ASTM D1493-97
(Test Method)Standard Test Method for Solidification Point of Industrial Organic Chemicals (Withdrawn 2004)
Standard Test Method for Solidification Point of Industrial Organic Chemicals (Withdrawn 2004)
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 -20 and +150°C.
1.2 This test method is applicable only to relatively pure compounds. Values obtained for grossly impure compounds can be low because of the freezing out of one component during the determination.
1.3 In order that the test method may be used on many materials, a choice of certain alternatives and a selection of apparatus are permitted. The report (Section 12) requires that the selected alternatives must be stated. Materials to which the test method is applicable in particular detail include phenol, naphthalene, phthalic anhydride, and maleic anhydride.
Note 1-A companion test method is Test Method D 852.
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 specific hazard statements, see Section 8.
WITHDRAWN RATIONALE
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 20 and +150C.
Formerly under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals, this test method was withdrawn in June 2004 in accordance with section 10.6.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
Designation: D 1493 – 97
Standard Test Method for
Solidification Point of Industrial Organic Chemicals
This standard is issued under the fixed designation D1493; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D1016 Test Method for Purity of Hydrocarbons from
Freezing Points
1.1 This test method covers a general procedure for deter-
D3437 Practice for Sampling and Handling Liquid Cyclic
mining the solidification point of most organic chemicals
Products
having appreciable heats of fusion and solidification points
D3438 Practice for Sampling and Handling Naphthalene,
between−20 and+150°C.
Maleic Anhydride, and Phthalic Anhydride
1.2 This test method is applicable only to relatively pure
D3852 Practice for Sampling and Handling Phenol and
compounds. Values obtained for grossly impure compounds
Cresyl Acid
can be low because of the freezing out of one component
E1 Specification for ASTM Thermometers
during the determination.
E29 Practice for Using Significant Digit in Test Data to
1.3 In order that the test method may be used on many
Determine Conformance with Specifications
materials, a choice of certain alternatives and a selection of
E77 Test Method for Inspection and Verification of Ther-
apparatus are permitted. The report (Section 12) requires that
mometers
the selected alternatives must be stated. Materials to which the
2.2 Other Document:
test method is applicable in particular detail include phenol,
OSHA Regulations, 29 CFR, paragraphs 1910.1000 and
naphthalene, phthalic anhydride, and maleic anhydride.
1910.1200
1.4 The following applies to all specified limits in this test
method: for purposes of determining conformance with this
3. Terminology
test method, an observed value or a calculated value shall be
3.1 Definitions:
rounded off “to the nearest unit” in the right-hand digit used in
3.1.1 solidification point—an empirical constant defined as
expressing the specification limit, in accordance with the
the temperature at which the liquid phase of a substance is in
rounding-off method of Practice E29E29.
approximate equilibrium with a relatively small amount of the
NOTE 1—A companion test method is Test Method D852D852.
same substance in its solid phase.
3.1.1.1 Discussion—Solidification point is distinguished
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the from freezing point, which is described in Test Method
D1015D1015. An interpretation of mole percent purity in
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- termsoffreezingpointisgiveninTestMethodD1016D1016.
bility of regulatory limitations prior to use. For specific hazard
4. Summary of Test Method
statements, see Section 8.
4.1 Solidificationpointismeasuredbynotingthemaximum
2. Referenced Documents
temperaturereachedduringacontrolledcoolingcycleafterthe
2.1 ASTM Standards: appearance of a solid phase in a liquid sample.
D850 Test Method for Distillation of Industrial Aromatic
2 5. Significance and Use
Hydrocarbons and Related Materials
5.1 This test method is suitable for setting specifications on
D852 Test Method for Solidification Point of Benzene
compoundsofthetypedescribedinSection1.Itisalsosuitable
D1015 Test Method for Freezing Points of High Purity
for use as an intense quality-control tool and in development
Hydrocarbons
and research work involving these compounds.
This test method is under the jurisdiction of ASTM Committee D-16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
Subcommittee D16.0E on Instrumental Analysis.
Current edition approved Feb. 10, 1997. Published September 1997. Originally Annual Book of ASTM Standards, Vol 14.03.
published as D1493–57T. Last previous edition D1493–92. Annual Book of ASTM Standards, Vol 14.02.
2 6
Annual Book of ASTM Standards, Vol 06.04. Available from Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 05.01. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
D1493–97
6. Apparatus series of three circular loops about 25 mm apart at right angles
to the shaft, the circle of each loop being about 20 mm in
6.1 Thermometer—An etched-stem liquid-in-glass ther-
diameter, so that the stirrer can move freely in the annular
mometerhavingarangeofnomorethan30°Cshallbeused.It
spacebetweentheinnerwallofthespecimencontainerandthe
shall be graduated in subdivisions no greater than 0.1°C.
thermometer stem when the latter is inserted in the container.
Unless otherwise specified, it shall be calibrated, for 76-mm
Theshaftofthestirrermaybeofanyconvenientlengthnotless
immersion, at no fewer than three points. These shall include
than 150 mm, and shall pass through an off-center hole in a
theapproximatesolidificationpointofthematerialbeingtested
two-hole cork stopper, the center hole of which holds the
and two other points, respectively, about 5°C above and below
thermometer. The upper end of the shaft may be attached to a
the solidification point.Atotal immersion thermometer can be
reciprocatingdeviceformechanicalstirring,ormaybeformed
used if it is specified for testing a particular material, as, for
into a loop to facilitate lifting it for stirring by hand.
example, benzene. (See Test Method D852D852.) The ther-
6.4 Flasks:
mometershallconformtoSpecificationE1E1.Itshouldbeso
6.4.1 A 200-mL, side-tube, heat-resistant glass distillation
chosenthatthegraduationatwhichthesolidificationpointisto
flask as described in Test Method D850D850 and
be observed is not hidden from view when the thermometer is
6.4.2 Two narrow-neck, heat-resistant glass Erlenmeyer
inserted in the sample container. Suitable thermometers are
flasks, 400-mL capacity each.
ASTM Thermometers 89C to 96C, inclusive. Table 1 lists
6.5 Heaters:
several of these thermometers and the materials for which,
6.5.1 A hot plate, and
respectively, they are useful in particular in accordance with
6.5.2 An electric heater that is fully adjustable as described
this test method. A thermometer, for example ASTM Ther-
in Test Method D850D850, or a bunsen or similar gas burner
mometer 17C, 18C, or 91C, is needed when the average
(see Section 9.2), or both.
temperature of the emergent mercury column of the
6.6 Insulation Board—Asheet of hard insulation board 3 to
solidification-point thermometer is measured.
TABLE 1 ASTM Thermometers for Solidification Point
Selected Standardization Average Temperature of Emergent
ASTM Number Range of Temperature, °C Material for Test
Temperature,° C Mercury Column, °C
91C 20 to 50 40 25 phenol
92C 40 to 70 52 25 maleic anhydride
93C 60 to 90 80 30 naphthalene
96C 120 to 150 130 35 phthalic anhydride
6.2 Specimen Container—A standard heat-resistant glass 6-mm thick and 15 cm square, with a circular hole 50 mm in
test tube with lip shall be used. The test tube shall measure 25 diameter in the center of it, is needed if the drying procedure
mm in outside diameter and 150 mm in length. given in 9.2 is used.
6.3 Stirrer (see Fig. 1)—The stirrer shall consist of a 1-mm
NOTE 2—Items described in 6.7, 6.8, and 6.9, are not essential for
diameter (B&S gage 18), corrosion-resistant wire bent into a
routinely testing materials that have solidification points substantially
aboveroomtemperature,forexampleabove30°C;but,forrefereetesting,
these items shall be used always, regardless of the solidification points of
the materials being tested.
6.7 Air Jacket—A standard heat-resistant glass tube with
lip, 38 mm in outside diameter and 200 mm in length, shall be
fitted with a cork stopper bored with a hole of 25 to 26-mm
diameter and into which the specimen container is to be
inserted up to its lip.
6.8 Cooling Bath—A 2-L beaker or similar suitable con-
tainer having an effective depth of at least 175 mm shall be
filled with a cooling medium, which shall be glycerin for
operatingattemperaturesbetween145and25°C,waterandice
between 25 and 0°C, and alcohol and dry ice between 0
and−25°C.Athermostatically controlled agitated bath may be
used optionally. (See Fig. 2 for assembly of apparatus.)
6.9 Clamp and Ring Stand—A clamp, attached to a stand,
holds the air jacket rigidly just below its lip when it is
immersed in the cooling bath to a depth between 160 and 200
mm.
NOTE 3—Items listed in 6.10-6.15 inclusive, are required only for
checkingtheaccuracyofthethermometeratthesolidificationpointofthe
FIG. 1 Stirrer material being tested. This check is desirable to detect changes that occur
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
D1493–97
thermometer, the lengths of the cell and the well shall be
increased to fit. The cell shall have a calibration temperature,
T , determined with a platinum resistance thermometer and
c
assigned to it for use as a thermometric standard. (See Section
10.)
6.11 Vacuum Flask—An open-mouthed Dewar-type of
vacuum-jacketed flask is needed. Its capacity shall be nomi-
nally 500-mL in size. It shall be provided with a base to hold
it upright. (See Fig. 4.)
6.12 Oven—An electrically heated oven, preferably with
internal circulation of air, shall be used if the crystallizable
compound described in 6.9 is solid at room temperature. The
oven must be thermostatically controlled over the temperature
rangeof60to200°Cwithtoleranceof 610°Catanysettingin
this range. Its chamber must be large enough to hold the items
described in 6.10, 6.11, 6.12 and 6.13 at the same time. A
chamber of satisfactory size shall be cubic, 500 mm to a side.
A thermometer shall be inserted at the top with its bulb about
125 mm below the ceiling of the chamber.
6.13 Cradle—Two pieces of fireproof, 6.4-mm board are
needed to support the thermometric cell in the oven. The
FIG. 2 Apparatus for Determining Solidification Point
dimensions of each piece shall be about 120 mm in length, 70
mm in width, and between 6 and 12 mm in thickness.
in a thermometer with time and use and to minimize errors generally.
6.14 Safety Items—For personal protection when handling
6.10 Thermometric Cell—A sealed glass cell made from
fragile cells with contents of a molten compound that is a
standard-wall glass tubing, 38 mm in outside diameter, and
skin-irritant or that has a melting point above 60°C, the
about 140 mm in length, has a thermometer well, 120-mm
operatorwillneedapairofheat-resistantgloves,alongrubber
deep, formed as an integral part lengthwise in it. The cell
apron, and a transparent visor.
contains a relatively pure crystallizable compound of known
6.15 Magnifying Glass—For accurately reading the tem-
freezing point that fills it to a level about 10 mm above the
perature indicated by the thermometer, it is advantangeous to
height of the 76-mm immersion mark of a partial immersion
use a magnifying glass, provided with an eyepiece and a
thermometer when the latter is inserted in the well down to the
cross-hair, and mounted on a friction-slide that fits over the
bottom. The well shall be made from 10-mm tubing, about 8
thermometer stem.
mm in inside diameter. (See Fig. 3.) For a total immersion
7. Reagents and Materials
7.1 Cork Stoppers—Suitable corks to be used as described
Enagonio, D. P., Pearson, E. G., and Saylor, C. P. Temperature—Its Measure-
in 6.2, 6.3, and 6.4.
ment and Control in Science and Industry, Reinhold Publishing Corp., New York,
NY, Vol 3, Part 1, 1962, pp. 219–230.
FIG. 3 Thermometric Reference Cell FIG. 4 Reference Cell in Vacuum Flask
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
D1493–97
7.2 Cooling Medium—Technical grade glycerin, technical sample from the drying agent and repeat the procedure with
grademethanolordenaturedalcohol,water,ice,anddryicefor fresh drying agent on the same sample. After drying the
use with the cooling bath. sample, proceed as described in 10.1.
7.3 Drying Agents—Amolecular sieve zeolite with 4Asize 10.4 In an alternative method, when specified, dry the
of pores shall be used for drying liquid hydrocarbons and sample by heating it to its initial boiling point. Support the
phenol. The zeolite may be in the form of a powder or of distillation flask on the asbestos board over the bunsen burner
cylindrical granules about 3 mm in diameter. The granules are or the electric heater by means of the ring stand. Attach the
preferred. The pore size is critical, because pores larger than clamp to the lower part of the neck of the flask.Transfer about
4A will absorb some hydrocarbons preferentially. Sodium 100 g of the sample to the flask and place a solid cork stopper
hydroxide pellets can be used for drying liquid hydrocarbons intheneck.Heattheflaskslowlyandallowthesampletomelt
and other nonacidic compounds. Anhydrous calcium sulfate and then to boil gently. Any water present in the sample will
granules, free of dust, can also be used. condense in the neck of the flask. If considerable water is
7.4 Packing Materials—Cotton wadding, cloth wipers, and present, it will distill out of the side tube of the flask and it
glass wool for packing around glass cells of hot, molten should be collected in a receiver and then discarded. This
compounds. Thin aluminum foil, light duty wrap, will also be method shall not be used for materials that have initial boiling
needed as described in 10.10. points below 80°C or above 260°C. Allow the dry condensed
liquid to rise in the neck of the flask by further heating, for not
more than 1 min, until the liquid just reaches the side tube.
8. Hazards
Removethesourceofheatandthestopper.Letthesamplecool
8.1 Consult current OSHA regulations, supplier’s Material
for 1 min.Then warm the neck of the flask above the side tube
Safety Data Sheets, and local regulations for all materials used
with a very small flame of the bunsen burner to drive off any
in this test method.
condensedmoisture.Thenstoppertheflaskwithadrycork.Let
the sample cool until it can be poured conveniently and safely;
9. Sampling and Handling
while its t
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