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Drop Melting Point of Petroleum Wax, Including Petrolatum: Standard Test Method For

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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: D127 − 19

Designation: 133/79 (87)

Standard Test Method for


Drop Melting Point of Petroleum Wax, Including Petrolatum1
This standard is issued under the fixed designation D127; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* method has shown to produce results that are close to those
1.1 This test method covers the determination of the drop determined by the original Test Method D127, Method A.
melting point of petroleum wax. It is used primarily for 1.2 The values stated in SI units are to be regarded as the
petrolatums and other microcrystalline wax. standard. The values given in parentheses are for information
only.
NOTE 1—Additional methods used for petroleum waxes are Test
Method D87 and Test Method D938. Results obtained may differ, 1.3 This standard does not purport to address all of the
depending on the method used. For pharmaceutical petrolatum, Test safety concerns, if any, associated with its use. It is the
Method D127 usually is used. responsibility of the user of this standard to establish appro-
1.1.1 Test Method A—The dropping point of wax is deter- priate safety, health, and environmental practices and deter-
mined with a mercury in glass thermometer, as stated below mine the applicability of regulatory limitations prior to use.
in6.3. (Warning—Mercury has been designated by many 1.4 This international standard was developed in accor-
regulatory agencies as a hazardous substance that can cause dance with internationally recognized principles on standard-
serious medical issues. Mercury, or its vapor, has been dem- ization established in the Decision on Principles for the
onstrated to be hazardous to health and corrosive to materials. Development of International Standards, Guides and Recom-
Use Caution when handling mercury and mercury-containing mendations issued by the World Trade Organization Technical
products. See the applicable product Safety Data Sheet (SDS) Barriers to Trade (TBT) Committee.
for additional information. The potential exists that selling
mercury or mercury-containing products, or both, is prohibited 2. Referenced Documents
by local or national law. Users must determine legality of sales 2.1 ASTM Standards:2
in their location.) D87 Test Method for Melting Point of Petroleum Wax
1.1.2 Test Method B—The dropping point of wax deter- (Cooling Curve)
mined in a dropping point cup in an instrument which detects D938 Test Method for Congealing Point of Petroleum
the drop and measures the temperature electronically, with a Waxes, Including Petrolatum
platinum thermometer instead of with mercury. Mercury has D3104 Test Method for Softening Point of Pitches (Mettler
been recognized as a poison and a health hazard. Removing Softening Point Method)
mercury from laboratories is a way of making the measuring D3954 Test Method for Dropping Point of Waxes
process more inherently safe. The instrumental dropping point E1 Specification for ASTM Liquid-in-Glass Thermometers
E177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
1
This test method is under the jurisdiction of ASTM Committee D02 on
E691 Practice for Conducting an Interlaboratory Study to
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Determine the Precision of a Test Method
Subcommittee D02.10.0A on Physical/Chemical Properties.
Current edition approved Nov. 1, 2019. Published February 2020. Originally TEST METHOD A
approved in 1922. Last previous edition approved in 2015 as D127 – 08 (2015).
DOI: 10.1520/D0127-19. 3. Terminology
This test method was adopted as a joint ASTM-IP standard in 1964. In the IP, this
test method is under the jurisdiction of Standardization Committee. 3.1 Definitions:
In 1963, the title, scope, and definition were changed to define the determination
of “drop melting point.” Sections on procedure, report, and precision were revised,
2
and a new section on significance was added. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
In 1964, minor editorial changes and additions to this method were made for its contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
publication as a joint ASTM-IP standard. Standards volume information, refer to the standard’s Document Summary page on
Only Method A of this test method is equivalent to IP 133/79 (87). the ASTM website.

*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
D127 − 19
3.1.1 drop melting point of petroleum wax—the temperature having a temperature of 16 °C 6 1 °C (60 °F 6 2 °F). Prepare
at which material becomes sufficiently fluid to drop from the another specimen from the same sample using this procedure.
thermometer used in making the determination under definite NOTE 2—A dipping temperature of 11 °C (20 °F) above the congealing
prescribed conditions. point in accordance with Test Method D938 usually will be 6 °C to 11 °C
(10 °F to 20 °F) above the actual drop melting point.
4. Summary of Test Method 7.2 Securely fix the thermometers in the test tubes by means
4.1 Specimens are deposited on two thermometer bulbs by of suitable stoppers, such as corks, so that the tip of each
dipping chilled thermometers into the sample. The thermom- thermometer is approximately 15 mm above the bottom of its
eters bearing the specimens are placed in test tubes and heated test tube. Insert the test tubes in the water bath which is at
by means of a water bath until the specimens melt and the first 16 °C 6 1 °C (60 °F 6 2 °F) and adjust the height of the test
drop falls from each thermometer bulb. The average of the tubes so that the immersion marks on the thermometers are
temperatures at which these drops fall is the drop melting point level with the top surface of the water. Raise the temperature of
of the sample. the bath at a rate of approximately 2 °C (3 °F) ⁄min to 38 °C
(100 °F), then at a rate of approximately 1 °C (2 °F) ⁄min until
5. Significance and Use the first drop of material leaves each thermometer. Record in
5.1 Melting point is a wax property that is of interest to most each case the temperature at which the first drop falls from the
wax consumers. It can be an indication of the performance thermometer.
properties of the wax. Drop melting point, Test Method D127, 8. Report
is often used to measure the melting characteristics of petro-
latums and other high viscosity petroleum waxes. 8.1 Report the average of the two determinations as the drop
melting point of the sample under test.
6. Apparatus
9. Precision and Bias
6.1 Test Tubes—Standard test tubes, 25 mm (1 in.) in out-
9.1 Precision—The precision of this test method as deter-
side diameter and 150 mm (6 in.) long. The test tubes shall
mined by statistical examination of interlaboratory results is as
utilize stoppers, such as corks, grooved at the sides to permit
follows:
air circulation and bored in the center to receive the thermom-
9.1.1 Repeatability—The difference between two test
eter.
results, obtained by the same operator with the same apparatus
6.2 Bath—A transparent container of not less than 1500 mL under constant operating conditions on identical test material,
capacity, that will permit the immersion of the test tubes to a would in the long run, in the normal and correct operation of
depth of at least 90 mm and still leave a depth of approximately the test method, exceed the following values only in one case
15 mm of water below the bottoms of the test tubes. in twenty:
6.3 Thermometer, having a range as shown below and 0.8 °C (1.4 °F)
conforming to the requirements as prescribed in Specification 9.1.2 Reproducibility—The difference between two single
E1 or in specifications for IP Standard Thermometers: and independent results obtained by different operators work-
Thermometer Number ing in different laboratories on identical test material would, in
Thermometer Range ASTM IP the long run, in the normal and correct operation of the test
32 °C to 127 °C 61C 63C
90 °F to 260 °F 61F ... method, exceed the following values only in one case in
twenty:
6.4 Bath Thermometer, any suitable type, accurate to 0.5 °C
1.3 °C (2.4 °F)
(1 °F) throughout the required range.
NOTE 3—The following information on the precision of this test method
7. Procedure was developed by the Institute of Petroleum (now Energy Institute) in
London and is being investigated:
7.1 Secure a sample of sufficient size that is representative (1) Results of duplicate tests should not differ by more than the
of the material under inspection. Use a fresh portion of the following amounts:
sample for each set of two determinations. Melt the sample Repeatability Reproducibility
slowly until the temperature reaches at least 11 °C (20 °F) 1 °C (2 °F) 1.2 °C (2.2 °F)

above the expected drop melting point. Place sufficient sample (2) These precision values were obtained in 1954 by statistical
in a flat bottom container to give a sample depth of 12 mm 6 examination of interlaboratory test results.
1 mm. Adjust the temperature of the sample to at least 6 °C 9.2 Bias—The procedure in this test method has no bias
(10 °F) (Note 2) above its drop melting point using any general because the value of drop melting point can be defined only in
laboratory thermometer for measurement. Chill one of the test terms of a test method.
thermometer bulbs to approximately 4 °C (40 °F). Wipe dry,
and, quickly but carefully, immerse the chilled bulb vertically TEST METHOD B
into the heated sample until it touches the bottom of the
container (about 12 mm submerged) and withdraw it immedi- 10. Summary of Test Method
ately. Hold the thermometer vertically away from the heat until 10.1 In this test method, the dropping point is defined as the
the surface dulls, and then place it for at least 5 min in water temperature at which the wax suspended in a cylindrical cup,

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D127 − 19
with a 2.8 mm diameter hole in the bottom, flows downward 12. Apparatus
and releases a drop as the sample is heated at a constant rate in 12.1 A METTLER TOLEDO3 dropping point furnace shall
air. The cups may be nickel plated brass or aluminum. A glass be used to determine pitch softening points by this test method.
receptacle contains the molten wax underneath the drop. These commercially available instruments consist of a control
unit with a digital temperature indicator, with furnace built in
11. Significance and Use
11.1 This closely defined method may be used as an 3
The sole source of supply of the apparatus known to the committee at this time
alternate to Test Method D127 part A to measure the melting is METTLER TOLEDO LLC, 1900 Polaris Parkway, Columbus, OH 43240,
characteristics of natural waxes, paraffin waxes, microcrys- 1-800-METTLER, www.mt.com. If you are aware of alternative suppliers, please
provide this information to ASTM International Headquarters. Your comments will
talling waxes and petrolatums and other high viscosity petro- receive careful consideration at a meeting of the responsible technical committee,1
leum waxes. which you may attend.

FIG. 1 Overview of DP70 Dropping Point Instrument

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D127 − 19
or attached, sample cartridges, and accessories. The control with as much wax as possible over the level of the cup in order
unit automatically regulates the heating rate of the furnace. The to minimize the cavity that forms in the center, after the excess
dropping point is indicated on the readout, and the heating wax is cut off.
program stopped, when the sample flow triggers a dropping 13.4.2 Fig. 3—The four cups from Fig. 2 have been poured
point detection. A general view of the contents of the MET- and cooled. The two cups sitting on top did not get enough
TLER TOLEDO dropping point instrument is shown in Fig. 1. wax. Cavities extend way down in the center of those. The one
on the left had a dropping point of 0.5° lower than the one on
13. Procedure the right. More wax should be poured to begin with, as is
13.1 Secure a sample of sufficient size that is representative evident in the samples in the holder. These will all need
of the material under inspection. Use a fresh portion of the trimming, but they will have a small cavity in the center that
sample for each set of two determinations. Melt the sample does not materially influence the dropping point.
slowly until the temperature reaches at least 11 °C (20 °F) 13.4.3 Fig. 4—A cup with wax after the drop. Note the
above the expected drop melting point. The sample should be hanging solidified drop and the pool of wax in the bottom of
completely melted. The wax should be hot enough that the the receiver glass.
wax, when poured, remains transparent enough to see the 13.4.4 Fig. 5—Two cups in the holder shortly after removal
opening in the bottom of the cup when the cup is poured full. from the DP70, showing the drops and wax in the bottom of the
This ensures that no air pockets are trapped in a solidifying receiver glass.
wax that is not hot enough. (See Note 4.) The cup should be 13.4.5 Fig. 6—The photo from the report with at the
poured full to the top plus 1 mm to 2 mm above the rim. As the moment of the drop on the right side at 62.2 °C. The sample on
wax cools in the cup, it cools from the outside in and there is the left had already dropped at 61.8 °C. The second drop is
shrinkage in the center. After cooling, any wax remaining about to fall.
above the top of the cup should be trimmed off with a flat sharp
edge. Any wax on the outside of the cup should be cleaned off. 14. Report
The cup should temper at room temperature (20 °C to 25 °C) 14.1 Report both determinations and the average of the two
for 2 h to allow the wax time to harden. If the wax is too hot determinations as the drop melting point of the sample under
when poured, there will be more shrinkage as it cools, and this test.
will cause a cavity down in the center. Pouring more wax in 14.1.1 The PDF report generated on a USB stick or trans-
after it hardens is not recommended because an air pocket can ferred to an Ethernet connected PC may be examined for
be trapped in the cavity. A small cavity is almost unavoidable photos of the drop to verify that the drop occurred correctly.
for some waxes but this should not cause a problem so long as See Fig. 6.
the cup is otherwise full.
NOTE 4—Center cavities are caused by the outside of the cup cooling 15. Precision and Bias
and hardening before the center. This can be minimized by heating the
sample preparation tool to near the expected drop temperature before
15.1 The precision of this test method is based on an
pouring into the dropping point cups. The cooling becomes more uniform interlaboratory study of ASTM D127 – 08 (2014), Standard
and the cavity less pronounced. Test Method for Drop Melting Point of Petroleum Wax,
13.2 Petrolatums should be dropped into ice water after they Including Petrolatum, conducted in 2014. Eleven laboratories
have cooled and gelled so that they retain the shape. The cup tested a total of nineteen different wax samples. Every “test
should sit in the ice water for at least one hour. result” represents an individual determination. All labs were
asked to report duplicate test results for every material tested.
13.3 The exterior of the cup is cleaned of any wax and Practice E691 was followed for the design and analysis of the
water, the cap is put on and the glass receptacle fitted to the data; the details are given in ASTM Research Report No.
bottom and held. It is then inserted in the sample holder. RR:D02-1921.4
Usually samples are analyzed in duplicate, as the sample 15.1.1 Repeatability Limit (r)—Two test results obtained
holder holds two cups. The start temperature should be at least within one laboratory shall be judged not equivalent if they
15° below the expected drop temperature, with a 120 s wait differ by more than the “r” value for that material; “r” is the
time before the temperature ramp of 1 °C ⁄minute is started. interval representing the critical difference between two test
When both cups have dropped, the temperature should return results for the same material, obtained by the same operator
to the insert temperature and the results presented on the using the same equipment on the same day in the same
display. The video of the drop can be examined if there is any laboratory.
doubt about the drop result, and the report can be viewed to see 15.1.1.1 Repeatability limits are listed in Table 3.
a photo of the drop at the moment it fell. 15.1.2 Reproducibility Limit (R)—Two test results shall be
13.4 Illustrations: judged not equivalent if they differ by more than the “R” value
13.4.1 Fig. 2—The dropping point cups have been recently for that material; “R” is the interval representing the critical
poured. The lower and right cups have been cooling for several
minutes. The top cup was just poured. The bottom can be seen
through the transparent molten wax, ensuring that there are no 4
Supporting data have been filed at ASTM International Headquarters and may
entrapped air pockets. The left cup has not been poured. In the be obtained by requesting Research Report RR:D02-1921. Contact ASTM Customer
right cup, the center is still molten. These cups were poured Service at service@astm.org.

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D127 − 19

FIG. 2 Four Recently Poured Dropping Point Cups

difference between two test results for the same material, laboratories, on nineteen materials. These nineteen materials
obtained by different operators using different equipment in were identified generically in the tables above. ÷DSC analysis
different laboratories. showed in general that waxes with a narrow melting range had
15.1.2.1 Reproducibility limits are listed in Tables 1-3. a consistent dropping point with small variation. Waxes with a
15.1.3 The above terms (repeatability limit and reproduc- broad melting range, such as the plant wax blends, showed
ibility limit) are used as specified in Practice E177. much greater variability in the dropping point by both methods
15.1.4 Any judgment in accordance with statements 15.1.1 A and B.
and 15.1.2 would have an approximate 95 % probability of
being correct. 15.4 To judge the equivalency of two test results, it is
recommended to choose the material closest in characteristics
15.2 Bias—At the time of the study, there was no accepted
to the test material.
reference material suitable for determining the bias for this test
method, therefore no statement on bias is being made.
16. Keywords
15.3 The precision statement was determined through sta-
tistical examination of all reported results, from eleven 16.1 drop melting point; petrolatum; petroleum wax; wax

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D127 − 19

FIG. 3 Four Dropping Point Cups after Pouring and Cooling

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D127 − 19

FIG. 4 Wax Cup After the Drop

FIG. 5 Two Cups in the Holder After Removal from the DP70

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D127 − 19

FIG. 6 Report Photo at the Moment of the Drop

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D127 − 19
TABLE 1 Dropping Point (°C) – Averages, Part A
Reproducibility Standard
Reproducibility
Sample Average Deviation Number of Labs Reporting
SR R
1 Petrolatum 54.32 3.16 8.86 8
2 Natural plant wax 71.95 1.13 3.17 8
3 Paraffin wax 64.80 0.41 1.15 8
4 Microcrystalline wax 89.32 0.75 2.10 8
5 Natural plant wax 96.02 2.14 6.00 8
6 Paraffin wax 69.57 0.58 1.64 8
7 Praffin wax 68.85 0.48 1.35 8
8 Natural wax, beeswax 59.98 0.66 1.85 8
9 Paraffin wax 53.34 0.78 2.18 8
10 Scale wax 53.66 5.93 16.60 8
11 Natural plant wax blend 71.83 8.24 23.07 9
12 Natural plant wax blend 82.23 7.16 20.06 8
13 Polyethylene wax 111.95 2.21 6.19 3
14 Microcrystalline wax 84.70 0.76 2.13 8
15 Paraffin wax 55.95 0.43 1.20 8
16 Petrolatum 61.26 1.34 3.74 8
17 Petrolatum 59.76 2.35 6.58 8
18 Microcrystalline wax 76.82 7.28 20.39 8
19 Microcrystalline wax 81.54 4.23 11.84 8

TABLE 2 Dropping Point (°C) – Averages, Part B


Reproducibility Standard
Reproducibility
Sample Average Deviation Number of Labs Reporting
SR R
1 Petrolatum 49.72 1.91 5.35 11
2 Natural plant wax 73.54 0.90 2.52 10
3 Paraffin wax 65.15 0.87 2.43 11
4 Microcrystalline wax 90.35 0.56 1.56 11
5 Natural plant wax 97.26 1.14 3.20 10
6 Paraffin wax 70.85 1.03 2.88 11
7 Paraffin wax 69.98 0.81 2.27 11
8 Natural wax, beeswax 60.18 0.75 2.09 11
9 Paraffin wax 53.56 0.75 2.11 11
10 Scale wax 51.81 2.00 5.61 11
11 Blend plant wax 71.56 4.07 11.38 11
12 Blend plant wax 75.99 5.86 16.41 10
13 Polyethylene wax 113.59 0.48 1.35 9
14 Microcrystalline wax 84.62 0.72 2.02 11
15 Paraffin wax 56.13 1.01 2.82 11
16 Petrolatum 58.82 2.22 6.23 11
17 Petrolatum 57.17 1.05 2.93 11
18 Microcrystalline wax 80.56 1.04 2.91 11
19 Microcrystalline wax 80.57 4.08 11.42 11

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D127 − 19
TABLE 3 Dropping Point (°C) – Individual Determinations, Part B
Repeatability Reproducibility
Repeatability Reproducibility Number of Labs
Sample Average Standard Deviation Standard Deviation
Reporting
Sr SR r R
1 Petrolatum 49.7 0.3 1.9 0.8 5.4 11
2 Natural plant wax 73.5 0.3 0.9 0.9 2.6 10
3 Paraffin wax 65.1 0.4 0.9 1.2 2.6 11
4 Microcrystalline wax 90.3 0.6 0.7 1.8 2.0 11
5 Natural plant wax 97.3 1.2 1.4 3.5 4.0 10
6 Paraffin wax 70.9 0.6 1.1 1.6 3.1 1
7 Paraffin wax 70.0 0.2 0.8 0.6 2.3 11
8 Natural wax, beeswax 60.2 0.2 0.8 0.6 2.1 1
9 Paraffin wax 53.6 0.5 0.8 1.5 2.4 11
10 Scale wax 51.8 0.5 2.0 1.4 5.7 11
11 Blend plant wax 71.6 2.2 4.4 6.2 12.2 11
12 Blend plant wax 76.0 1.1 5.9 3.1 16.6 10
13 Polyethylene wax 113.6 0.3 0.5 0.7 1.4 9
14 Microcrystalline wax 84.6 0.4 0.8 1.2 2.2 1
15 Paraffin wax 56.1 0.3 1.0 0.8 2.9 1
16 Petrolatum 58.8 0.2 2.2 0.7 6.2 11
17 Petrolatum 57.2 0.3 1.1 1.0 3.0 11
18 Microcrystalline wax 80.6 0.2 1.0 0.6 2.9 11
19 Microcrystalline wax 80.6 0.6 4.1 1.8 11.5 11

SUMMARY OF CHANGES

Committee D02.10 has identified the location of selected changes to this standard since the last issue
(D127 – 08 (2015)) that may impact the use of this standard. (Approved Nov. 1, 2019.)

(1) Added subsections 1.1.1 and 1.1.2. (3) Added Test Method B in Sections 10 – 15
(2) Added D3104, D3954, E177, and E691 to 2.1.

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