ASTM D6269-98

Test Method for Solidification Point of <I>p</I>-Xylene

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.

General Information

• Status: Historical
• Publication Date: 09-May-1998
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

Relations

• Replaced By: ASTM D6269-98e1 - Test Method for Solidification Point of <I>p</I>-Xylene (Withdrawn 2004)
• Effective Date: 10-May-1998

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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: D 6269 – 98
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Test Method for
1
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.
1. Scope 3. Terminology
1.1 This test method covers the determination of the solidi- 3.1 Definitions:
fication point of p-Xylene with purity greater than 99.5 %. 3.1.1 solidification point—an empirical constant defined as
the temperature at which the liquid phase of a substance is in
NOTE 1—Other test methods for determining freeze point and solidifi-
approximate equilibrium with a relatively small portion of the
cation point of aromatic hydrocarbons include Test Methods D 852, D
solid phase.
1015, D 1016, and D 1493.
3.1.1.1 Discussion—Solidification point as distinguished
1.2 The following applies to all specified limits in this test
from freezing point is described in Test Method D 1015. An
method: for purposes of determining conformance with this
interpretation of mole percent in terms of freezing point is
test method, an observed value or a calculated value shall be
given in Test Method D 1016.
rounded off “to the nearest unit” in the last right hand digit used
3.1.2 anhydrous—p-xylene that has been treated with 3A
in expressing the specification limit, in accordance with the
molecular sieve to remove water.
rounding-off method of Practice E 29.
1.3 This standard does not purport to address all the safety
4. Summary of Test Method
concerns, if any, associated with its use. It is the responsibility
4.1 P-Xylene is dried with a 3-A molecular sieve. The
of the user of this test method to establish appropriate safety
solidification point is then measured by noting the maximum
and health practices and determine the applicability of regu-
temperature reached after the appearance of a solid phase.
latory limitations prior to use. For a specific hazard statement,
see Section 7.
5. Significance and Use
5.1 This test method may be used for process control during
2. Referenced Documents
the manufacture of p-xylene, for setting specifications, and to
2.1 ASTM Standards:
determine if contamination was introduced into the p-xylene
2
D 852 Test Method for Solidification Point of Benzene
during shipment.
D 1015 Test Method for Freezing Point of High-Purity
3
Hydrocarbons
6. Apparatus
D 1016 Test Method for Purity of Hydrocarbons from
6.1 Temperature Bath, controlled at 10 6 1°C.
3
Freezing Points
6,7
6.2 Ohm Meter , capable of measuring resistance to the
D 1493 Test Method for Solidification Point of Industrial
nearest 0.1 V in range 1000 to 10 000 V with direct
2
Organic Chemicals
temperature readout.
D 3437 Practice for Sampling and Handling Liquid Cyclic
6.3 Sample Container, thick walled test tube with 18-mm
2
Products
outside diameter and 14-mm inside diameter, and 150-mm
E 29 Practice for Using Significant Digits in Test Data to
long.
4
Determine Conformance with Specifications
6.4 Stirrer, consisting of a 1-mm copper or stainless steel
2.2 Other Documents:
wire (copper or stainless steel) bent into a circular form at right
OSHA Regulations, 29 CRFR, paragraphs 1910.1000 and
angles to the shaft so it will move freely in the annular space
5
1910.1200
between the thermistor and the wall of the test tube.
6.5 Stirring Apparatus, (Optional) The apparatus illustrated
in Fig. 1 has been demonstrated to be an acceptable replace-
1 ment for manually stirring the p-xylene solution.
This test method is under the jurisdiction of ASTM Committee D-16 on
Aromatic Hydrocarbons and Related Chemicals and are the direct responsibility of
Subcommittee D16.0E on Instrumental Analysis.
6
Current edition approved May 10, 1998. Published July 1998.
The sole source of supply of an ohm meter meeting these specifications is the
2
Annual Book of ASTM Standards, Vol 06.04.
Hart Scientific Model 1504., 220 N. 1300 West, P.O. Box 460, Pleasant Grove, Utah
3
Annual Book of ASTM Standards, Vol 05.01.
84062.
4
7
Annual Book of ASTM Standards, Vol 14.02.
If you are aware of alternative suppliers, please provide this information to
5
Available fro the Superintendent of Documents, U.S. Government Printing
ASTM Headquarters. Your comments will receive careful consideration at a meeting
Office, Washington, DC 20402.
of the responsible technical committee, D-16, which you may attend.
1

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D 6269
FIG. 1 p-Xylene Solidification Point Apparatus
7,8
6.6 Thermistor —in stainl
...