ASTM D5348-95
(Test Method)Standard Test Method for Determination of the Moisture Content of Sulfonated and Sulfated Oils by Distillation with Xylene
Standard Test Method for Determination of the Moisture Content of Sulfonated and Sulfated Oils by Distillation with Xylene
SCOPE
1.1 This test method covers the determination of water existing in a sample of sulfonated or sulfated oil, or both, by distilling the sample with a volatile solvent. The test method is applicable only to sulfonated and sulfated oils that do not contain the following: mineral acids, free sulfonic acids, or free sulfuric acid esters; or alkali hydroxides, carbonates or acetates: or alcohol, glycerin, diethylene glycol, acetone, or other water-miscible volatile compounds. This test method was derived from Test Methods D500, Sections 4 through 9.
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.
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Designation: D 5348 – 95
Standard Test Method for
Determination of the Moisture Content of Sulfonated and
Sulfated Oils by Distillation with Xylene
This standard is issued under the fixed designation D 5348; 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 flask. A suitable assembly of the apparatus is illustrated in Fig.
1.
1.1 This test method covers the determination of water
4.1.1 Flask, 500-mL, of either the short-neck, round-bottom
existing in a sample of sulfonated or sulfated oil, or both, by
type or the Erlenmeyer type.
distilling the sample with a volatile solvent. The test method is
4.1.2 Heat Source—The source of heat may be either an oil
applicable only to sulfonated and sulfated oils that do not
bath (stearic acid, paraffin wax, etc.), or an electric heater
contain the following: mineral acids, free sulfonic acids, or free
provided with a sliding rheostat or other means of heat control.
sulfuric acid esters; or alkali hydroxides, carbonates or ac-
4.1.3 Condenser, a water-cooled glass reflux condenser
etates: or alcohol, glycerin, diethylene glycol, acetone, or other
(Fig. 1), having a jacket approximately 400 mm (15 ⁄4 in.) in
water-miscible volatile compounds. This test method was
3 1
length with an inner tube 9.5 to 12.7 mm ( ⁄8 to ⁄2 in.) in
derived from Test Methods D 500, Sections 4 through 9.
outside diameter. The end of the condenser to be inserted in the
1.2 The values stated in SI units are to be regarded as the
trap shall be ground off at an angle of 30° from the vertical axis
standard. The values given in parentheses are provided for
of the condenser. When inserted into the trap, the tip of the
information only.
condenser shall be about 7 mm ( ⁄4 in.) above the surface of the
1.3 This standard does not purport to address all of the
liquid in the trap after the distillation conditions have been
safety concerns, if any, associated with its use. It is the
established. Fig. 1 shows a conventional sealed-in type of
responsibility of the user of this standard to establish appro-
condenser, but any other condenser fulfilling the detailed
priate safety and health practices and determine the applica-
requirements above may be used.
bility of regulatory limitations prior to use.
4.1.4 Trap, a trap made of well-annealed glass constructed
2. Referenced Documents in accordance with Fig. 1 and graduated as shown to contain 5
mL at 20°C. It shall be subdivided into 0.1-mL divisions, with
2.1 ASTM Standards:
each 1-mL line numbered (5 mL at top). The error in any
D 500 Test Methods of Chemical Analysis of Sulfonated
indicated capacity may not be greater than 0.05 mL.
and Sulfated Oils
5. Purity of Reagents
3. Significance and Use
5.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 This test method is intended to determine the moisture
used in all tests. Unless otherwise indicated, it is intended that
content of fats, oils, and fatliquors used in the softening and
all reagents shall conform to the specifications of the Commit-
stuffing of leather. The moisture content is measured for the
tee on Analytical Reagents of the American Chemical Society.
purpose of quality assurance.
6. Reagents
4. Apparatus
6.1 Oleic Acid, heated previous to use for 5 to 10 min over
4.1 The apparatus required consists of a glass flask heated
a free flame at a temperature of 130 to 135°C.
by suitable means and provided with a reflux condenser
6.2 Xylene.
discharging into a trap and connected to the flask. The
connections between the trap and the condenser and flask shall
7. Calibration
be interchangeable ground joints. The trap serves to collect and
7.1 To calibrate the apparatus add approximately1gof
measure the condensed water and to return the solvent to the
water to a mixture of 80 g of xylene and 10 g of oleic acid.
This test method is under the jurisdiction of ASTM Committee D-31 on Leather
and is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This test Reagent Chemicals, American Chemical Society Specifications, American
method was developed in cooperation with the American Leather Chemists Assn. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
(Method H 40-1957). listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved May 15, 1995. Published July 1995. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 5348 – 93. Last previous edition D 5348 – 93. and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 15.04. MD.
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