Designation: D87 − 09

Designation: 55/77(83) Technical Association of Pulp

and Paper Industry
Standard Method T 630m-61
Method 1402-Federal Test
Method Standard No. 791b
British Standard 4695

Standard Test Method for

Melting Point of Petroleum Wax (Cooling Curve)1
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* E1 Specification for ASTM Liquid-in-Glass Thermometers

1.1 This test method covers the determination of the melting 3. Terminology
point (cooling curve) of petroleum wax. It is unsuitable for
waxes of the petrolatum group, microcrystalline waxes, or 3.1 Definitions:
blends of such waxes with paraffin wax or scale wax. 3.1.1 melting point (cooling curve) of petroleum 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
usually is used. 3.1.1.1 Discussion—The so-called “American Melting
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 Procedure A (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
2.1 ASTM Standards:2 the cooling curve. The temperature at that point is recorded as
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
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 5.1 Melting point (cooling curve) is a test that is widely
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.
Current edition approved Dec. 1, 2009. Published December 2009. Originally line in nature. A plateau occurs with specimens containing
approved in 1921. Last previous edition approved in 2007 as D87–07a. DOI: appreciable amounts of hydrocarbons that crystallize at the
10.1520/D0087-09.
2
same temperature, giving up heat of fusion, thus temporarily
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
retarding the cooling rate. In general, petroleum waxes with
Standards volume information, refer to the standard’s Document Summary page on large amounts of non-normal hydrocarbons or with amorphous
the ASTM website. solid forms will not exhibit a plateau.

*A Summary of Changes section appears at the end of this standard

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 D87 − 09
6. Apparatus 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)
6.1 The necessary apparatus for Procedure A is 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 ex- Applicable for the sample (see Note 1 for other methods).
ample, an aluminum block with two measuring locations, two
apertures to place the test tubes, and two apertures for the 9. Procedure B (Automatic Method)
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
thermometer or an electronic temperature measuring device of 9.3 Bring the sample to a temperature at least 8°C (15°F)
equivalent precision and accuracy. above the expected melting point. Heat the sample in a 93°C
(200°F) maximum temperature water bath.
6.3 Other types of equivalent automatic apparatus are ac-
ceptable. 9.4 Add the molten sample to the test tube to the filling
mark. Place the stopper with the probe on the test tube
7. Test Specimen assembly.
7.1 Obtain a sample of wax representative of the shipment 9.5 Insert the assembly into the aluminum block aperture,
to be tested. From each test unit obtain a portion of wax and initiate the analysis in accordance with the manufacturer’s
weighing at least 25 g for each melting point determination. instructions.
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
8.1 Support the air bath in its proper position in the water resulting melting point will be displayed on the digital monitor,
bath. Fill the water bath to within 13 mm (1 ⁄2 in.) of the top or printed on a printer, or both.
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
direct heat such as flame or hot plate. Do not keep the sample 10.2 The automatic apparatus will average the first five
in the molten state longer than 1 h. consecutive temperature probe readings within 60.1°C
(60.2°F).
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 10.3 Report the result to at least the nearest 0.05°C (0.1°F)
completely molten, or to from 90 to 93°C (195 to 200°F) before as the Petroleum Wax Melting Point (Cooling Curve), Test
proceeding to the next step. Method D87. Also report whether the test was performed
8.3 Fill the test tube to a height of 51 mm (2 in.) with the manually or using automatic apparatus, as applicable.
melted sample. Insert the melting point temperature measuring 11. Quality Control (QC)
device through the center of a one-holed stopper, such as a
cork. In the case of a thermometer, position the 79-mm 11.1 Confirm the performance of the instrument or the test
(31⁄8-in.) immersion line at the lower surface of the stopper. procedure by analyzing a quality control (QC) sample.
Insert the stopper into the test tube so that the bottom of the 11.1.1 When QC/Quality Assurance (QA) protocols are
thermometer bulb or temperature measuring probe is 10 mm already established in the testing facility, these may be used
(3⁄8 in.) from the bottom of the test tube. Support the test tube when they confirm the reliability of the test result.
assembly in the air bath, as shown in Fig. A1.1, while the 11.1.2 When there is no QC/QA protocol established in the
temperature of the molten wax is still at least 8°C (15°F) above testing facility, Appendix X1 can be used as the QC/QA
its expected melting point (Note 2). system.

8.4 Take a temperature reading every 15 s. Record each 12. Precision and Bias3
reading to at least the nearest 0.05°C (0.1°F). Monitor the 12.1 Precision—The precision of this test method as deter-
progress of these sequential readings to determine the appear- mined by statistical examination of interlaboratory results is as
ance of the plateau. Identify the plateau as the first five follows:
consecutive readings all of which agree within 0.1°C (0.2°F).
You may discontinue the test after obtaining these five plateau 3
Supporting data have been filed at ASTM International Headquarters and may
readings. be obtained by requesting Research Report RR:D02-1617.

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 D87 − 09
12.1.1 Repeatability—The difference between two test re- based on a study among 14 laboratories, using seven paraffin
sults, obtained by the same operator with the same apparatus waxes with a melting point range of 52 to 70°C (126 to 158°F).
under constant operating conditions on identical test material, 12.3 Bias—The bias of this test method cannot be deter-
would in the long run, in the normal and correct operation of mined since no generally acceptable standard reference mate-
the test method, exceed the following values only in one case rial is available for this analysis.
in twenty:
Manual apparatus 0.11°C
12.4 Relative Bias—The sample set was analyzed using
Automatic apparatus 0.23°C both manual and automatic apparatus. The difference between
12.1.2 Reproducibility—The difference between two single the two sets of measurements was not very significant. Auto-
and independent results obtained by different operators work- matic mode results were biased very slightly low (averaging
ing in different laboratories on identical test material would, in 0.064 difference).
the long run, in the normal and correct operation of the test 12.4.1 Based on the comparison of analysis of three sets of
method, exceed the following values only in one case in wax samples in the melting point range of 115 to 159°F (a total
twenty: of 70 data points by each method) by both manual and
automatic apparatus in one laboratory, a correlation coefficient
Manual apparatus 0.41°C
Automatic apparatus 0.50°C of r2 of 0.9999 was obtained indicating that there is no bias
12.2 This test method is considered suitable for waxes of a between the two modes of measurement.
melting point between 38°C (100°F) and 82°C (180°F). These
precision values have been obtained by statistical examination 13. Keywords
of interlaboratory test results from 2005. These values are 13.1 cooling curve; melting point; petroleum wax; wax

ANNEX

(Mandatory Information)

A1. APPARATUS

A1.1 Test Tube—A standard glass test tube, 25 mm (1 in.) NOTE A1.1—The air bath, water bath, and water bath cover may be
in outside diameter, and 100 mm (4 in.) in length. It may be made in one assembly as shown in Fig. A1.1.
marked with a reference line for sample filling at 51 mm (2 in.)
A1.4 Melting Point Thermometer—A wax melting point
above the bottom, and a reference line for positioning of the
thermometer having the range shown below and conforming to
bottom of the temperature measuring device at 10 mm (3⁄8 in.)
the requirements as prescribed in Specification E1 or in the
above the bottom.
specifications for IP thermometers:
A1.2 Air Bath—A cylinder 51 mm (2 in.) in inside diameter Thermometer Number
and 114 mm (41⁄2 in.) in depth, equipped to hold the test tube Temperature Range ASTM IP
38 to 82°C 14C 17C
firmly in a vertical position in the center of the air bath. As 100 to 180°F 14F 17F
examples, a tight-fitting cork having a central opening or a
metal plate top with a spring clamp that holds the test tube NOTE A1.2—Other means of monitoring the temperature (for example,
firmly in place have been found suitable to use. a resistance temperature detector, in conjunction with a data logger or
computer) may be used in place of the specified melting point thermom-
A1.3 Water Bath—A suitable cylindrical vessel, 130 mm eter, provided that the results are found to be statistically equivalent and
(51⁄8 in.) in inside diameter and 152 mm (6 in.) in depth. that the laboratory making the substitution has collected the necessary data
to demonstrate this equivalency.
Provide a fitted cover equipped to support the air bath
vertically so that the sides and bottom of the air bath are A1.5 Bath Temperature Measuring Device—Any suitable
surrounded by a layer of water 38 mm (11⁄2 in.) thick. Provide partial immersion thermometer, or other equivalent device,
the cover with an opening through which the bath temperature accurate to at least 1.0°C (2°F) throughout the required range.
measuring device may be suspended 19 mm (3⁄4 in.) from the
outside wall of the water bath. A1.6 Timer—Interval timer or stop watch.

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 D87 − 09

NOTE 1—Dimensions in inches (millimetres).

FIG. A1.1 Apparatus for Determination of Melting Point (Cooling
Curve) of Petroleum Wax

APPENDIX

(Nonmandatory Information)

X1. QUALITY CONTROL MONITORING

X1.1 Confirm the performance of the instrument or the test stability of the testing process, and customer requirements.
procedure by analyzing a quality control (QC) sample(s). Generally, a QC sample should be analyzed each testing day
with routine samples. The QC frequency should be increased if
X1.2 Prior to monitoring the measurement process, the user a large number of samples are routinely analyzed. However,
of the method needs to determine the average value and control
when it is demonstrated that the testing is under statistical
limits of the QC sample (see Practice D6299 and MNL74).
control, the QC testing frequency may be reduced. The QC
X1.3 Record the QC results and analyze by control charts sample testing precision should be periodically checked against
or other statistically equivalent techniques to ascertain the the ASTM method precision to ensure data quality (see
statistical control status of the total testing process (see Practice Practice D6299 and MNL74).
D6299 and MNL74). (In the absence of explicit requirements
given in the test method, this clause provides guidance on QC X1.5 It is recommended that, if possible, the type of QC
testing frequency.) Investigate any out of control data for root sample that is regularly tested be representative of the material
cause(s). The results of this investigation may, but not neces- routinely analyzed. An ample supply of QC sample material
sarily, result in instrument recalibration. should be available for the intended period of use, and must be
homogenous and stable under the anticipated storage condi-
X1.4 The frequency of QC testing is dependent on the tions.
criticality of the quality being measured, the demonstrated
X1.6 See Practice D6299 and MNL74 for further guidance
4
MNL7, Manual on Presentation of Data Control Chart Analysis, 6th ed., on QC and Control Charting techniques.
ASTM International, W. Conshohocken, PA.

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 D87 − 09
SUMMARY OF CHANGES

Subcommittee D02.10 has identified the location of selected changes to this standard since the last issue
(D87–07a) that may impact the use of this standard.

(1) Revised 4.1, 4.2, 5.1, 8.3, 8.4, 10.1, 10.3, A1.1, A1.3, and
A1.5.

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of infringement of such rights, are entirely their own responsibility.

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