1、Designation: D721 06 (Reapproved 2011)Designation: 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
2、of last revision. 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 Department of Defense.1. Scope1.1 This test method covers the determ
3、ination of oil inpetroleum waxes having a congealing point of 30C (86F) orhigher as 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 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 onlyand are not co
5、nsidered 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 limitations prior to u
6、se.2. Referenced Documents2.1 ASTM Standards:3D938 Test Method for Congealing Point of PetroleumWaxes, Including PetrolatumE1 Specification for ASTM Liquid-in-Glass ThermometersE128 Test Method for Maximum Pore Diameter and Per-meability of Rigid Porous Filters for Laboratory Use2.2 Energy Institute
7、 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 and weighing the
8、 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 these effectsmay be d
9、ependent 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. Itis provided wit
10、h 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 diameter, as determi
11、ned by Test Method E128, hasbeen found to be satisfactory.5The metallic apparatus is inserted into a 25by 150mm test tube and held in place by means of a cork.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of Sub
12、committeeD02.10.0A on Physical/Chemical Properties.Current edition approved Oct. 1, 2011. Published October 2011. Originallyapproved in 1943. Last previous edition approved in 2006 as D721-06. DOI:10.1520/D0721-06R11.In the IP, this test method is under the jurisdiction of the StandardizationCommitt
13、ee. 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 andPaper Industry and ASTM International.This test method has been adopted for use by government agencies to replaceMethod 5431 of Federal Test Method Stand
14、ard No. 79lb.2This test method is being used by some laboratories 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 Do
15、cument Summary page onthe ASTM website.4Available from Energy 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
16、11548. A list of United Kingdom suppliers canbe obtained from 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 mee
17、ting of the responsible technical committee,1whichyou may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 Cooling Bath, consisting of an insulated box with 30 65-mm (1.2 6 0.2-in.) holes in the center to accommodate anydes
18、ired 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 is shown in Fig. 2.5.3 Pipet, or equivalent dispensing device
19、 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 and pressure required togive an even flow of filtrate. Eithe
20、r 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 stopper grooved at the sides to permit theescape of excess air.
21、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 of mercury by spattering. The airpressure regulatory is conn
22、ected 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 for IP Standard Thermometers.Thermometer NumberTemperature Ran
23、ge 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 mercury-in-glass thermometers.5.7 Weighing Bottles, glass-stoppered
24、, 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 evaporation flask. Construct the jets with an insidediameter of 4 6
25、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 to 3 L/min per jet. One way to purify the air is by passageth
26、rough 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 the residue does not exceed 0.1 mg, the evaporationequipment
27、 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 the clean dry filter stickwhich has previously been cooled by p
28、lacing 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 together with the glassstopper to the nearest 0.1 mg, under th
29、e 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 ethyl ketone, wipe dryon the outside with a cloth, and place in
30、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 stopperhave been dried in the evaporation assembly, lift onl
31、y 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 permit the liquid to drain backslowly from the delivery nozzle. Re
32、move 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 maintained at 35 6 1C (95 62F), with the air jet centered inside the
33、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 nearest 0.1 mg. Repeat theevaporation procedure, using a 5-min e
34、vaporation 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, g,B = weight of wax sample, g,C = weight of solvent, g, obt
35、ained 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 plus filtrate (8.5),and0.15 = average factor correcting for
36、the solubility of wax inthe solvent at 32C (25F).10. Report10.1 Report the result as oil content, Test Method D721. Ifthe result is negative, report as zero.11. Precision and Bias11.1 PrecisionThe precision of this test method as deter-mined by statistical examination of interlaboratory results is a
37、sfollows: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 operation ofthe test method, exceed the following values only in
38、 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 the normal and correct operation of the testmethod, exceed th
39、e 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 wax; waxAll dimensions are in millimetresFIG. 3 Air Pressure R
40、egulatorD721 06 (2011)4All dimensions are in millimetres (inches)FIG. 4 Evaporation AssemblyD721 06 (2011)5APPENDIX(Nonmandatory Information)X1. TEST METHOD FOR MEASUREMENT OF MAXIMUM PORE DIAMETER OF RIGID POROUS FILTERSX1.1 ScopeX1.1.1 This test method covers the determination of theacceptability
41、of porous filter sticks used for filtration in TestMethod D721. 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 diameterthe diameter in microm-eters of the largest open
42、ing 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. Because of the irregularity in shape and otherphen
43、omena 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 Summary of Test MethodX1.3.1 The filter is cleaned
44、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 pressure.X1.4 ApparatusX1.4.1 Pressure Measuring De
45、vice, 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 sticks by soaking in concentratedhydrochloric a
46、cid, 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. X1.1.Apply pressure slowly from a source of c
47、lean 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 mm Hg (orequivalent pressure value if using di
48、fferent 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 pressuremeasuring device when the first bubble
49、 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 SticksD721 06 (2011)6ASTM International takes no position respecting the validity of any patent rights asserted in conne
