.2 In the Presence of Ammonium Salts—Proceed as
describedin6.1.1for
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