ASTM D721-2017 Standard Test Method for Oil Content of Petroleum Waxes《石油蜡含油量的标准试验方法》.pdf

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1、Designation: D721 15D721 17Designation: 158/69(85)Standard Test Method forOil Content of Petroleum Waxes1This standard is issued under the fixed designation D721; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev

2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript 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*1.1 This test method covers the determinati

3、on of oil in petroleum waxes having a congealing point of 30 C (86 F) or higheras determined in accordance with Test Method D938, and containing not more than 15 % of oil.2NOTE 1With some types of waxes, of oil contents greater than 5 %, there may be an incompatibility with MEK resulting in the form

4、ation of twoliquid phases. If this occurs, the test method is not applicable to the material under test.1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information only and are not

5、 considered standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to

6、use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers t

7、o Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D938 Test Method for Congealing Point of Petroleum Waxes, Including PetrolatumE1 Specification for ASTM Liquid-in-Glass ThermometersE128 Test Method for Maximum Pore Diameter and Permeability of Rigid Porous Filters for Laboratory Us

8、eE2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids2.2 Energy Institute Standards:Specification for IP Standard Thermometers43. Summary of Test Method3.1 The sample is dissolved in methyl ethyl ketone, the solution cooled to 32 C (25 F) to precipitate the wax

9、, and filtered.The oil content of the filtrate is determined by evaporating the methyl ethyl ketone and weighing the residue.4. Significance and Use4.1 The oil content of a wax may have significant effects on several of its properties, such as strength, hardness, flexibility, scuffresistance, coeffi

10、cient of friction, coefficient of expansion, melting point, and oil straining. The importance of these effects may bedependent upon the ultimate use of the wax.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct resp

11、onsibility of SubcommitteeD02.10.0A on Physical/Chemical Properties.Current edition approved June 1, 2015May 1, 2017. Published June 2015June 2017. Originally approved in 1943. Last previous edition approved in 20112015 as D721 06(2011).D721 15. DOI: 10.1520/D0721-15.10.1520/D0721-17.In the IP, this

12、 test method is under the jurisdiction of the Standardization Committee. This test method was issued as a joint ASTM-IP tentative in 1964.This test method was prepared jointly by the Technical Association of Pulp and Paper Industry and ASTM International.This test method has been adopted for use by

13、government agencies to replace Method 5431 of Federal Test Method Standard No. 79lb.2 This test method is being used by some laboratories for products of higher oil content.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For An

14、nual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.4 Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indicati

15、on of what changes have been made to the previous version. Becauseit 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 versionof the standard as published by ASTM is to be consi

16、dered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Apparatus5.1 Filter Stick and Assembly, consisting of a 10 mm diameter sintered glass filt

17、er stick of 10 m to 15 m maximum porediameter as determined by the method in Appendix X1, provided with an air pressure inlet tube and delivery nozzle. It is providedwith a ground-glass joint to fit a 25 mm by 170 mm test tube. The dimensions for a suitable filtration assembly are shown in Fig.1.NOT

18、E 2Ametallic filter stick may be employed if desired.Afilter stick made of stainless steel and having a 12.7 mm (12 in.) disk of 10 m to 15 mmaximum pore diameter, as determined by Test Method E128, has been found to be satisfactory.5 The metallic apparatus is inserted into a 25 mm by150 mm test tub

19、e and held in place by means of a cork.5.2 Cooling Bath, consisting of an insulated box with 30 mm 6 5 mm (1.2 in. 6 0.2 in.) holes in the center to accommodateany desired number of test tubes. The bath may be filled with a suitable medium such as kerosine, and may be cooled by circulatinga refriger

20、ant through coils, or by using solid carbon dioxide. A suitable cooling bath to accommodate three test tubes is shown inFig. 2.5.3 Pipet, or equivalent dispensing device capable of delivering 1 g 6 0.05 g of molten wax.5.4 Transfer Pipet, or equivalent volume dispensing device, capable of delivering

21、 15 mL 6 0.06 mL.5.5 Air Pressure Regulator, designed to supply air to the filtration assembly (8.5) at the volume and pressure required to givean even flow of filtrate. Either the conventional pressure-reducing valve or a mercury bubbler-type regulator has been foundsatisfactory. The latter type, i

22、llustrated in Fig. 3, consists of a 250 mL glass cylinder and a T-tube held in the cylinder by meansof a rubber stopper grooved at the sides to permit the escape of excess air. The volume and pressure of the air supplied to thefiltration assembly is regulated by the depth to which the T-tube is imme

23、rsed in mercury at the bottom of the cylinder. Absorbentcotton placed in the space above the mercury prevents the loss of mercury by spattering. The air pressure regulatory is connectedto the filter stick and assembly by means of rubber tubing.5.6 Temperature Measuring Temperature-Measuring Device:5

24、 The sole source of supply of a suitable metal filter stick with designated porosity G known to the committee at this time is the Pall Corporation, 2200 Northern BoulevardEast Hills, NY 11548. A list of United Kingdom suppliers can be obtained from Energy Institute, 61 New Cavendish St., London, W1G

25、 7AR, United Kingdom. If you areaware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1 which you may attend.All dimensions are in millimetresFIG. 1 Filte

26、r StickD721 1725.6.1 Thermometer, having a range as shown below and conforming to the requirements as prescribed in Specification E1,Specification E2251, or in the Specification for IP Standard Thermometers.Thermometer NumberTemperature Range ASTM IP38 C to +50 C S5C .36 F to +120 F S5F .37 C to +21

27、 C 71C 72C35 F to +70 F 71F 72F5.6.2 Temperature measuring Temperature-measuring devices other than those described in 5.6.1 are satisfactory for this testmethod, provided that they exhibit the same temperature response as the equivalent mercury-in-glass thermometers.5.7 Weighing Bottles, glass-stop

28、pered, having a typical capacity of 15 mL to 25 mL.5.8 Evaporation Assembly, consisting of an evaporating cabinet and connections, essentially as illustrated in Fig. 4, and capableof maintaining a temperature of 35 C 6 1 C (95 F 6 2 F) around the evaporation flask. Construct the jets with an insided

29、iameter of 4 mm 6 0.2 mm for delivering a stream of clean, dry air vertically downward into the weighing bottle. Support eachjet so that the tip is 15 mm 6 5 mm above the surface of the liquid at the start of the evaporation. Supply purified air at the rateof 2 Lmin to 3 Lmin per jet. One way to pur

30、ify the air is by passage through a tube of approximately 10-mm10 mm bore packedAll dimensions are in millimetres (inches)FIG. 2 Cooling BathD721 173loosely to a height of approximately 200 mm with absorbent cotton. Periodically check the cleanliness of the air by evaporating4 mL of methyl ethyl ket

31、one by the procedure specified in 8.5. When the residue does not exceed 0.1 mg, the evaporationequipment is operating satisfactorily.5.9 Analytical Balance, capable of reproducing weights to 0.1 mg.5.10 Wire StirrerA piece of stiff wire, made of iron, stainless steel, or Nichrome wire of about No. 2

32、0 B then immediately immerse in the mixture the clean, dry filter stick which has previously been cooled by placing it in a testtube and holding at 34.5 C 6 1.0 C (30.0 F 6 2.0 F) in the cooling bath for a minimum of 10 min. Seat the ground-glassjoint of the filter so as to make an airtight seal. Pl

33、ace an unstoppered weighing bottle, previously weighed together with the glassstopper to the nearest 0.1 mg, under the delivery nozzle of the filtration assembly.NOTE 7Take every precaution to ensure the accuracy of the weight of the stoppered weighing bottle. Prior to determining this weight, rinse

34、 the clean,dry weighing bottle and stopper with methyl ethyl ketone, wipe dry on the outside with a cloth, and place in the evaporation assembly to dry for about5 min. Then remove the weighing bottle and stopper, place near the balance, and allow to stand for 10 min prior to weighing. Stopper the bo

35、ttle duringthis cooling period. Once the weighing bottle and stopper have been dried in the evaporation assembly, lift only with forceps. Take care to remove andreplace the glass stopper with a light touch.8.5 Apply air pressure to the filtration assembly, and immediately collect about 4 mL of filtr

36、ate in the weighing bottle. Releasethe air pressure to permit the liquid to drain back slowly from the delivery nozzle. Remove the weighing bottle immediately, andstopper and weigh to at least the nearest 10 mg without waiting for it to come to room temperature. Unstopper the weighing bottleand plac

37、e it under one of the jets in the evaporation assembly maintained at 35 C 6 1 C (95 F 6 2 F), with the air jet centeredinside the neck, and the tip 15 mm 6 5 mm above the surface of the liquid. After the solvent has evaporated, which usually takesless than 30 min, remove the bottle and stopper, and

38、place them near the balance. Allow to stand for 10 min and weigh to thenearest 0.1 mg. Repeat the evaporation procedure, using a 5 min evaporation period instead of 30 min, until the loss betweensuccessive weighings is not over 0.2 mg.9. Calculation9.1 Calculate the amount of oil in the wax as follo

39、ws:Oil in wax,weight %5100 AC/BD!20.15 (1)where:where:A = weight of oil residue, g,B = weight of wax sample, g,C = weight of solvent, g, obtained by subtracting weight of test tube plus wax sample (8.1) from weight of test tube andcontents (8.2),D = weight of solvent evaporated, g, obtained by subtr

40、acting weight of weighing bottle plus oil residue from weight ofweighing bottle plus filtrate (8.5), and0.15 = average factor correcting for the solubility of wax in the solvent at 32 C (25 F).A = weight of oil residue, g,B = weight of wax sample, g,C = weight of solvent, g, obtained by subtracting

41、weight of test tube plus wax sample (8.1) from weight of test tube andcontents (8.2),D = weight of solvent evaporated, g, obtained by subtracting weight of weighing bottle plus oil residue from weight ofweighing bottle plus filtrate (8.5), and0.15 = average factor correcting for the solubility of wa

42、x in the solvent at 32 C (25 F).10. Report10.1 Report the result as oil content, Test Method D721. If the result is negative, report as zero.11. Precision and Bias11.1 PrecisionThe precision of this test method as determined by statistical examination of interlaboratory results is asfollows:11.1.1 R

43、epeatabilityThe difference between two test results, obtained by the same operator with the same apparatus underconstant operating conditions on identical test material, would in the long run, in the normal and correct operation of the testmethod, exceed the following values only in one case in twen

44、ty:0.0618%of the mean11.1.2 ReproducibilityThe difference between two single and independent results obtained by different operators working indifferent laboratories on identical test material would, in the long run, in the normal and correct operation of the test method,exceed the following values

45、only in one case in twenty:0.2111%of the mean11.2 BiasThe procedure in this test method has no bias because the value of oil content can be defined only in terms of a testmethod.D721 17612. Keywords12.1 oil content; petroleum wax; waxAPPENDIX(Nonmandatory Information)X1. TEST METHOD FOR MEASUREMENT

46、OF MAXIMUM PORE DIAMETER OF RIGID POROUS FILTERSX1.1 ScopeX1.1.1 This test method covers the determination of the acceptability of porous filter sticks used for filtration in Test MethodD721. This test method establishes the maximum pore diameter and also provides a means of detecting and measuring

47、changeswhich occur form continued use.X1.2 DefinitionX1.2.1 maximum pore diameterthe diameter in micrometers of the largest opening in the filter.NOTE X1.1It is recognized that the maximum pore diameter as defined herein does not necessarily indicate the physical dimensions of the largest porein the

48、 filter. It is further recognized that the pores are highly irregular in shape. Because of the irregularity in shape and other phenomena characteristicof filtration, a filter may be expected to retain all particles larger than the maximum pore diameter as defined and determined herein, and will gene

49、rallyretain particles which are much smaller than the determined diameter.X1.3 Summary of Test MethodX1.3.1 The filter is cleaned and wetted with water. It is then immersed in water and air pressure is applied against its upper surfaceuntil the first bubble of air passes through the filter. The maximum pore diameter is calculated from the surface tension of waterand the applied pressure.X1.4 ApparatusX1.4.1 Pressure Measuring Pressure-Measuring Device, mercury-filled manometer or equivalent, capable of measuring pre