This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D87 − 09 (Reapproved 2018) 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)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 Wax, Including Petrolatum

1.1 This test method covers the determination of the melting D938 Test Method for Congealing Point of Petroleum
point (cooling curve) of petroleum wax. It is unsuitable for Waxes, Including Petrolatum
waxes of the petrolatum group, microcrystalline waxes, or D6299 Practice for Applying Statistical Quality Assurance
blends of such waxes with paraffin wax or scale wax. and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
NOTE 1—For additional methods used for testing petroleum waxes, see E1 Specification for ASTM Liquid-in-Glass Thermometers
Test Method D127 and Test Method D938. Results may differ, depending
on the method used. For pharmaceutical petrolatum, Test Method D127
usually is used. 3. Terminology
1.2 The values stated in SI units are to be regarded as 3.1 Definitions:
standard. The values given in parentheses after SI units are 3.1.1 melting point (cooling curve) of petroleum wax—
provided for information only and are not considered standard. temperature at which melted petroleum wax first shows a
minimum rate of temperature change when allowed to cool
1.3 This standard does not purport to address all of the
under prescribed conditions.
safety concerns, if any, associated with its use. It is the
3.1.1.1 Discussion—The so-called “American Melting
responsibility of the user of this standard to establish appro-
Point” is arbitrarily 1.65 °C (3 °F) above the Melting Point
priate safety, health, and environmental practices and deter-
(Cooling Curve) of Petroleum Wax.
mine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accor- 4. Summary of Test Method
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 4.1 In Procedure A (Manual Method), a specimen of molten
Development of International Standards, Guides and Recom- wax in a test tube fitted with a thermometer or equivalent
mendations issued by the World Trade Organization Technical temperature measuring device is placed in an air bath, which in
Barriers to Trade (TBT) Committee. turn is surrounded by a water bath held at 16 °C to 28 °C (60 °F
to 80 °F). As the molten wax cools, periodic readings of its
2. Referenced Documents temperature are taken. When solidification of the wax occurs,
2.1 ASTM Standards:2 the rate of temperature change decreases, yielding a plateau in
D127 Test Method for Drop Melting Point of Petroleum 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
1
This test method is under the jurisdiction of ASTM Committee D02 on molten wax cools, the sample temperature decrease is mea-
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.10.0A on Physical/Chemical Properties. sured every 15 s in 0.01 °C (0.1 °F) readings. The melting
In the IP, this test method is under the jurisdiction of the Standardization point is considered to be reached when five consecutive
Committee. This test method was adopted as a joint ASTM-IP standard in 1966. measurements are constant within a given temperature interval,
Current edition approved Oct. 1, 2018. Published November 2018. Originally
approved in 1921. Last previous edition approved in 2014 as D87 – 09 (2014). DOI:
usually 0.1 °C (0.2 °F).
10.1520/D0087-09R18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5. Significance and Use
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 5.1 Melting point (cooling curve) is a test that is widely
the ASTM website. used by wax suppliers and consumers. it is particularly applied

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 D87 − 09 (2018)
to petroleum waxes that are rather highly paraffinic or crystal- 8.4 Take a temperature reading every 15 s. Record each
line in nature. A plateau occurs with specimens containing reading to at least the nearest 0.05 °C (0.1 °F). Monitor the
appreciable amounts of hydrocarbons that crystallize at the progress of these sequential readings to determine the appear-
same temperature, giving up heat of fusion, thus temporarily ance of the plateau. Identify the plateau as the first five
retarding the cooling rate. In general, petroleum waxes with consecutive readings all of which agree within 0.1 °C (0.2 °F).
large amounts of non-normal hydrocarbons or with amorphous You may discontinue the test after obtaining these five plateau
solid forms will not exhibit a plateau. readings.
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
Annex A1. 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
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,
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 °C and 26 °C (72 °F and 79 °F). A heating device is used to 9.2 Insert the temperature probe into a centrally bored,
increase the temperature, and a cooling device with cold water one-holed stopper, and insert it in the test tube. Check the
circulation is used to decrease the temperature. probe height to reach manufacturer’s suggested height. Place
6.2.2 The temperature may be monitored with a calibrated the stopper with the probe back in the resting holder provided.
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
6.3 Other types of equivalent automatic apparatus are ac- (200 °F) maximum temperature water bath.
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.
8. Procedure A (Manual Method) 9.6 When the melting point is detected, the analysis will
8.1 Support the air bath in its proper position in the water automatically stop. Per available options on the instrument, the
bath. Fill the water bath to within 13 mm (1⁄2 in.) of the top resulting melting point will be displayed on the digital monitor,
with water at a temperature of 16 °C to 28 °C (60 °F to 80 °F). or printed on a printer, or both.
The bath temperature is kept within these limits throughout the
10. Calculation and Report
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 °C to 93 °C (195 °F 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
device through the center of a one-holed stopper, such as a 11. Quality Control (QC)
cork. In the case of a thermometer, position the 79 mm (31⁄8 in.) 11.1 Confirm the performance of the instrument or the test
immersion line at the lower surface of the stopper. Insert the procedure by analyzing a quality control (QC) sample.
stopper into the test tube so that the bottom of the thermometer 11.1.1 When QC/Quality Assurance (QA) protocols are
bulb or temperature measuring probe is 10 mm (3⁄8 in.) from already established in the testing facility, these may be used
the bottom of the test tube. Support the test tube assembly in when they confirm the reliability of the test result.
the air bath, as shown in Fig. A1.1, while the temperature of the 11.1.2 When there is no QC/QA protocol established in the
molten wax is still at least 8 °C (15 °F) above its expected testing facility, Appendix X1 can be used as the QC/QA
melting point (Note 2). --``,,``,```,`,,`,,`,`,`,,``,``-`-`,,`,,`,`,,`---
system.

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 D87 − 09 (2018)
12. Precision and Bias3 12.2 This test method is considered suitable for waxes of a
12.1 Precision—The precision of this test method as deter- melting point between 38 °C (100 °F) and 82 °C (180 °F).
mined by statistical examination of interlaboratory results is as These precision values have been obtained by statistical
follows: examination of interlaboratory test results from 2005. These
12.1.1 Repeatability—The difference between two test values are based on a study among 14 laboratories, using seven
results, obtained by the same operator with the same apparatus paraffin waxes with a melting point range of 52 °C to 70 °C
under constant operating conditions on identical test material, (126 °F to 158 °F).
would in the long run, in the normal and correct operation of 12.3 Bias—The bias of this test method cannot be deter-
the test method, exceed the following values only in one case mined since no generally acceptable standard reference mate-
in twenty: rial is available for this analysis.
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 °F to 159 °F (a
twenty: total of 70 data points by each method) by both manual and
Manual apparatus 0.41 °C automatic apparatus in one laboratory, a correlation coefficient
Automatic apparatus 0.50 °C
of r2 of 0.9999 was obtained indicating that there is no bias
between the two modes of measurement.
3
Supporting data have been filed at ASTM International Headquarters and may 13. Keywords
be obtained by requesting Research Report RR:D02-1617. Contact ASTM Customer
Service at [email protected]. 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.)

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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 °C to 82 °C 14C 17C
firmly in a vertical position in the center of the air bath. As 100 °F 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
A1.3 Water Bath—A suitable cylindrical vessel, 130 mm thermometer, provided that the results are found to be statistically
(51⁄8 in.) in inside diameter and 152 mm (6 in.) in depth. equivalent and 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 (2018)

NOTE 1—Dimensions in inches (millimetres).

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

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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 routinely analyzed. An ample supply of QC sample material
necessarily, 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 (2018)
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