ASTM D6875-03

Standard Test Method for Solidification Point of Industrial Organic Chemicals by Thermistor

SIGNIFICANCE AND USE
This test method may be used for process control during the manufacture of organic chemicals described in Section 1, for setting specifications, for development and research work, and to determine if contamination was introduced during shipment.
SCOPE
1.1 This test method covers a general procedure for determining the solidification point of most organic chemicals having appreciable heats of fusion and solidification points between 4 and 41°C.
Note 1—Other test methods for determining freeze point and solidification point of aromatic hydrocarbons include Test Methods D 852, D 1015, D 1016, D 1493, D 3799, D 4493, and D 6269.
1.2 This test method is applicable to relatively pure compounds only. Solidification point depression is dependent on impurity concentrations.
1.3 The following applies to all specified limits in this test method: for purposes of determining conformance with applicable specifications using 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.
1.4 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. For a specific hazard statement, see Section 8, Hazards.

General Information

• Status: Historical
• Publication Date: 09-Feb-2003
• ICS: 71.080.01 - Organic chemicals in general
• Technical Committee: D16 - Aromatic, Industrial, Specialty and Related Chemicals
• Drafting Committee: D16.04 - Instrumental Analysis

Relations

• Replaced By: ASTM D6875-08 - Standard Test Method for Solidification Point of Industrial Organic Chemicals by Thermistor
• Effective Date: 01-Oct-2008
• Referred By: ASTM D2439-20 - Standard Specification for Refined Phenol
• Effective Date: 10-Feb-2003
• Referred By: ASTM D7185-19 - Standard Specification for Low Toluene Low Dioxane (LTLD) Benzene
• Effective Date: 10-Feb-2003
• Referred By: ASTM D2359-19 - Standard Specification for Refined Benzene-535
• Effective Date: 10-Feb-2003
• Referred By: ASTM E324-23 - Standard Test Method for Relative Initial and Final Melting Points and the Melting Range of Organic Chemicals
• Effective Date: 10-Feb-2003
• Referred By: ASTM D4734-20 - Standard Specification for Refined Benzene-545
• Effective Date: 10-Feb-2003
• Referred By: ASTM D5871-19 - Standard Specification for Benzene for Cyclohexane Feedstock
• Effective Date: 10-Feb-2003

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 6875 – 03
Standard Test Method for
Solidification Point of Industrial Organic Chemicals by
Thermistor
This standard is issued under the fixed designation D 6875; 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 D 3438 Practice for Sampling and Handling Naphthalene,
Maleic Anhydride, and Phthalic Anhydride
1.1 This test method covers a general procedure for deter-
D 3799 TestMethodforPurityofStyrenebyFreezingPoint
mining the solidification point of most organic chemicals
Method
having appreciable heats of fusion and solidification points
D 3852 Practice for Sampling and Handling Phenol,
between 4 and 41°C.
Cresols, and Cresylic Acid
NOTE 1—Other test methods for determining freeze point and solidifi-
D 4297 Practice for Sampling and Handling Bisphenol A
cation point of aromatic hydrocarbons include Test Methods D 852,
(4,4’-Isoproplyidenediphenol)
D 1015, D 1016, D 1493, D 3799, D 4493, and D 6269.
D 4493 Test Method for Solidification Point of BisphenolA
1.2 This test method is applicable to relatively pure com- 2
(4,4’-Isoproplyidenediphenol)
pounds only. Solidification point depression is dependent on
D 6269 Test Method for Solidification Point of p-Xylene
impurity concentrations.
E 29 Practice for Using Significant Digits in Test Data to
1.3 The following applies to all specified limits in this test
Determine Conformance with Specifications
method: for purposes of determining conformance with appli-
2.2 Other Documents:
cable specifications using this test method, an observed value
OSHA Regulations, 29 CRFR, paragraphs 1910.1000 and
or a calculated value shall be rounded off “to the nearest unit”
1910.1200
in the last right hand digit used in expressing the specification
limit,inaccordancewiththe“rounding-offmethod”ofPractice 3. Terminology
E 29.
3.1 Definitions:
1.4 This standard does not purport to address all of the
3.1.1 solidification point, n—an empirical constant defined
safety concerns, if any, associated with its use. It is the
as the temperature at which the liquid phase of a substance is
responsibility of the user of this standard to establish appro-
in approximate equilibrium with a relatively small portion of
priate safety and health practices and determine the applica-
the solid phase.
bility of regulatory limitations prior to use. For a specific
3.1.1.1 Discussion—Solidification point as distinguished
hazard statement, see Section 8, Hazards.
from freezing point is described in Test Method D 1015. An
interpretation of mole percent in terms of freezing point is
2. Referenced Documents
given in Test Method D 1016.
2.1 ASTM Standards:
4. Summary of Test Method
D 852 Test Method for Solidification Point of Benzene
D 1015 Test Method for Freezing Point of High-Purity
4.1 The solidification point is measured by noting the
Hydrocarbons
maximum temperature reached during a cooling cycle after the
D 1016 Test Method for Purity of Hydrocarbons from
appearance of a solid phase.
Freezing Points
5. Significance and Use
D 1493 Test Method for Solidification Point of Industrial
Organic Chemicals
5.1 This test method may be used for process control during
D 3437 Practice for Sampling and Handling Liquid Cyclic
the manufacture of organic chemicals described in Section 1,
Products
for setting specifications, for development and research work,
and to determine if contamination was introduced during
shipment.
This test method is under the jurisdiction of ASTM Committee D16 on
Packaging and is the direct responsibility of Subcommittee D16.04 on Instrumental
Analysis.
Current edition approved Feb. 10, 2003. Published April 2003. Annual Book of ASTM Standards, Vol 14.02.
2 5
Annual Book of ASTM Standards, Vol 06.04. AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Annual Book of ASTM Standards, Vol 05.01. 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6875–03
6. Apparatus 8. Hazards
6.1 Ohmmeter, capable of measuring resistance to the near- 8.1 Consult current OSHA regulations, supplier’s Material
est 0.1 ohm in the range of 1000 to 10 000 ohms with direct Safety Data Sheets, and local regulations for all materials used
temperature readout. in this procedure.
6.2 Specimen Container, thick walled test tube with 18 mm 8.2 Appropriate personal protection equipment such as
outside diameter and 14 mm inside diameter and 150 mm long. gloves, safety glasses, a long rubber apron, and a full face
6.3 Stirrer, consisting of a 1-mm stainless steel wire bent shield should be worn when handling hot or corrosive chemi-
into a circular form at right angles to the shaft so it will move cals, or both.
freely in the annular space between the thermistor and the wall 8.3 A fume hood should be used when performing the test
of the test tube. method on hazardous chemicals (OSHA1910.1450 definition).
6.4 Stirring Apparatus (Optional)—The apparatus illus-
9. Sampling and Handling
trated in Fig. 1 has been demonstrated to be an acceptable
replacement for manual stirring.
9.1 Sample the material in accordance with Practices
6.5 Temperature Bath, capable of being controlled at 5 6
D 3437, D 3438, D 3852, and D 4297.
1°C below the expected solidification point.
6.6 Thermistor, in stainless steel housing with resistance 10. Preparation of Apparatus
greater than 2K ohms at 25°C. Calibration accuracy 6 0.01°C.
10.1 Fit the sample container with a two-hole stopper.
Drift in resistance equivalent to less than 6 0.01°C/year.
Through one hole insert the thermistor. Through the other hole
Thermistor shall be calibrated to cover the range it is used.
insert the shaft of the stirrer. (See Fig. 1).
10.2 Set temperature bath at 5 6 1°C. below the expected
7. Reagents and Materials
solidification point of the sample.
7.1 Cooling Media:
7.1.1 Water is recommended for solidification points be-
11. Calibration of Thermistor
tween 4 and 30°C.
11.1 Thermistor should be calibrated by the factory at a
7.2 Drying Agents:
minimum every two years.
7.2.1 3A Molecular Sieve, in the form of a powder or
11.2 The thermistor may be checked by determining the ice
cylindrical granules about 3 mm in diameter.
point of water 0.00°C.
12. Sample Preparation
The sole source of supply of the apparatus known to the committee at this time
istheHartScienti
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