1、Designation: D 721 06Designation: 158/69(85)An American National StandardStandard Test Method forOil Content of Petroleum Waxes1This standard is issued under the fixed designation D 721; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method co
3、vers the determination of oil inpetroleum waxes having a congealing point of 30C (86F) orhigher as determined in accordance with Test Method D 938,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 result
4、ing in the formation oftwo liquid phases. If this occurs, the test method is not applicable to thematerial under test.1.2 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onl
5、yand are not considered standard.1.3 This standard does not purport to address all of thesafety concerns, if 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 limitat
6、ions prior to use.2. Referenced Documents2.1 ASTM Standards:3D 938 Test Method for Congealing Point of PetroleumWaxes, Including PetrolatumE1 Specification for ASTM Liquid-in-Glass ThermometersE 128 Test Method for Maximum Pore Diameter and Per-meability of Rigid Porous Filters for Laboratory Use2.2
7、 Energy Institute Standards:Specification for IP Standard Thermometers43. Summary of Test Method3.1 The sample is dissolved in methyl ethyl ketone, thesolution cooled to 32C (25F) to precipitate the wax, andfiltered. The oil content of the filtrate is determined byevaporating the methyl ethyl ketone
8、 and weighing the residue.4. Significance and Use4.1 The oil content of a wax may have significant effects onseveral of its properties, such as strength, hardness, flexibility,scuff resistance, coefficient of friction, coefficient of expansion,melting point, and oil straining. The importance of thes
9、e effectsmay be dependent upon the ultimate use of the wax.5. Apparatus5.1 Filter Stick and Assembly, consisting of a 10-mmdiameter sintered glass filter stick of 10 to 15 m maximumpore diameter as determined by the method in Appendix X1,provided with an air pressure inlet tube and delivery nozzle.
10、Itis provided with a ground-glass joint to fit a 25 by 170-mm testtube. The dimensions for a suitable filtration assembly areshown in Fig. 1.NOTE 2A metallic filter stick may be employed if desired. A filterstick made of stainless steel and having a 12.7mm (12-in.) disk of 10 to15-m maximum pore dia
11、meter, as determined by Test Method E 128, hasbeen found to be satisfactory.5The metallic apparatus is inserted into a 251This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10.0A on Physical/Chemica
12、l Properties.Current edition approved Nov. 1, 2006. Published November 2006. Originallyapproved in 1943. Last previous edition approved in 2005 as D 721-05.In the IP, this test method is under the jurisdiction of the StandardizationCommittee. This test method was issued as a joint ASTM-IP tentative
13、in 1964.This test method was prepared jointly by the Technical Association of Pulp andPaper Industry and ASTM International.This test method has been adopted for use by government agencies to replaceMethod 5431 of Federal Test Method Standard No. 79lb.2This test method is being used by some laborato
14、ries for products of higher oilcontent.3For 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.4Available from Energy
15、 Institute, 61 New Cavendish St., London, WIG 7AR,U.K.5The sole source of supply of a suitable metal filter stick with designatedporosity G known to the committee at this time is the Pall Corporation, 2200Northern Boulevard East Hills, NY 11548. A list of United Kingdom suppliers canbe obtained from
16、 Energy Institute, 61 New Cavendish St., London, W1G 7AR,United Kingdom. If you are aware of alternative suppliers, please provide thisinformation to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may att
17、end.1*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.by 150mm test tube and held in place by means of a cork.5.2 Cooling Bath, consisting of an insulated box with 30 65
18、-mm (1.2 6 0.2-in.) holes in the center to accommodate anydesired number of test tubes. The bath may be filled with asuitable medium such as kerosine, and may be cooled bycirculating a refrigerant through coils, or by using solid carbondioxide. A suitable cooling bath to accommodate three testtubes
19、is shown in Fig. 2.5.3 Pipet, or equivalent dispensing device capable of deliv-ering 1 6 0.05 g of molten wax.5.4 Transfer Pipet, or equivalent volume dispensing device,capable of delivering 15 6 0.06 mL.5.5 Air Pressure Regulator, designed to supply air to thefiltration assembly (8.5) at the volume
20、 and pressure required togive an even flow of filtrate. Either the conventional pressure-reducing valve or a mercury bubbler-type regulator has beenfound satisfactory. The latter type, illustrated in Fig. 3, consistsof a 250-mL glass cylinder and a T-tube held in the cylinder bymeans of a rubber sto
21、pper grooved at the sides to permit theescape of excess air. The volume and pressure of the airsupplied to the filtration assembly is regulated by the depth towhich the T-tube is immersed in mercury at the bottom of thecylinder. Absorbent cotton placed in the space above themercury prevents the loss
22、 of mercury by spattering. The airpressure regulatory is connected to the filter stick and assemblyby means of rubber tubing.5.6 Temperature Measuring Device:5.6.1 Thermometer, having a range as shown below andconforming to the requirements as prescribed in SpecificationE1, or in the Specification f
23、or IP Standard Thermometers.Thermometer NumberTemperature Range ASTM IP37 to +21C 71C 72C35 to +70F 71F 72F5.6.2 Temperature measuring devices other than those de-scribed in 5.6.1 are satisfactory for this test method, providedthat they exhibit the same temperature response as the equiva-lent mercur
24、y-in-glass thermometers.5.7 Weighing Bottles, glass-stoppered, having a typical ca-pacity of 15 to 25 mL.5.8 Evaporation Assembly, consisting of an evaporatingcabinet and connections, essentially as illustrated in Fig. 4, andcapable of maintaining a temperature of 35 6 1C (95 6 2F)around the evapora
25、tion flask. Construct the jets with an insidediameter of 4 6 0.2 mm for delivering a stream of clean, dryair vertically downward into the weighing bottle. Support eachjet so that the tip is 15 6 5 mm above the surface of the liquidat the start of the evaporation. Supply purified air at the rate of2
26、to 3 L/min per jet. One way to purify the air is by passagethrough a tube of approximately 10-mm bore packed loosely toa height of approximately 200 mm with absorbent cotton.Periodically check the cleanliness of the air by evaporating 4mL of methyl ethyl ketone by the procedure specified in 8.5.When
27、 the residue does not exceed 0.1 mg, the evaporationequipment is operating satisfactorily.5.9 Analytical Balance, capable of reproducing weights to0.1 mg.5.10 Wire StirrerA piece of stiff wire, made of iron,stainless steel, or Nichrome wire of about No. 20 B thenimmediately immerse in the mixture th
28、e clean dry filter stickwhich has previously been cooled by placing it in a test tubeand holding at 34.5 6 1.0C (30.0 6 2.0F) in the coolingbath for a minimum of 10 min. Seat the ground-glass joint ofthe filter so as to make an airtight seal. Place an unstopperedweighing bottle, previously weighed t
29、ogether with the glassstopper to the nearest 0.1 mg, under the delivery nozzle of thefiltration assembly.NOTE 7Take every precaution to ensure the accuracy of the weight ofthe stoppered weighing bottle. Prior to determining this weight, rinse theclean, dry weighing bottle and stopper with methyl eth
30、yl ketone, wipe dryon the outside with a cloth, and place in the evaporation assembly to dryfor about 5 min. Then remove the weighing bottle and stopper, place nearthe balance, and allow to stand for 10 min prior to weighing. Stopper thebottle during this cooling period. Once the weighing bottle and
31、 stopperhave been dried in the evaporation assembly, lift only with forceps. Takecare to remove and replace the glass stopper with a light touch.8.5 Apply air pressure to the filtration assembly, and imme-diately collect about 4 mL of filtrate in the weighing bottle.Release the air pressure to permi
32、t the liquid to drain backslowly from the delivery nozzle. Remove the weighing bottleimmediately, and stopper and weigh to at least the nearest10 mg without waiting for it to come to room temperature.Unstopper the weighing bottle and place it under one of the jetsin the evaporation assembly maintain
33、ed at 35 6 1C (95 62F), with the air jet centered inside the neck, and the tip 15 65 mm above the surface of the liquid. After the solvent hasevaporated, which usually takes less than 30 min, remove thebottle and stopper, and place them near the balance. Allow tostand for 10 min and weigh to the nea
34、rest 0.1 mg. Repeat theevaporation procedure, using a 5-min evaporation periodinstead of 30 min, until the loss between successive weighingsis not over 0.2 mg.9. Calculation9.1 Calculate the amount of oil in the wax as follows:Oil in wax, weight % 5 100 AC/BD! 0.15 (1)where:A = weight of oil residue
35、, g,B = weight of wax sample, g,C = weight of solvent, g, obtained by subtracting weightof test tube plus wax sample (8.1) from weight oftest tube and contents (8.2),D = weight of solvent evaporated, g, obtained by sub-tracting weight of weighing bottle plus oil residuefrom weight of weighing bottle
36、 plus filtrate (8.5),and0.15 = average factor correcting for the solubility of wax inthe solvent at 32C (25F).10. Report10.1 Report the result as oil content, Test Method D 721. Ifthe result is negative, report as zero.11. Precision and Bias11.1 PrecisionThe precision of this test method as deter-mi
37、ned by statistical examination of interlaboratory results is asfollows:11.1.1 RepeatabilityThe difference between two test re-sults, obtained by the same operator with the same apparatusunder constant operating conditions on identical test material,would in the long run, in the normal and correct op
38、eration ofthe test method, exceed the following values only in one casein twenty:0.06 1 8% of the mean11.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, in
39、 the normal and correct operation of the testmethod, exceed the following values only in one case intwenty:0.2 1 11% of the mean11.2 BiasThe procedure in this test method has no biasbecause the value of oil content can be defined only in terms ofa test method.12. Keywords12.1 oil content; petroleum
40、wax; waxAll dimensions are in millimetresFIG. 3 Air Pressure RegulatorD721064All dimensions are in millimetres (inches)FIG. 4 Evaporation AssemblyD721065APPENDIX(Nonmandatory Information)X1. TEST METHOD FOR MEASUREMENT OF MAXIMUM PORE DIAMETER OF RIGID POROUS FILTERSX1.1 ScopeX1.1.1 This test method
41、 covers the determination of theacceptability of porous filter sticks used for filtration in TestMethod D 721. This test method establishes the maximum porediameter and also provides a means of detecting and measuringchanges which occur form continued use.X1.2 DefinitionX1.2.1 maximum pore diametert
42、he diameter in microme-ters of the largest opening in the filter.NOTE X1.1It is recognized that the maximum pore diameter asdefined herein does not necessarily indicate the physical dimensions of thelargest pore in the filter. It is further recognized that the pores are highlyirregular in shape. Bec
43、ause of the irregularity in shape and otherphenomena characteristic of filtration, a filter may be expected to retain allparticles larger than the maximum pore diameter as defined and deter-mined herein, and will generally retain particles which are much smallerthan the determined diameter.X1.3 Summ
44、ary of Test MethodX1.3.1 The filter is cleaned and wetted with water. It is thenimmersed in water and air pressure is applied against its uppersurface until the first bubble of air passes through the filter. Themaximum pore diameter is calculated from the surface tensionof water and the applied pres
45、sure.X1.4 ApparatusX1.4.1 Pressure Measuring Device, mercury-filled manom-eter or equivalent, capable of measuring pressures in incre-ments of 0.5 mm of Hg.X1.4.2 Air Supply, clean and filtered.X1.4.3 Air Pressure Regulator, needle-valve type.X1.4.4 Drying Oven.X1.5 ProcedureX1.5.1 Clean the filter
46、sticks by soaking in concentratedhydrochloric acid, and then wash them with distilled water.Rinse with acetone, air dry, and place in drying oven at 220F(105C) for 30 min.X1.5.2 Thoroughly wet the clean filter to be tested bysoaking it in distilled water.X1.5.3 Assemble the apparatus as shown in Fig
47、. X1.1.Apply pressure slowly from a source of clean air.X1.5.4 Immerse the filter just below the surface of thewater.NOTE X1.2If a head of liquid exists above the surface of the filter, theback pressure produced must be deducted from the observed pressure.X1.5.5 Increase the air pressure to about 10
48、 mm Hg (orequivalent pressure value if using different units) below theacceptable pressure limit and then at a slow uniform rateequivalent to about 3 mm Hg/min until the first bubble passesthrough the filter. This can be conveniently observed byplacing the beaker or test tube over a mirror. Read the
49、 pressuremeasuring device when the first bubble passes off the undersideof the filter.X1.6 CalculationX1.6.1 Calculate the pore diameter as follows:D 5 2180/pwhere:D = pore diameter, m, andp = pressure reading, mm Hg.NOTE X1.3From this equation, pressure corresponding to the upperand lower limits of the specified pore diameters can be calculated. Thesepressures may be used for acceptance testing.FIG. X1.1 Assembly of Apparatus for Checking Pore Diameter orFilter SticksD721066SUMMARY OF CHANGESSubcommittee D02.10 has identified the locatio
