Location via proxy:   [ UP ]  
[Report a bug]   [Manage cookies]                

Astm D127 19

Download as pdf or txt
Download as pdf or txt
You are on page 1of 6

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: D127 − 08 (Reapproved 2015) D127 − 19 Technical Association of Pulp and Paper Industry
Tentative Method T 634ts-64

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 Scope*
1.1 This test method covers the determination of the drop melting point of petroleum wax. It is used primarily for petrolatums
and other microcrystalline wax.
NOTE 1—Additional methods used for petroleum waxes are Test Method D87 and Test Method D938. Results obtained may differ, depending on the
method used. For pharmaceutical petrolatum, Test Method D127 usually is used.
1.1.1 Test Method A—The dropping point of wax is determined with a mercury in glass thermometer, as stated below in6.3.
(Warning—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical
issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when
handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional
information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national
iTeh Standards
law. Users must determine legality of sales in their location.)
1.1.2 Test Method B—The dropping point of wax determined in a dropping point cup in an instrument which detects the drop
(https://standards.iteh.ai)
and measures the temperature electronically, with a platinum thermometer instead of with mercury. Mercury has been recognized
as a poison and a health hazard. Removing mercury from laboratories is a way of making the measuring process more inherently

Document Preview
safe. The instrumental dropping point method has shown to produce results that are close to those determined by the original Test
Method D127, Method A.
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 ofASTM
the safety concerns, if any, associated with its use. It is the responsibility
D127-19
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
https://standards.iteh.ai/catalog/standards/sist/ffcb8b4f-8108-4174-98cd-ffa3ca6ab30d/astm-d127-19
applicability of regulatory limitations prior to use.
1.4 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.
2. Referenced Documents
2.1 ASTM Standards:2
D87 Test Method for Melting Point of Petroleum Wax (Cooling Curve)
D938 Test Method for Congealing Point of Petroleum Waxes, Including Petrolatum
D3104 Test Method for Softening Point of Pitches (Mettler Softening Point Method)

1
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.10.0A on Physical/Chemical Properties.
Current edition approved Jan. 1, 2015Nov. 1, 2019. Published February 2015February 2020. Originally approved in 1922. Last previous edition approved in 20082015
as D127 – 08.D127 – 08 (2015). DOI: 10.1520/D0127-19.
This test method is sponsored jointly by the Technical Association of Pulp and Paper Industry and ASTM International.
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.
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, and
a new section on significance was added.
In 1964, minor editorial changes and additions to this method were made for its publication as a joint ASTM-IP standard. DOI: 10.1520/D0127-08R15.
Only Method A of this test method is equivalent to IP 133/79 (87).
2
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.

*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

1
D127 − 19
D3954 Test Method for Dropping Point of Waxes
E1 Specification for ASTM Liquid-in-Glass Thermometers
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
TEST METHOD A

3. Terminology
3.1 Definitions:
3.1.1 drop melting point of petroleum wax—the temperature at which material becomes sufficiently fluid to drop from the
thermometer used in making the determination under definite prescribed conditions.

4. Summary of Test Method


4.1 Specimens are deposited on two thermometer bulbs by dipping chilled thermometers into the sample. The thermometers
bearing the specimens are placed in test tubes and heated by means of a water bath until the specimens melt and the first drop falls
from each thermometer bulb. The average of the temperatures at which these drops fall is the drop melting point of the sample.

5. Significance and Use


5.1 Melting point is a wax property that is of interest to most wax consumers. It can be an indication of the performance
properties of the wax. Drop melting point, Test Method D127, is often used to measure the melting characteristics of petrolatums
and other high viscosity petroleum waxes.

6. Apparatus

iTeh Standards
6.1 Test Tubes—Standard test tubes, 25-mm (1-in.)25 mm (1 in.) in outside diameter and 150-mm (6-in.)150 mm (6 in.) long.
The test tubes shall utilize stoppers, such as corks, grooved at the sides to permit air circulation and bored in the center to receive
the thermometer.
(https://standards.iteh.ai)
6.2 Bath—A transparent container of not less than 1500-mL1500 mL capacity, that will permit the immersion of the test tubes
to a depth of at least 90 mm 90 mm and still leave a depth of approximately 15 mm 15 mm of water below the bottoms of the
test tubes.
Document Preview
6.3 Thermometer, having a range as shown below and conforming to the requirements as prescribed in Specification E1 or in
specifications for IP Standard Thermometers:
ASTM D127-19 Thermometer Number

https://standards.iteh.ai/catalog/standards/sist/ffcb8b4f-8108-4174-98cd-ffa3ca6ab30d/astm-d127-19
Thermometer Range
32 to 127°C
ASTM
61C
IP
63C
32 °C to 127 °C 61C 63C
90 to 260°F 61F ...
90 °F to 260 °F 61F ...
6.4 Bath Thermometer, any suitable type, accurate to 0.5°C (1°F)0.5 °C (1 °F) throughout the required range.

7. Procedure
7.1 Secure a sample of sufficient size that is representative of the material under inspection. Use a fresh portion of the sample
for each set of two determinations. Melt the sample slowly until the temperature reaches at least 11°C (20°F)11 °C (20 °F) above
the expected drop melting point. Place sufficient sample in a flat bottom container to give a sample depth of 1212 mm 6 1 mm.
1 mm. Adjust the temperature of the sample to at least 6°C (10°F)6 °C (10 °F) (Note 2) above its drop melting point using any
general laboratory thermometer for measurement. Chill one of the test thermometer bulbs to approximately 4°C (40°F).4 °C
(40 °F). Wipe dry, and, quickly but carefully, immerse the chilled bulb vertically into the heated sample until it touches the bottom
of the container (about 12 mm submerged) and withdraw it immediately. Hold the thermometer vertically away from the heat until
the surface dulls, and then place it for at least 5 min 5 min in water having a temperature of 1616 °C 6 1°C (601 °C (60 °F 6
2°F).2 °F). Prepare another specimen from the same sample using this procedure.
NOTE 2—A dipping temperature of 11°C (20°F)11 °C (20 °F) above the congealing point in accordance with Test Method D938 usually will be 66 °C
to 11°C (1011 °C (10 °F to 20°F)20 °F) above the actual drop melting point.
7.2 Securely fix the thermometers in the test tubes by means of suitable stoppers, such as corks, so that the tip of each
thermometer is approximately 15 mm 15 mm above the bottom of its test tube. Insert the test tubes in the water bath which is at
1616 °C 6 1°C (601 °C (60 °F 6 2°F)2 °F) and adjust the height of the test tubes so that the immersion marks on the thermometers
are level with the top surface of the water. Raise the temperature of the bath at a rate of approximately 2°C (3°F)/min2 °C
(3 °F) ⁄min to 38°C (100°F),38 °C (100 °F), then at a rate of approximately 1°C (2°F)/min1 °C (2 °F) ⁄min until the first drop of
material leaves each thermometer. Record in each case the temperature at which the first drop falls from the thermometer.

2
D127 − 19
8. Report
8.1 Report the average of the two determinations as the drop melting point of the sample under test.
9. Precision and Bias
9.1 Precision—The precision of this test method as determined by statistical examination of interlaboratory results is as follows:
9.1.1 Repeatability—The difference between two test results, obtained by the same operator with the same apparatus under
constant operating conditions on identical test material, would in the long run, in the normal and correct operation of the test
method, exceed the following values only in one case in twenty:
0.8°C (1.4°F)

0.8 °C (1.4 °F)


9.1.2 Reproducibility—The difference between two single and independent results obtained by different operators working in
different laboratories on identical test material would, in the long run, in the normal and correct operation of the test method,
exceed the following values only in one case in twenty:
1.3°C (2.4°F)

1.3 °C (2.4 °F)

NOTE 3—The following information on the precision of this test method was developed by the Institute of Petroleum (now Energy Institute) in London
and is being investigated:
(1) Results of duplicate tests should not differ by more than the following amounts:
Repeatability Reproducibility
1°C (2°F) 1.2°C (2.2°F)
1 °C (2 °F) 1.2 °C (2.2 °F)

(2) These precision values were obtained in 1954 by statistical examination of interlaboratory test results.
9.2 Bias—The procedure in this test method has no bias because the value of drop melting point can be defined only in terms
of a test method. iTeh Standards
10. Summary of Test Method
(https://standards.iteh.ai)
TEST METHOD B

10.1 In this test method, the dropping Document Preview


point is defined as the temperature at which the wax suspended in a cylindrical cup, with
a 2.8 mm diameter hole in the bottom, flows downward and releases a drop as the sample is heated at a constant rate in air. The
cups may be nickel plated brass or aluminum. A glass receptacle contains the molten wax underneath the drop.
11. Significance and Use
ASTM D127-19
https://standards.iteh.ai/catalog/standards/sist/ffcb8b4f-8108-4174-98cd-ffa3ca6ab30d/astm-d127-19
11.1 This closely defined method may be used as an alternate to Test Method D127 part A to measure the melting characteristics
of natural waxes, paraffin waxes, microcrystalling waxes and petrolatums and other high viscosity petroleum waxes.
12. Apparatus
12.1 A METTLER TOLEDO3 dropping point furnace shall be used to determine pitch softening points by this test method.
These commercially available instruments consist of a control unit with a digital temperature indicator, with furnace built in or
attached, sample cartridges, and accessories. The control unit automatically regulates the heating rate of the furnace. The dropping
point is indicated on the readout, and the heating program stopped, when the sample flow triggers a dropping point detection. A
general view of the contents of the METTLER TOLEDO dropping point instrument is shown in Fig. 1.
13. Procedure
13.1 Secure a sample of sufficient size that is representative of the material under inspection. Use a fresh portion of the sample
for each set of two determinations. Melt the sample slowly until the temperature reaches at least 11 °C (20 °F) above the expected
drop melting point. The sample should be completely melted. The wax should be hot enough that the wax, when poured, remains
transparent enough to see the opening in the bottom of the cup when the cup is poured full. This ensures that no air pockets are
trapped in a solidifying wax that is not hot enough. (See Note 4.) The cup should be poured full to the top plus 1 mm to 2 mm
above the rim. As the wax cools in the cup, it cools from the outside in and there is shrinkage in the center. After cooling, any
wax remaining 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. The cup should temper at room temperature (20 °C to 25 °C) for 2 h to allow the wax time to harden. If the wax
is too hot when poured, there will be more shrinkage as it cools, and this will cause a cavity down in the center. Pouring more

3
The sole source of supply of the apparatus known to the committee at this time is METTLER TOLEDO LLC, 1900 Polaris Parkway, Columbus, OH 43240,
1-800-METTLER, www.mt.com. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive
careful consideration at a meeting of the responsible technical committee,1 which you may attend.

3
D127 − 19

iTeh Standards
(https://standards.iteh.ai)
Document Preview
ASTM D127-19
https://standards.iteh.ai/catalog/standards/sist/ffcb8b4f-8108-4174-98cd-ffa3ca6ab30d/astm-d127-19

FIG. 1 Overview of DP70 Dropping Point Instrument

wax in after it hardens is not recommended because an air pocket can be trapped in the cavity. A small cavity is almost unavoidable
for some waxes but this should not cause a problem so long as the cup is otherwise full.
NOTE 4—Center cavities are caused by the outside of the cup cooling and hardening before the center. This can be minimized by heating the sample
preparation tool to near the expected drop temperature before pouring into the dropping point cups. The cooling becomes more uniform and the cavity
less pronounced.
13.2 Petrolatums should be dropped into ice water after they have cooled and gelled so that they retain the shape. The cup should
sit in the ice water for at least one hour.
13.3 The exterior of the cup is cleaned of any wax and water, the cap is put on and the glass receptacle fitted to the bottom and
held. It is then inserted in the sample holder. Usually samples are analyzed in duplicate, as the sample holder holds two cups. The
start temperature should be at least 15° below the expected drop temperature, with a 120 s wait time before the temperature ramp
of 1 °C ⁄minute is started. When both cups have dropped, the temperature should return to the insert temperature and the results
presented on the display. The video of the drop can be examined if there is any doubt about the drop result, and the report can be
viewed to see a photo of the drop at the moment it fell.
13.4 Illustrations:
13.4.1 Fig. 2—The dropping point cups have been recently 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
entrapped air pockets. The left cup has not been poured. In the right cup, the center is still molten. These cups were poured with
as much wax as possible over the level of the cup in order to minimize the cavity that forms in the center, after the excess wax
is cut off.

4
D127 − 19

iTeh Standards
(https://standards.iteh.ai)
Document Preview
FIG. 2 Four Recently Poured Dropping Point Cups

13.4.2 Fig. 3—The four cups from Fig. 2 have beenASTM poured D127-19
and cooled. The two cups sitting on top did not get enough wax.
Cavitieshttps://standards.iteh.ai/catalog/standards/sist/ffcb8b4f-8108-4174-98cd-ffa3ca6ab30d/astm-d127-19
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 the right.
More wax should be poured to begin with, as is evident in the samples in the holder. These will all need trimming, but they will
have a small cavity in the center that does not materially influence the dropping point.
13.4.3 Fig. 4—A cup with wax after the drop. Note the hanging solidified drop and the pool of wax in the bottom of the receiver
glass.
13.4.4 Fig. 5—Two cups in the holder shortly after removal from the DP70, showing the drops and wax in the bottom of the
receiver glass.
13.4.5 Fig. 6—The photo from the report with at the moment of the drop on the right side at 62.2 °C. The sample on the left
had already dropped at 61.8 °C. The second drop is about to fall.

14. Report
14.1 Report both determinations and the average of the two determinations as the drop melting point of the sample under test.
14.1.1 The PDF report generated on a USB stick or transferred to an Ethernet connected PC may be examined for photos of
the drop to verify that the drop occurred correctly. See Fig. 6.

15. Precision and Bias


15.1 The precision of this test method is based on an interlaboratory study of ASTM D127 – 08 (2014), Standard Test Method
for Drop Melting Point of Petroleum Wax, Including Petrolatum, conducted in 2014. Eleven laboratories tested a total of nineteen
different wax samples. Every “test result” represents an individual determination. All labs were asked to report duplicate test results
for every material tested. Practice E691 was followed for the design and analysis of the data; the details are given in ASTM
Research Report No. RR:D02-1921.4

4
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1921. Contact ASTM Customer
Service at service@astm.org.

5
D127 − 19

iTeh Standards
(https://standards.iteh.ai)
Document Preview
ASTM D127-19
https://standards.iteh.ai/catalog/standards/sist/ffcb8b4f-8108-4174-98cd-ffa3ca6ab30d/astm-d127-19
FIG. 3 Four Dropping Point Cups after Pouring and Cooling

15.1.1 Repeatability Limit (r)—Two test results obtained within one laboratory shall be judged not equivalent if they differ by
more than the “r” value for that material; “r” is the interval representing the critical difference between two test results for the same
material, obtained by the same operator using the same equipment on the same day in the same laboratory.
15.1.1.1 Repeatability limits are listed in Table 3.
15.1.2 Reproducibility Limit (R)—Two test results shall be judged not equivalent if they differ by more than the “R” value for
that material; “R” is the interval representing the critical difference between two test results for the same material, obtained by
different operators using different equipment in different laboratories.
15.1.2.1 Reproducibility limits are listed in Tables 1-3.
15.1.3 The above terms (repeatability limit and reproducibility limit) are used as specified in Practice E177.
15.1.4 Any judgment in accordance with statements 15.1.1 and 15.1.2 would have an approximate 95 % probability of being
correct.
15.2 Bias—At the time of the study, there was no accepted reference material suitable for determining the bias for this test
method, therefore no statement on bias is being made.
15.3 The precision statement was determined through statistical examination of all reported results, from eleven laboratories,
on nineteen materials. These nineteen materials were identified generically in the tables above. ÷DSC analysis showed in general
that waxes with a narrow melting range had a consistent dropping point with small variation. Waxes with a broad melting range,
such as the plant wax blends, showed much greater variability in the dropping point by both methods A and B.
15.4 To judge the equivalency of two test results, it is recommended to choose the material closest in characteristics to the test
material.
16. Keywords
16.1 drop melting point; petrolatum; petroleum wax; wax

You might also like