ASTM D3944-88(1993)e1
(Test Method)Standard Test Method for Solidification Point of Petroleum Wax
Standard Test Method for Solidification Point of Petroleum Wax
SCOPE
1.1 This test method describes a procedure for rapidly determining the solidification point of petroleum wax.
Note 1-This test method is also applicable to similar materials such as synthetic waxes but the precision may vary.
1.2 The values in acceptable metric units are to be regarded as the standard. The values in parentheses are for information only.
1.3 This standard does not purport to address all of the safety problems, 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 3944 – 88 (Reapproved 1993) An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Solidification Point of Petroleum Wax
This standard is issued under the fixed designation D 3944; 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.
e NOTE—Keywords were added editorially in October 1993.
1. Scope cooling wax traces a curve on the chart paper of the recorder.
The first significant change in the slope of the curve is the
1.1 This test method describes a procedure for rapidly
solidification point.
determining the solidification point of petroleum wax.
NOTE 1—This test method is also applicable to similar materials such as
5. Significance and Use
synthetic waxes but the precision may vary.
5.1 The related methods of determining the melt point of
1.2 The values in acceptable metric units are to be regarded
petroleum wax are relatively time-consuming. This method
as the standard. The values in parentheses are for information
endeavors to reduce the duration of testing significantly and at
only.
the same time maintain a reasonable precision. This method
1.3 This standard does not purport to address all of the
can be useful for quality control of petroleum waxes as well as
safety problems, if any, associated with its use. It is the
research and product development work on these waxes.
responsibility of the user of this standard to establish appro-
5.2 For methods used for testing melt points of petroleum
priate safety and health practices and determine the applica-
waxes, see Tests Method D 87, D 127, including Petrolatum
bility of regulatory limitations prior to use.
and Test Method D 938.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
6.1 Thermocouple, with an iron-constantan junction.
D 87 Test Method for Melting Point of Petroleum Wax
6.2 Recorder capable of recording voltage and equipped
(Cooling Curve)
with a time-base module. The recorder should have the
D 127 Test Method for Drop Melting Point of Petroleum
following minimum specifications:
Wax Including Petrolatum
6.2.1 Span, 0 to 10 mV or other suitable ranges.
D 938 Test Method for Congealing Point of Petroleum
6.2.2 Accuracy, 0.25 % of full scale.
Waxes Including Petrolatum
6.2.3 Step Response Time, 1-s full scale, 3-s full scale is also
appropriate.
3. Terminology
6.2.4 Zero Junction/Reference Junction/Temperature Com-
3.1 Definition
pensated Junction—Must be included.
3.1.1 solidification point of petroleum wax—that tempera-
6.3 TFE-Fluorocarbon Holder Adapter—See Fig. 1 and
ture in the cooling curve of the wax where the slope of the
Fig. 2.
curve first changes significantly as the wax sample changes
6.4 TFE-Fluorocarbon Disk Centering Guide—See Fig. 1
from a liquid to a solid state.
and Fig. 2.
6.5 Test Tubes, 6 by 50-mm.
4. Summary of Test Method
6.6 Vial, 25 by 52-mm.
4.1 A 50-mg sample of wax is placed in a test tube at
6.7 Apparatus for Calibrating Temperature Recorder:
ambient temperature and heated above the solidification point
of the wax sample. A thermocouple probe, attached to a
recorder, is inserted into the wax sample, which is allowed to
Suitable thermocouples are available from: Claud S. Gordon Co., 5710
Kenosha St., Richmond, IL 60071, (815) 678-2211.
cool at room temperature. The thermocouple response of the
For “J” (iron-constantan) junction the following is suitable: Xactpak Type MM
Assembly, Catalog No. 402-1101.
Junction: grounded (G)
This test method is under the jurisdiction of ASTM Committee D-2 on Transition fitting: TH 2780-020
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Thermocouple wire: J30-1-305
D02.10 on Properties of Petroleum Wax (Joint ASTM – TAPPI). L (length of metal sheath)
Current edition approved Oct. 31, 1988. Published January 1989. Originally E (lead length): specify length desired.
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published as D 3944 – 80. Last previous edition D 3944 – 80 (1985) . Not commercially available and hence must be made in a machine shop or
Annual Book of ASTM Standards, Vol 05.01. elsewhere.
D 3944
FIG. 1 Solidification Point Apparatus
FIG. 2 Apparatus for Heating Wax Sample
6.7.1 Stainless Steel Beaker, 1000-mL. 30-W cartridge heater, about 9 by 38 mm, commercially
6.7.2 Heating Mantle, to fit 6.7.1. available (see Fig. 2).
6.7.3 Autotransformer to control heat to 6.7.2. 6.8.2.1 Autotransformer, to control heat in 6.8.2.
6.7.4 Variable-Speed-Stirrer.
7. Procedure
6.7.5 Thermometer, ASTM No. 61C or 61F, 79-mm immer-
sion. 7.1 Calibrate the recorder at least every 60 days when in
6.8 Methods for Heating Specimen: frequent use (see Annex A1).
6.8.1 Hot Air Blower at 1000 W, 1200 W, or other suitable 7.2 Obtain a wax sample representative of the material to be
power. This could be a laboratory or a hou
...
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