ASTM D6269-98e1
(Test Method)Test Method for Solidification Point of p-Xylene (Withdrawn 2004)
Test Method for Solidification Point of <I>p</I>-Xylene (Withdrawn 2004)
SCOPE
1.1 This test method covers the determination of the solidification point of p-Xylene with purity greater than 99.5 %.
Note 1—Other test methods for determining freeze point and solidification point of aromatic hydrocarbons include Test Methods D 852, D 1015, D 1016, and D 1493.
1.2 The following applies to all specified limits in this test method: for purposes of determining conformance with this test method, an observed value or a calculated value shall be rounded off "to the nearest unit" in the last right hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E 29.
1.3 This standard does not purport to address all the safety concerns, if any, associated with its use. It is the responsibility of the user of this test method to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 7.
WITHDRAWN RATIONALE
This test method covers the determination of the solidification point of p-Xylene with purity greater than 99.5 %.
Formerly under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Materials, this test method was withdrawn in December 2004 in accordance with section 10.6.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
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Designation: D 6269 – 98
Test Method for
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Solidification Point of p-Xylene
This standard is issued under the fixed designation D 6269; 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.
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e NOTE—RR: D16–1027 was added editorially in March 2002.
1. Scope 2.2 Other Documents:
OSHA Regulations, 29 CRFR, paragraphs 1910.1000 and
1.1 This test method covers the determination of the solidi-
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1910.1200
fication point of p-Xylene with purity greater than 99.5 %.
NOTE 1—Other test methods for determining freeze point and solidifi- 3. Terminology
cation point of aromatic hydrocarbons include Test Methods D 852,
3.1 Definitions:
D 1015, D 1016, and D 1493.
3.1.1 solidification point—an empirical constant defined as
1.2 The following applies to all specified limits in this test
the temperature at which the liquid phase of a substance is in
method: for purposes of determining conformance with this
approximate equilibrium with a relatively small portion of the
test method, an observed value or a calculated value shall be
solid phase.
roundedoff“tothenearestunit”inthelastrighthanddigitused
3.1.1.1 Discussion—Solidification point as distinguished
in expressing the specification limit, in accordance with the
from freezing point is described in Test Method D 1015.An
rounding-off method of PracticeE29.
interpretation of mole percent in terms of freezing point is
1.3 This standard does not purport to address all the safety
given in Test Method D 1016.
concerns, if any, associated with its use. It is the responsibility
3.1.2 anhydrous—p-xylene that has been treated with 3A
of the user of this test method to establish appropriate safety
molecular sieve to remove water.
and health practices and determine the applicability of regu-
4. Summary of Test Method
latory limitations prior to use. For a specific hazard statement,
see Section 7.
4.1 P-Xylene is dried with a 3-A molecular sieve. The
solidification point is then measured by noting the maximum
2. Referenced Documents
temperature reached after the appearance of a solid phase.
2.1 ASTM Standards:
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5. Significance and Use
D 852 Test Method for Solidification Point of Benzene
D 1015 Test Method for Freezing Point of High-Purity
5.1 This test method may be used for process control during
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Hydrocarbons
the manufacture of p-xylene, for setting specifications, and to
D 1016 Test Method for Purity of Hydrocarbons from
determine if contamination was introduced into the p-xylene
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Freezing Points
during shipment.
D 1493 Test Method for Solidification Point of Industrial
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6. Apparatus
Organic Chemicals
D 3437 Practice for Sampling and Handling Liquid Cyclic
6.1 Temperature Bath, controlled at 10 6 1°C.
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6,7
Products
6.2 Ohm Meter , capable of measuring resistance to the
E29 Practice for Using Significant Digits in Test Data to
nearest 0.1 V in range 1000 to 10 000 V with direct
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Determine Conformance with Specifications
temperature readout.
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This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and are the direct responsibility of
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Subcommittee D16.04 on Instrumental Analysis. Available fro the Superintendent of Documents, U.S. Government Printing
Current edition approved May 10, 1998. Published July 1998. Office, Washington, DC 20402.
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Annual Book of ASTM Standards, Vol 06.04. The sole source of supply of an ohm meter meeting these specifications is the
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Annual Book of ASTM Standards, Vol 05.01. Hart Scientific Model 1504., 220 N. 1300West, P.O. Box 460, Pleasant Grove, Utah
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Annual Book of ASTM Standards, Vol 14.02. 84062.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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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.
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D6269–98
6.3 Sample Container, thick walled test tube with 18-mm 6.5 Stirring Apparatus, (Optional) The apparatus illustrated
outside diameter and 14-mm inside diameter, and 150-mm in Fig. 1 has been demonstrated to be an acceptable replace-
long. ment for manually stirring the p-xylene solution.
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6.4 Stirrer, consisting of a 1-mm copper or stainless steel 6.6 Thermistor —in stainless steel housing with resis-
wire (copper or stainless steel) bent into a circular form at right tance greater than 2 kV at 25°C. Calibration accuracy
angles to the shaft so it will move freely in the annular space 60.005°C. from 0 to 25°C. Drift in resistance equivalent to
between the
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