ASTM D87-09(2014)
(Test Method)Standard Test Method for Melting Point of Petroleum Wax (Cooling Curve)
Standard Test Method for Melting Point of Petroleum Wax (Cooling Curve)
SIGNIFICANCE AND USE
5.1 Melting point (cooling curve) is a test that is widely used by wax suppliers and consumers. it is particularly applied to petroleum waxes that are rather highly paraffinic or crystalline in nature. A plateau occurs with specimens containing appreciable amounts of hydrocarbons that crystallize at the same temperature, giving up heat of fusion, thus temporarily retarding the cooling rate. In general, petroleum waxes with large amounts of non-normal hydrocarbons or with amorphous solid forms will not exhibit a plateau.
SCOPE
1.1 This test method covers the determination of the melting point (cooling curve) of petroleum wax. It is unsuitable for waxes of the petrolatum group, microcrystalline waxes, or blends of such waxes with paraffin wax or scale wax.
Note 1: For additional methods used for testing petroleum waxes, see Test Method D127 and Test Method D938. Results may differ, depending on the method used. For pharmaceutical petrolatum, Test Method D127 usually is used.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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.
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Designation: D87 − 09 (Reapproved 2014) Technical Association of Pulp
and Paper Industry
Standard Method T 630m-61
Method 1402-Federal Test
Method Standard No. 791b
British Standard 4695
Designation: 55/77(83)
Standard Test Method for
Melting Point of Petroleum Wax (Cooling Curve)
This standard is issued under the fixed designation D87; 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.Asuperscript
epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope E1 Specification for ASTM Liquid-in-Glass Thermometers
1.1 Thistestmethodcoversthedeterminationofthemelting
3. Terminology
point (cooling curve) of petroleum wax. It is unsuitable for
3.1 Definitions:
waxes of the petrolatum group, microcrystalline waxes, or
3.1.1 melting point (cooling curve) of petroleum wax—
blends of such waxes with paraffin wax or scale wax.
temperature at which melted petroleum wax first shows a
NOTE 1—For additional methods used for testing petroleum waxes, see
minimum rate of temperature change when allowed to cool
Test Method D127 and Test Method D938. Results may differ, depending
under prescribed conditions.
on the method used. For pharmaceutical petrolatum, Test Method D127
3.1.1.1 Discussion—The so-called “American Melting
usually is used.
Point” is arbitrarily 1.65°C (3°F) above the Melting Point
1.2 The values stated in SI units are to be regarded as the
(Cooling Curve) of Petroleum Wax.
standard. The values given in parentheses are for information
only.
4. Summary of Test Method
1.3 This standard does not purport to address all of the
4.1 In ProcedureA(Manual Method), a specimen of molten
safety concerns, if any, associated with its use. It is the
wax in a test tube fitted with a thermometer or equivalent
responsibility of the user of this standard to establish appro-
temperature measuring device is placed in an air bath, which in
priate safety and health practices and determine the applica-
turn is surrounded by a water bath held at 16 to 28°C (60 to
bility of regulatory limitations prior to use.
80°F). As the molten wax cools, periodic readings of its
temperature are taken. When solidification of the wax occurs,
2. Referenced Documents
the rate of temperature change decreases, yielding a plateau in
the cooling curve. The temperature at that point is recorded as
2.1 ASTM Standards:
D127 Test Method for Drop Melting Point of Petroleum the melting point (cooling curve) of the sample.
Wax, Including Petrolatum
4.2 In Procedure B, an automatic analyzer is used. As the
D938 Test Method for Congealing Point of Petroleum
molten wax cools, the sample temperature decrease is mea-
Waxes, Including Petrolatum
sured every 15 s in 0.01°C (0.1°F) readings. The melting point
D6299 Practice for Applying Statistical Quality Assurance
is considered to be reached when five consecutive measure-
and Control Charting Techniques to Evaluate Analytical
ments are constant within a given temperature interval, usually
Measurement System Performance
0.1°C (0.2°F).
5. Significance and Use
This test method is under the jurisdiction of ASTM Committee D02 on
5.1 Melting point (cooling curve) is a test that is widely
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.10.0A on Physical/Chemical Properties.
used by wax suppliers and consumers. it is particularly applied
In the IP, this test method is under the jurisdiction of the Standardization
to petroleum waxes that are rather highly paraffinic or crystal-
Committee. This test method was adopted as a joint ASTM-IP standard in 1966.
line in nature. A plateau occurs with specimens containing
CurrenteditionapprovedMay1,2014.PublishedJuly2014.Originallyapproved
appreciable amounts of hydrocarbons that crystallize at the
in 1921. Last previous edition approved in 2009 as D87 – 09. DOI: 10.1520/D0087-
09R14.
same temperature, giving up heat of fusion, thus temporarily
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
retarding the cooling rate. In general, petroleum waxes with
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
large amounts of non-normal hydrocarbons or with amorphous
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. solid forms will not exhibit a plateau.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D87 − 09 (2014)
NOTE 3—If no plateau appears as defined above, the reading procedure
6. Apparatus
is continued until either (1) the temperature reached 38°C (100°F) or (2)
6.1 The necessary apparatus for ProcedureAis described in
the temperature reaches a point 8°C (15°F) below a temperature where the
Annex A1.
wax has solidified (as may be observed through a transparent bath). In
either of these cases the test is discontinued and the method is judged Not
6.2 The automatic instrument consists of a bath (for
Applicable for the sample (see Note 1 for other methods).
example, an aluminum block with two measuring locations,
9. Procedure B (Automatic Method)
two apertures to place the test tubes, and two apertures for the
temperature probes). The apparatus may have an accessory
9.1 Place a clean test tube held in a PTFE holder ring in the
digital display and a printer.
aperture provided in the apparatus.
6.2.1 The temperature of the bath is maintained between 22
9.2 Insert the temperature probe into a centrally bored,
and 26°C (72 and 79°F). A heating device is used to increase
one-holed stopper, and insert it in the test tube. Check the
the temperature, and a cooling device with cold water circula-
probe height to reach manufacturer’s suggested height. Place
tion is used to decrease the temperature.
the stopper with the probe back in the resting holder provided.
6.2.2 The temperature may be monitored with a calibrated
9.3 Bring the sample to a temperature at least 8°C (15°F)
thermometer or an electronic temperature measuring device of
above the expected melting point. Heat the sample in a 93°C
equivalent precision and accuracy.
(200°F) maximum temperature water bath.
6.3 Other types of equivalent automatic apparatus are ac-
9.4 Add the molten sample to the test tube to the filling
ceptable.
mark. Place the stopper with the probe on the test tube
assembly.
7. Test Specimen
9.5 Insert the assembly into the aluminum block aperture,
7.1 Obtain a sample of wax representative of the shipment
and initiate the analysis in accordance with the manufacturer’s
to be tested. From each test unit obtain a portion of wax
instructions.
weighing at least 25 g for each melting point determination.
9.6 When the melting point is detected, the analysis will
8. Procedure A (Manual Method)
automatically stop. Per available options on the instrument, the
resultingmeltingpointwillbedisplayedonthedigitalmonitor,
8.1 Support the air bath in its proper position in the water
1 or printed on a printer, or both.
bath. Fill the water bath to within 13 mm ( ⁄2 in.) of the top
with water at a temperature of 16 to 28°C (60 to 80°F). The
10. Calculation and Report
bath temperature is kept within these limits throughout the test.
10.1 When using a manual apparatus, average the first five
8.2 Heat the wax sample to at least 8°C (15°F) above its
consecutive temperature readings of the identified plateau,
expected melting point (see Note 2). To heat the wax sample
which agree within 0.1°C (0.2°F). Correct this average for
use a suitable container in an oven or water bath which is held
error in the thermometer scale where necessary.
at a temperature not exceeding 93°C (200°F).Avoid the use of
10.2 The automatic apparatus will average the first five
direct heat such as flame or hot plate. Do not keep the sample
consecutive temperature probe readings within 60.1°C
in the molten state longer than 1 h.
(60.2°F).
NOTE 2—If no estimate of the melting point is available, heat the wax
10.3 Report the result to at least the nearest 0.05°C (0.1°F)
sample to 10°C (15°F) above the temperature at which the wax is
as the Petroleum Wax Melting Point (Cooling Curve), Test
completely molten, or to from 90 to 93°C (195 to 200°F) before
proceeding to the next step. Method D87. Also report whether the test was performed
manually or using automatic apparatus, as applicable.
8.3 Fill the test tube to a height of 51 mm (2 in.) with the
melted sample. Insert the melting point temperature measuring
11. Quality Control (QC)
device through the center of a one-holed stopper, such as a
11.1 Confirm the performance of the instrument or the test
cork. In the case of a thermometer, position the 79-mm
procedure by analyzing a quality control (QC) sample.
(3 ⁄8-in.) immersion line at the lower surface of the stopper.
11.1.1 When QC/Quality Assurance (QA) protocols are
Insert the
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D87 − 09 D87 − 09 (Reapproved 2014) Technical Association of Pulp
and Paper Industry
Standard Method T 630m-61
Method 1402-Federal Test
Method Standard No. 791b
British Standard 4695
Designation: 55/77(83)
Standard Test Method for
Melting Point of Petroleum Wax (Cooling Curve)
This standard is issued under the fixed designation D87; 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*Scope
1.1 This test method covers the determination of the melting point (cooling curve) of petroleum wax. It is unsuitable for waxes
of the petrolatum group, microcrystalline waxes, or blends of such waxes with paraffin wax or scale wax.
NOTE 1—For additional methods used for testing petroleum waxes, see Test Method D127 and Test Method D938. Results may differ, depending on
the method used. For pharmaceutical petrolatum, Test Method D127 usually is used.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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.
2. Referenced Documents
2.1 ASTM Standards:
D127 Test Method for Drop Melting Point of Petroleum Wax, Including Petrolatum
D938 Test Method for Congealing Point of Petroleum Waxes, Including Petrolatum
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
E1 Specification for ASTM Liquid-in-Glass Thermometers
3. Terminology
3.1 Definitions:
3.1.1 melting point (cooling curve) of petroleum wax—temperature at which melted petroleum wax first shows a minimum rate
of temperature change when allowed to cool under prescribed conditions.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.10.0A on Physical/Chemical Properties.
In the IP, this test method is under the jurisdiction of the Standardization Committee. This test method was adopted as a joint ASTM-IP standard in 1966.
Current edition approved Dec. 1, 2009May 1, 2014. Published December 2009July 2014. Originally approved in 1921. Last previous edition approved in 20072009 as
D87D87 – 09.–07a. DOI: 10.1520/D0087-09.10.1520/D0087-09R14.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3.1.1.1 Discussion—
The so-called “American Melting Point” is arbitrarily 1.65°C (3°F) above the Melting Point (Cooling Curve) of Petroleum Wax.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D87 − 09 (2014)
4. Summary of Test Method
4.1 In Procedure A (Manual Method), a specimen of molten wax in a test tube fitted with a thermometer or equivalent
temperature measuring device is placed in an air bath, which in turn is surrounded by a water bath held at 16 to 28°C (60 to 80°F).
As the molten wax cools, periodic readings of its temperature are taken. When solidification of the wax occurs, the rate of
temperature change decreases, yielding a plateau in the cooling curve. The temperature at that point is recorded as the melting point
(cooling curve) of the sample.
4.2 In Procedure B, an automatic analyzer is used. As the molten wax cools, the sample temperature decrease is measured every
15 s in 0.01°C (0.1°F) readings. The melting point is considered to be reached when five consecutive measurements are constant
within a given temperature interval, usually 0.1°C (0.2°F).
5. Significance and Use
5.1 Melting point (cooling curve) is a test that is widely used by wax suppliers and consumers. it is particularly applied to
petroleum waxes that are rather highly paraffinic or crystalline in nature. A plateau occurs with specimens containing appreciable
amounts of hydrocarbons that crystallize at the same temperature, giving up heat of fusion, thus temporarily retarding the cooling
rate. In general, petroleum waxes with large amounts of non-normal hydrocarbons or with amorphous solid forms will not exhibit
a plateau.
6. Apparatus
6.1 The necessary apparatus for Procedure A is described in Annex A1.
6.2 The automatic instrument consists of a bath (for example, an aluminum block with two measuring locations, two apertures
to place the test tubes, and two apertures for the temperature probes). The apparatus may have an accessory digital display and
a printer.
6.2.1 The temperature of the bath is maintained between 22 and 26°C (72 and 79°F). A heating device is used to increase the
temperature, and a cooling device with cold water circulation is used to decrease the temperature.
6.2.2 The temperature may be monitored with a calibrated thermometer or an electronic temperature measuring device of
equivalent precision and accuracy.
6.3 Other types of equivalent automatic apparatus are acceptable.
7. Test Specimen
7.1 Obtain a sample of wax representative of the shipment to be tested. From each test unit obtain a portion of wax weighing
at least 25 g for each melting point determination.
8. Procedure A (Manual Method)
8.1 Support the air bath in its proper position in the water bath. Fill the water bath to within 13 mm ( ⁄2 in.) of the top with water
at a temperature of 16 to 28°C (60 to 80°F). The bath temperature is kept within these limits throughout the test.
8.2 Heat the wax sample to at least 8°C (15°F) above its expected melting point (see Note 2). To heat the wax sample use a
suitable container in an oven or water bath which is held at a temperature not exceeding 93°C (200°F). Avoid the use of direct heat
such as flame or hot plate. Do not keep the sample in the molten state longer than 1 h.
NOTE 2—If no estimate of the melting point is available, heat the wax sample to 10°C (15°F) above the temperature at which the wax is completely
molten, or to from 90 to 93°C (195 to 200°F) before proceeding to the next step.
8.3 Fill the test tube to a height of 51 mm (2 in.) with the melted sample. Insert the melting point temperature measuring device
through the center of a one-holed stopper, such as a cork. In the case of a thermometer, position the 79-mm (3 ⁄8-in.) immersion
line at the lower surface of the stopper. Insert the stopper into the test tube so that the bottom of the thermometer bulb or
temperature measuring probe is 10 mm ( ⁄8 in.) from the bottom of the test tube. Support the test tube assembly in the air bath,
as shown in Fig. A1.1, while the temperature of the molten wax is still at least 8°C (15°F) above its expected melting point (Note
2).
8.4 Take a temperature reading every 15 s. Record each reading to at least the nearest 0.05°C (0.1°F). Monitor the progress of
these sequential readings to determine the appearance of the plateau. Identify the plateau as the first five consecutive readings all
of which agree within 0.1°C (0.2°F). You may discontinue the test after obtaining these five plateau readings.
NOTE 3—If no plateau appears as defined above, the reading procedure is continued until either (1) the temperature reached 38°C (100°F) or (2) the
temperature reaches a point 8°C (15°F) below a temperature where the wax has solidified (as may be observed through a transparent bath). In either of
these cases the test is discontinued and the method is judged Not Applicable for the sample (see Note 1 for other methods).
9. Procedure B (Automatic Method)
9.1 Place a clean test tube held in a PTFE holder ring in the aperture provided in the apparatus.
D87 − 09 (2014)
9.2 Insert the temperature probe into a centrally bored, one-holed stopper, and insert it in the test tube. Check the probe height
to reach manufacturer’s suggested height. Place the stopper with the probe back in the resting holder provided.
9.3 Bring the sample to a temperature at least 8°C (15°F) above the expected melting point. Heat the sample in a 93°C (200°F)
maximum temperature water bath.
9.4 Add the molten sample to the test tube to the filling mark. Place the stopper with the probe on the test tube assembly.
9.5 Insert the assembly into the aluminum block aperture, and initiate the analysis in accordance with the manufacturer’s
instructions.
9.6 When the melting point is detected, the analysis will automatically stop. Per available options on the instrument, the
resulting melting point will be displayed on the digital moni
...
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