Standard Test Method for Solidification Point of Petroleum Wax

SIGNIFICANCE AND USE
The related methods of determining the melt point of petroleum wax are relatively time-consuming. This method endeavors to reduce the duration of testing significantly and at the same time maintain a reasonable precision. This method can be useful for quality control of petroleum waxes as well as research and product development work on these waxes.
For methods used for testing melt points of petroleum waxes, see Tests Method D 87, D 127, including Petrolatum and Test Method D 938.
SCOPE
1.1 This test method covers 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 stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3This 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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Publication Date
30-Apr-2005
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ASTM D3944-88(2005) - Standard Test Method for Solidification Point of Petroleum Wax
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D3944 −88(Reapproved2005)
StandardTest Method for
Solidification Point of Petroleum Wax
This standard is issued under the fixed designation D3944; 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 of the wax sample. A thermocouple probe, attached to a
recorder, is inserted into the wax sample, which is allowed to
1.1 This test method covers a procedure for rapidly deter-
cool at room temperature. The thermocouple response of the
mining the solidification point of petroleum wax.
cooling wax traces a curve on the chart paper of the recorder.
NOTE1—Thistestmethodisalsoapplicabletosimilarmaterialssuchas
The first significant change in the slope of the curve is the
synthetic waxes but the precision may vary.
solidification point.
1.2 The values stated in SI units are to be regarded as the
5. Significance and Use
standard. The values given in parentheses are for information
only.
5.1 The related methods of determining the melt point of
petroleum wax are relatively time-consuming. This method
1.3 This standard does not purport to address all of the
endeavors to reduce the duration of testing significantly and at
safety problems, if any, associated with its use. It is the
the same time maintain a reasonable precision. This method
responsibility of the user of this standard to establish appro-
can be useful for quality control of petroleum waxes as well as
priate safety and health practices and determine the applica-
research and product development work on these waxes.
bility of regulatory limitations prior to use.
5.2 For methods used for testing melt points of petroleum
2. Referenced Documents
waxes, seeTests Method D87, D127, including Petrolatum and
2.1 ASTM Standards:
Test Method D938.
D87 Test Method for Melting Point of Petroleum Wax
6. Apparatus
(Cooling Curve)
D127 Test Method for Drop Melting Point of Petroleum
6.1 Thermocouple, with an iron-constantan junction.
Wax, Including Petrolatum
6.2 Recorder capable of recording voltage and equipped
D938 Test Method for Congealing Point of Petroleum
with a time-base module. The recorder should have the
Waxes, Including Petrolatum
following minimum specifications:
E1 Specification for ASTM Liquid-in-Glass Thermometers
6.2.1 Span, 0 to 10 mV or other suitable ranges.
3. Terminology 6.2.2 Accuracy, 0.25 % of full scale.
6.2.3 Step Response Time,1-sfullscale,3-sfullscaleisalso
3.1 Definitions: Related to This Standard:
appropriate.
3.2 solidification point of petroleum wax—that temperature
6.2.4 Zero Junction/Reference Junction/Temperature Com-
in the cooling curve of the wax where the slope of the curve
pensated Junction—Must be included.
first changes significantly as the wax sample changes from a
6.3 TFE-Fluorocarbon HolderAdapter—SeeFig.1andFig.
liquid to a solid state.
2.
4. Summary of Test Method
6.4 TFE-Fluorocarbon Disk Centering Guide—See Fig. 1
4.1 A 50-mg sample of wax is placed in a test tube at
and Fig. 2.
ambient temperature and heated above the solidification point
Suitable thermocouples are available from: Claud S. Gordon Co., 5710
This test method is under the jurisdiction of ASTM Committee D02 on Kenosha St., Richmond, IL 60071, (815) 678-2211. For “J” (iron-constantan)
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee junction the following is suitable: Xactpak Type MM Assembly, Catalog No.
D02.10.0A on Physical/Chemical Properties. 402-1101.
Current edition approved May 1, 2005. Published May 2005. Originally Junction: grounded (G)
approved in 1980. Last previous edition approved in 2000 as D3944 – 88 (2000). Transition fitting: TH 2780-020
DOI: 10.1520/D3944-88R05. Thermocouple wire: J30-1-305
For referenced ASTM standards, visit the ASTM website, www.astm.org, or L (length of metal sheath)
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM E (lead length): specify length desired.
Standards volume information, refer to the standard’s Document Summary page on Not commercially available and hence must be made in a machine shop or
the ASTM website. elsewhere.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3944−88(Reapproved2005)
FIG. 1 Solidification Point Apparatus
FIG. 2 Apparatus for Heating Wax Sample
6.5 Test Tubes, 6 by 50-mm. 6.8.2 Aluminum Heating Block, about 50 by 50 by 50 mm.
In the center of one face of the block, a hole is made 7 mm in
6.6 Vial, 25 by 52-mm.
diameter and 37 mm deep to accommodatea6by 50-mm test
6.7 Apparatus for Calibrating Temperature Recorder:
tube and another hole adjacent to it to accommodate a 110-V,
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.
6.7.5 Thermometer,ASTM No. 61C or 61F, 79-mm immer-
7. Procedure
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
power. This could be a laboratory or a household
...

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