ASTM D127-08 Standard Test Method for Drop Melting Point of Petroleum Wax, Including Petrolatum

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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 determined by the original Test Method D127, Method A 1.1 This test method covers the determination of the drop 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- priate safety, health, and environmental practices and deter- 1.1.1 Test Method A—The dropping point of wax is deter- mine the applicability of regulatory limitations prior to use mined with a mercury in glass thermometer, as stated below 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 (Cooling Curve) 1.1.2 Test Method B—The dropping point of wax deter- D938 Test Method for Congealing Point of Petroleum mined in a dropping point cup in an instrument which detects Waxes, Including Petrolatum the drop and measures the temperature electronically, with a D3104 Test Method for Softening Point of Pitches (Mettler platinum thermometer instead of with mercury Mercury has Softening Point Method) been recognized as a poison and a health hazard Removing D3954 Test Method for Dropping Point of Waxes mercury from laboratories is a way of making the measuring E1 Specification for ASTM Liquid-in-Glass Thermometers process more inherently safe The instrumental dropping point 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 TEST METHOD A Current edition approved Nov 1, 2019 Published February 2020 Originally approved in 1922 Last previous edition approved in 2015 as D127 – 08 (2015) 3 Terminology DOI: 10.1520/D0127-19 3.1 Definitions: 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 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 In 1963, the title, scope, and definition were changed to define the determination Standards volume information, refer to the standard’s Document Summary page on of “drop melting point.” Sections on procedure, report, and precision were revised, the ASTM website 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 Only Method A of this test method is equivalent to IP 133/79 (87) *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 prescribed conditions NOTE 2—A dipping temperature of 11 °C (20 °F) above the congealing point in accordance with Test Method D938 usually will be 6 °C to 11 °C 4 Summary of Test Method (10 °F to 20 °F) above the actual drop melting point 4.1 Specimens are deposited on two thermometer bulbs by 7.2 Securely fix the thermometers in the test tubes by means dipping chilled thermometers into the sample The thermom- of suitable stoppers, such as corks, so that the tip of each eters bearing the specimens are placed in test tubes and heated thermometer is approximately 15 mm above the bottom of its by means of a water bath until the specimens melt and the first test tube Insert the test tubes in the water bath which is at drop falls from each thermometer bulb The average of the 16 °C 6 1 °C (60 °F 6 2 °F) and adjust the height of the test temperatures at which these drops fall is the drop melting point tubes so that the immersion marks on the thermometers are of the sample level with the top surface of the water Raise the temperature of the bath at a rate of approximately 2 °C (3 °F) ⁄min to 38 °C 5 Significance and Use (100 °F), then at a rate of approximately 1 °C (2 °F) ⁄min until 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, is often used to measure the melting characteristics of petro- 8 Report 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- eter 9.1.1 Repeatability—The difference between two test 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 E1 or in specifications for IP Standard Thermometers: 9.1.2 Reproducibility—The difference between two single and independent results obtained by different operators work- Thermometer Number ing in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test Thermometer Range ASTM IP method, exceed the following values only in one case in 32 °C to 127 °C twenty: 90 °F to 260 °F 61C 63C 1.3 °C (2.4 °F) 61F 6.4 Bath Thermometer, any suitable type, accurate to 0.5 °C (1 °F) throughout the required range 7 Procedure NOTE 3—The following information on the precision of this test method was developed by the Institute of Petroleum (now Energy Institute) in 7.1 Secure a sample of sufficient size that is representative London and is being investigated: of the material under inspection Use a fresh portion of the sample for each set of two determinations Melt the sample (1) Results of duplicate tests should not differ by more than the slowly until the temperature reaches at least 11 °C (20 °F) following amounts: above the expected drop melting point Place sufficient sample in a flat bottom container to give a sample depth of 12 mm 6 Repeatability Reproducibility 1 mm Adjust the temperature of the sample to at least 6 °C 1 °C (2 °F) 1.2 °C (2.2 °F) (10 °F) (Note 2) above its drop melting point using any general laboratory thermometer for measurement Chill one of the test (2) These precision values were obtained in 1954 by statistical thermometer bulbs to approximately 4 °C (40 °F) Wipe dry, examination of interlaboratory test results and, quickly but carefully, immerse the chilled bulb vertically into the heated sample until it touches the bottom of the 9.2 Bias—The procedure in this test method has no bias container (about 12 mm submerged) and withdraw it immedi- because the value of drop melting point can be defined only in ately Hold the thermometer vertically away from the heat until terms of a test method the surface dulls, and then place it for at least 5 min in water TEST METHOD B 10 Summary of Test Method 10.1 In this test method, the dropping point is defined as the temperature at which the wax suspended in a cylindrical cup, 2 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 receptacle contains the molten wax underneath the drop be used to determine pitch softening points by this test method These commercially available instruments consist of a control 11 Significance and Use unit with a digital temperature indicator, with furnace built in 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 talling waxes and petrolatums and other high viscosity petro- provide this information to ASTM International Headquarters Your comments will leum waxes receive careful consideration at a meeting of the responsible technical committee,1 which you may attend FIG 1 Overview of DP70 Dropping Point Instrument 3 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 point detection A general view of the contents of the MET- 13.4.2 Fig 3—The four cups from Fig 2 have been poured TLER TOLEDO dropping point instrument is shown in Fig 1 and cooled The two cups sitting on top did not get enough wax Cavities extend way down in the center of those The one 13 Procedure 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 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) above the expected drop melting point The sample should be 13.4.3 Fig 4—A cup with wax after the drop Note the completely melted The wax should be hot enough that the hanging solidified drop and the pool of wax in the bottom of wax, when poured, remains transparent enough to see the the receiver glass opening in the bottom of the cup when the cup is poured full This ensures that no air pockets are trapped in a solidifying 13.4.4 Fig 5—Two cups in the holder shortly after removal wax that is not hot enough (See Note 4.) The cup should be from the DP70, showing the drops and wax in the bottom of the poured full to the top plus 1 mm to 2 mm above the rim As the receiver glass wax cools in the cup, it cools from the outside in and there is shrinkage in the center After cooling, any wax remaining 13.4.5 Fig 6—The photo from the report with at the above the top of the cup should be trimmed off with a flat sharp moment of the drop on the right side at 62.2 °C The sample on edge Any wax on the outside of the cup should be cleaned off the left had already dropped at 61.8 °C The second drop is The cup should temper at room temperature (20 °C to 25 °C) about to fall 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 14 Report will cause a cavity down in the center Pouring more wax in after it hardens is not recommended because an air pocket can 14.1 Report both determinations and the average of the two be trapped in the cavity A small cavity is almost unavoidable determinations as the drop melting point of the sample under for some waxes but this should not cause a problem so long as test the cup is otherwise full 14.1.1 The PDF report generated on a USB stick or trans- NOTE 4—Center cavities are caused by the outside of the cup cooling ferred to an Ethernet connected PC may be examined for and hardening before the center This can be minimized by heating the photos of the drop to verify that the drop occurred correctly sample preparation tool to near the expected drop temperature before See Fig 6 pouring into the dropping point cups The cooling becomes more uniform and the cavity less pronounced 15 Precision and Bias 13.2 Petrolatums should be dropped into ice water after they 15.1 The precision of this test method is based on an have cooled and gelled so that they retain the shape The cup interlaboratory study of ASTM D127 – 08 (2014), Standard should sit in the ice water for at least one hour Test Method for Drop Melting Point of Petroleum Wax, Including Petrolatum, conducted in 2014 Eleven laboratories 13.3 The exterior of the cup is cleaned of any wax and tested a total of nineteen different wax samples Every “test water, the cap is put on and the glass receptacle fitted to the result” represents an individual determination All labs were bottom and held It is then inserted in the sample holder asked to report duplicate test results for every material tested Usually samples are analyzed in duplicate, as the sample Practice E691 was followed for the design and analysis of the holder holds two cups The start temperature should be at least data; the details are given in ASTM Research Report No 15° below the expected drop temperature, with a 120 s wait RR:D02-1921.4 time before the temperature ramp of 1 °C ⁄minute is started When both cups have dropped, the temperature should return 15.1.1 Repeatability Limit (r)—Two test results obtained to the insert temperature and the results presented on the within one laboratory shall be judged not equivalent if they display The video of the drop can be examined if there is any differ by more than the “r” value for that material; “r” is the doubt about the drop result, and the report can be viewed to see interval representing the critical difference between two test a photo of the drop at the moment it fell results for the same material, obtained by the same operator using the same equipment on the same day in the same 13.4 Illustrations: laboratory 13.4.1 Fig 2—The dropping point cups have been recently poured The lower and right cups have been cooling for several 15.1.1.1 Repeatability limits are listed in Table 3 minutes The top cup was just poured The bottom can be seen 15.1.2 Reproducibility Limit (R)—Two test results shall be through the transparent molten wax, ensuring that there are no judged not equivalent if they differ by more than the “R” value entrapped air pockets The left cup has not been poured In the for that material; “R” is the interval representing the critical right cup, the center is still molten These cups were poured 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 4 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 a consistent dropping point with small variation Waxes with a 15.1.2.1 Reproducibility limits are listed in Tables 1-3 broad melting range, such as the plant wax blends, showed 15.1.3 The above terms (repeatability limit and reproduc- much greater variability in the dropping point by both methods ibility limit) are used as specified in Practice E177 A and B 15.1.4 Any judgment in accordance with statements 15.1.1 and 15.1.2 would have an approximate 95 % probability of 15.4 To judge the equivalency of two test results, it is being correct recommended to choose the material closest in characteristics to the test material 15.2 Bias—At the time of the study, there was no accepted reference material suitable for determining the bias for this test 16 Keywords method, therefore no statement on bias is being made 16.1 drop melting point; petrolatum; petroleum wax; wax 15.3 The precision statement was determined through sta- tistical examination of all reported results, from eleven 5 D127 − 19 FIG 3 Four Dropping Point Cups after Pouring and Cooling 6 D127 − 19 FIG 4 Wax Cup After the Drop FIG 5 Two Cups in the Holder After Removal from the DP70 7 D127 − 19 FIG 6 Report Photo at the Moment of the Drop 8 D127 − 19 TABLE 1 Dropping Point (°C) – Averages, Part A Sample Average Reproducibility Standard Reproducibility Number of Labs Reporting Deviation 1 Petrolatum 54.32 SR R 8 2 Natural plant wax 71.95 3.16 8.86 8 3 Paraffin wax 64.80 1.13 3.17 8 4 Microcrystalline wax 89.32 0.41 1.15 8 5 Natural plant wax 96.02 0.75 2.10 8 6 Paraffin wax 69.57 2.14 6.00 8 7 Praffin wax 68.85 0.58 1.64 8 8 Natural wax, beeswax 59.98 0.48 1.35 8 9 Paraffin wax 53.34 0.66 1.85 8 10 Scale wax 53.66 0.78 2.18 8 11 Natural plant wax blend 71.83 5.93 16.60 9 12 Natural plant wax blend 82.23 8.24 23.07 8 13 Polyethylene wax 111.95 7.16 20.06 3 14 Microcrystalline wax 84.70 2.21 6.19 8 15 Paraffin wax 55.95 0.76 2.13 8 16 Petrolatum 61.26 0.43 1.20 8 17 Petrolatum 59.76 1.34 3.74 8 18 Microcrystalline wax 76.82 2.35 6.58 8 19 Microcrystalline wax 81.54 7.28 20.39 8 4.23 11.84 Sample Number of Labs Reporting TABLE 2 Dropping Point (°C) – Averages, Part B 1 Petrolatum 11 2 Natural plant wax Average Reproducibility Standard Reproducibility 10 3 Paraffin wax Deviation 11 4 Microcrystalline wax 49.72 SR R 11 5 Natural plant wax 73.54 1.91 5.35 10 6 Paraffin wax 65.15 0.90 2.52 11 7 Paraffin wax 90.35 0.87 2.43 11 8 Natural wax, beeswax 97.26 0.56 1.56 11 9 Paraffin wax 70.85 1.14 3.20 11 10 Scale wax 69.98 1.03 2.88 11 11 Blend plant wax 60.18 0.81 2.27 11 12 Blend plant wax 53.56 0.75 2.09 10 13 Polyethylene wax 51.81 0.75 2.11 9 14 Microcrystalline wax 71.56 2.00 5.61 11 15 Paraffin wax 75.99 4.07 11.38 11 16 Petrolatum 113.59 5.86 16.41 11 17 Petrolatum 84.62 0.48 1.35 11 18 Microcrystalline wax 56.13 0.72 2.02 11 19 Microcrystalline wax 58.82 1.01 2.82 11 57.17 2.22 6.23 80.56 1.05 2.93 80.57 1.04 2.91 4.08 11.42 9 D127 − 19 TABLE 3 Dropping Point (°C) – Individual Determinations, Part B Sample Average Repeatability Reproducibility Repeatability Reproducibility Number of Labs Standard Deviation Standard Deviation Reporting 1 Petrolatum 49.7 r R 2 Natural plant wax 73.5 Sr SR 0.8 5.4 11 3 Paraffin wax 65.1 0.3 1.9 0.9 2.6 10 4 Microcrystalline wax 90.3 0.3 0.9 1.2 2.6 11 5 Natural plant wax 97.3 0.4 0.9 1.8 2.0 11 6 Paraffin wax 70.9 0.6 0.7 3.5 4.0 10 7 Paraffin wax 70.0 1.2 1.4 1.6 3.1 1 8 Natural wax, beeswax 60.2 0.6 1.1 0.6 2.3 11 9 Paraffin wax 53.6 0.2 0.8 0.6 2.1 1 10 Scale wax 51.8 0.2 0.8 1.5 2.4 11 11 Blend plant wax 71.6 0.5 0.8 1.4 5.7 11 12 Blend plant wax 76.0 0.5 2.0 6.2 12.2 11 13 Polyethylene wax 113.6 2.2 4.4 3.1 16.6 10 14 Microcrystalline wax 84.6 1.1 5.9 0.7 1.4 9 15 Paraffin wax 56.1 0.3 0.5 1.2 2.2 1 16 Petrolatum 58.8 0.4 0.8 0.8 2.9 1 17 Petrolatum 57.2 0.3 1.0 0.7 6.2 11 18 Microcrystalline wax 80.6 0.2 2.2 1.0 3.0 11 19 Microcrystalline wax 80.6 0.3 1.1 0.6 2.9 11 0.2 1.0 1.8 11.5 11 0.6 4.1 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 ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned in this standard Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters Your comments will receive careful consideration at a meeting of the responsible technical committee, which you may attend If you feel that your comments have not received a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website (www.astm.org) Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222 Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/ 10