1、Designation: D3944 12 (Reapproved 2017)Standard Test Method forSolidification Point of Petroleum Wax1This standard is issued under the fixed designation D3944; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for rapidly deter-mining the solidification point of petroleum wax.NOTE 1This test method is
3、also applicable to similar materials such assynthetic waxes but the precision may vary.1.2 The values stated in SI units are to be regarded as thestandard.1.2.1 ExceptionThe values given in parentheses are forinformation only1.3 This standard does not purport to address all of thesafety problems, if
4、 any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recogniz
5、ed principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D87 Test Method for Melt
6、ing Point of Petroleum Wax(Cooling Curve)D127 Test Method for Drop Melting Point of PetroleumWax, Including PetrolatumD938 Test Method for Congealing Point of PetroleumWaxes, Including PetrolatumE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions of Terms Specific to
7、This Standard:3.1.1 solidification point of petroleum wax, nthat tempera-ture in the cooling curve of the wax where the slope of thecurve first changes significantly as the wax sample changesfrom a liquid to a solid state.4. Summary of Test Method4.1 A 50 mg sample of wax is placed in a test tube at
8、ambient temperature and heated above the solidification pointof the wax sample. A thermocouple probe, attached to arecorder, is inserted into the wax sample, which is allowed tocool at room temperature. The thermocouple response of thecooling wax traces a curve on the chart paper of the recorder.The
9、 first significant change in the slope of the curve is thesolidification point.5. Significance and Use5.1 The related methods of determining the melt point ofpetroleum wax are relatively time-consuming. This methodendeavors to reduce the duration of testing significantly and atthe same time maintain
10、 a reasonable precision. This methodcan be useful for quality control of petroleum waxes as well asresearch and product development work on these waxes.5.2 For methods used for testing melt points of petroleumwaxes, see Tests Method D87, D127, including Petrolatum andTest Method D938.6. Apparatus6.1
11、 Thermocouple, with an iron-constantan junction.36.2 Recorder, capable of recording voltage and equippedwith a time-base module. The recorder should have thefollowing minimum specifications:6.2.1 Span, 0 mV to 10 mV or other suitable ranges.6.2.2 Accuracy, 0.25 % of full scale.1This test method is u
12、nder the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.10.0A on Physical/Chemical Properties.Current edition approved June 1, 2017. Published July 2017. Originally approvedin 1980. Last previous edition appro
13、ved in 2012 as D3944 12. DOI: 10.1520/D3944-12R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Suitable t
14、hermocouples are available from: Claud S. Gordon Co., 5710Kenosha St., Richmond, IL 60071, (815) 678-2211. For “J” (iron-constantan)junction the following is suitable: Xactpak Type MM Assembly, Catalog No.402-1101.Junction: grounded (G)Transition fitting: TH 2780-020Thermocouple wire: J30-1-305L (le
15、ngth of metal sheath)E (lead length): specify length desired.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization establis
16、hed in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.16.2.3 Step Response Time, 1 s full scale, 3 s full scale is alsoappropriate.6.2.4 Zero Junction/Reference Ju
17、nction/Temperature Com-pensated JunctionMust be included.6.3 TFE-Fluorocarbon Holder AdapterSee Fig. 1 and Fig.2.46.4 TFE-Fluorocarbon Disk Centering GuideSee Fig. 1and Fig. 2.46.5 Test Tubes, 6mmby50mm.6.6 Vial, 25 mm by 52 mm.6.7 Apparatus for Calibrating Temperature Recorder:6.7.1 Stainless Steel
18、 Beaker, 1000 mL.6.7.2 Heating Mantle, to fit 6.7.1.6.7.3 Autotransformer to control heat to 6.7.2.6.7.4 Variable-Speed-Stirrer.6.7.5 Thermometer, or other temperature measuring device,as specified in A1.1.6.8 Methods for Heating Specimen:6.8.1 Hot Air Blower at 1000 W, 1200 W, or other suitablepowe
19、r. This could be a laboratory or a household hair dryertype.6.8.2 Aluminum Heating Block, about 50 mm by 50 mm by50 mm. In the center of one face of the block, a hole is made7 mm in diameter and 37 mm deep to accommodate a 6 mm by50 mm test tube and another hole adjacent to it to accommo-date a 110
20、V, 30 W cartridge heater, about 9 mm by 38 mm,commercially available (see Fig. 2).6.8.2.1 Autotransformer, to control heat in 6.8.2.7. Procedure7.1 Calibrate the recorder at least every 60 days when infrequent use (see Annex A1).7.2 Obtain a wax sample representative of the material to betested.7.3
21、Using a balance accurate to at least 1 mg, weigh50 mg 6 5 mg of sample by putting a few tiny pieces of solidwax into a tared 6 mm by 50 mm test tube.7.4 Start the temperature recorder.Ahorizontal pen speed ofabout 150 mm (5 in.) 10 min for a X-Y recorder or a chartspeed of about 150 mm (5 in.) 10 mi
22、n for a strip chart recorderis usually appropriate.7.5 Heat the sample by any convenient method, such as byuse of:7.5.1 A hot air blower.7.5.2 An aluminum heating block.7.6 When using any method of heating a sample, note thatthe wax absorbs heat slowly. Hence caution must be used notto overheat the
23、surface near the heating medium. Overheatedwax can degrade. A minute amount of degradation affectsresults.7.7 When the sample melts, insert the thermocouple probeinto the melted wax.7.8 Let the wax sample temperature rise 10 C to 15 Cabove the expected solidification point.7.9 Transfer the 6 mm by 5
24、0 mm test tube, together with itsheated specimen, from the heating medium to a 25 mm by52 mm vial which acts as a cooling chamber (See Fig. 1).7.10 Let the specimen cool until the curve traced by thecooling wax on the recorder chart paper levels off.4Not commercially available and hence must be made
25、 in a machine shop orelsewhere.FIG. 1 Solidification Point ApparatusD3944 12 (2017)27.11 Determine the point in the curve which shows the firstsignificant change in the slope of the curve (see Fig. 3). This isthe solidification point.8. Report8.1 Report the solidification point to the nearest 0.1 C.
26、9. Precision and Bias59.1 The precision of this test method as determined bystatistical examination of interlaboratory results is as follows:9.1.1 RepeatabilityThe difference between two testresults, obtained by the same operator with the same apparatusunder constant operating conditions on identica
27、l material,would in the long run, in the normal and correct operation ofthe test method, exceed the following values only in one casein twenty:Distillate waxes 0.6 C (1.0 F)Residual waxes 0.7 C (1.3 F)9.1.2 ReproducibilityThe difference between two singleand independent results obtained by different
28、 operators work-ing in different laboratories on identical test material would, inthe long run, in the normal and correct operation of the testmethod, exceed the following values only in one case intwenty:Distillate waxes 1.2 C (2.2 F)Residual waxes 2.4 C (4.3 F)9.2 The precision data were obtained
29、in an interlaboratorystudy involving five laboratories in which solidification pointsof five distillate waxes (51 C to 69 C 123 F to 155 F) andfive residual waxes (53 C to 85 C 128 F to 185 F) weredetermined.9.3 BiasThe procedure in this test method has no biasbecause the value of solidification poi
30、nt can be defined only interms of a test method.10. Keywords10.1 petroleum wax; solidification print; wax5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1133. ContactASTM CustomerService at serviceastm.org.FIG. 2 Apparatus f
31、or Heating Wax SampleD3944 12 (2017)3ANNEX(Mandatory Information)A1. CALIBRATION OF RECORDERA1.1 Set up a calibration assembly consisting of a 1000 mLbeaker, with the thermocouple probe suspended in the centerand with a thermometer or other thermometric device withequal or better accuracy suspended
32、in a closely adjacentposition at the proper immersion level. The thermometricdevice should cover a range of 32 C to 127 C (90 F to260 F). If used, mercury-in-glass thermometers shall conformto the requirements prescribed in Specification E1,orinSpecifications for IP Standard Thermometers:Thermometer
33、 Range Thermometer Number32 C to 127 C 61C90 F to 260 F 61FA1.2 Place hot water which is near boiling at about 95 C inthe beaker and stir thoroughly with a variable speed stirrer.Start the recorder. As the water cools, record the exacttemperature reading and the recorder pen reading (inmillivolts),
34、taking a series of readings at 5 C intervals until thebath cools to 50 C.A1.3 Plot a calibration curve, showing the pen reading onthe abscissa (X-axis) and the corrected value (certified thermo-metric device readings) on the ordinate (Y-axis). Use this plotfor obtaining corrected solidification poin
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38、ittee 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 aboveaddre
39、ss or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.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, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 3 A Typical CurveD3944 12 (2017)4
