1、Designation: D 1321 04An American National StandardStandard Test Method forNeedle Penetration of Petroleum Waxes1This standard is issued under the fixed designation D 1321; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o
2、f 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 covers the empir
3、ical estimation of theconsistency of waxes derived from petroleum by measurementof the extent of penetration of a standard needle. This testmethod is applicable to waxes having a penetration of notgreater than 250.NOTE 1This test method is similar to the needle method for deter-mining the penetratio
4、n of bituminous material, Test Method D5. Conemethods applicable to greases and to petrolatum are described in TestMethods D 217 and Test Method D 937, respectively.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This s
5、tandard 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 use.2. Referenced Documents2.
6、1 ASTM Standards:2D 5 Test Method for Penetration of Bituminous MaterialsD 87 Test Method for Melting Point of Petroleum Wax(Cooling Curve)D 217 Test Methods for Cone Penetration of LubricatingGreaseD 937 Test Method for Cone Penetration of PetrolatumD 938 Test Method for Congealing Point of Petrole
7、umWaxes, Including PetrolatumE 1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 penetration, n, of petroleum waxthe depth in tenthsof a millimetre to which a standard needle penetrates into thewax under defined conditions.3.1.1.1 DiscussionAs an example, a pen
8、etration readingof 85 from the indicator scale corresponds to a penetrationdepth of 8.5 mm.3.1.2 penetrometer, nan instrument that measures theconsistency or hardness of semiliquid to semisolid materials bymeasuring the depth to which a specified cone or needle undera given force falls into the mate
9、rial.3.1.2.1 DiscussionIn this test method, a standard pen-etrometer needle (6.3) is used to determine the hardness ofpetroleum wax. The penetration force is determined by thetotal mass (100 g) of the needle, plunger, and 50 g weight.4. Summary of Test Method4.1 The sample is heated to at least 17C
10、(30F) above itsexpected congealing point or melting point, poured into acontainer, and then air cooled under controlled conditions. Thesample then is conditioned at test temperature in a water bath.Penetration is measured with a penetrometer, which applies astandard needle to the sample for 5 s unde
11、r a load of 100 g.5. Significance and Use5.1 Petroleum waxes differ in hardness. Needle penetrationis a measurement of hardness. Hardness may have a significanteffect upon other physical properties.6. Apparatus6.1 Penetrometer, for applying the standard needle to thesurface of the sample specimen an
12、d for measuring the extent ofpenetration at the conclusion of the test. The penetrometer shallbe constructed in such a manner that the accurate placement ofthe tip of the needle at the level surface of the specimen maybe made while maintaining a “zero” reading on the indicator.The apparatus shown in
13、 Fig. 1 represents a composite drawingillustrating the two available types of instrument, one with anadjustable table and the other with an adjustable needleassembly; the use of either type of instrument is permissible.The loaded needle must fall, when released, without appre-ciable friction. The in
14、strument shall be provided with levelingscrews and a spirit level to maintain the plunger shaft in a true1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10 on Properties of Petroleum Wax.Current
15、 edition approved Nov. 1, 2004. Published November 2004. Originallyapproved in 1954. Last previous edition approved in 2002 as D 132102a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume i
16、nformation, refer to the standards Document Summary page onthe ASTM website.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.vertical position. The indicator scale shal
17、l be calibrated intenths of a millimetre division and shall have a range of at least250 tenths of millimetres.6.2 Timing DeviceAn automatic timing release mecha-nism attached to the penetrometer may be used. Alternatively,a stop watch graduated in 0.1-s intervals may be used.6.3 Needle and PlungerTh
18、e needle shall be approxi-mately 83 mm in length and conform to the dimensions shownin Fig. 2. It shall be symmetrically tapered at one end to a conewhose angle shall be within the range from 8, 55 min to 9, 25min over the entire length of the cone. The axis of the coneshall be coincident with the s
19、haft axis within 0.13-mm (0.005-in.) maximum runout (total indicator reading). The taperedsection of the needle shall be made from fully hardened andtempered stainless steel, Grade 440-C or equal, Rockwellhardness C57 to 60. After tapering, the point shall be groundoff to a truncated cone, the small
20、er base of which shall be from0.14 to 0.16 mm in diameter. The truncation shall be squarewith the needle axis within 2, and the edge shall be sharp andfree from burrs. The conical surface and the truncation shall befinished to a smoothness of 0.2 m (8 in.) (rms). The finalweight of the needle shall
21、be 2.5 6 0.05 g. The total weight ofthe plunger shall be 47.5 6 0.05 g; a weight of 50 6 0.05 g isrequired for mounting on the plunger.NOTE 2The National Institute of Standards and Technology willmeasure and certify the accuracy of penetration needles in accordancewith these permissible variations.6
22、.4 Test Specimen Container, consisting of a brass cylinderopen at both ends, having a 25.4 6 1.6-mm (1 6116-in.) insidediameter, 31.8 6 1.6-mm (114 6116-in.) height, and 3.2 61.6-mm (18 6116-in.) wall thickness. To prevent slippage ofvery hard wax, a few screw threads or grooves shall be cut intothe
23、 center part of the inside wall of the cylinder. The cylindershall be placed on a base plate of brass, wetted with an equalvolume mixture of glycerin and water, when casting a testspecimen.6.5 Test Room or Cabinet, capable of being maintained at23.9 6 2.2C (75 6 4F).6.6 Water Bath, of at least 10-L
24、capacity, capable of beingmaintained at the test temperature within 60.1C (60.2F)(Note 4). The water bath should be made of glass or othersuitable transparent material, or have a window to permit ahorizontal view of the specimen. It shall be possible toimmerse the test specimen in the bath to a dept
25、h of not less than102 mm (4 in.) and to support it on a perforated conditioningshelf not less than 51 mm (2 in.) from the bottom of the bath.The bath also shall be equipped with a rigid perforated testshelf about 51 mm below the water level to support thespecimen during the penetration by the needle
26、.6.7 Thermometer, for use in the water bath. An ASTMPrecision Thermometer, total immersion, having a range from25 to 55C or 77 to 131F and conforming to the requirementsfor Thermometer 64C or 64F as prescribed in SpecificationE1.6.8 Brass Plate, 63.5 6 1.6 mm by 38 6 1.6 mm by 6.4 61.6 mm (212 6116
27、in. by 112 6116 in. by14 6116 in.) forsupporting test specimen during preparation of the sample. Thespecimen support is placed on an insulating material, such ascorks or rubber stoppers during the cooling period.7. Preparation of Test Specimen7.1 Heat the wax sample to at least 17C (30F) above itsex
28、pected congealing point or melting point (as determined byTest Method D 938 or Test Method D87, respectively), usingcare to prevent local overheating. Make sure the sample ishomogeneous and free from air bubbles. In the test room orcabinet maintained at 23.9 6 2.2C (75 6 4F), place the brassplate on
29、 a stable support, such as stoppers or corks, and wet theupper surface of the plate with a mixture of equal volumes ofglycerin and water. Place the test specimen container on theplate and then pour the melted wax into it in such a way thata convex meniscus is formed. Allow the container and contents
30、to cool in the room at 23.9 6 2.2C for 1 h. Then shave anyexcess wax from the top of the container and remove the brassplate. Place the smooth wax surface up. Condition the speci-men in the bath at the test temperature within 0.1C (0.2F) for1h.NOTE 3Very hard waxes occasionally will shrink away from
31、 the wallsof the test specimen container; in such cases, it is permissible to wedge thespecimen in the container.FIG. 1 PenetrometerFIG. 2 Standard NeedleD13210428. Procedure8.1 Reverse the penetrometer base and place the penetrom-eter head over the edge of the water bath and above theperforated tes
32、t shelf used for supporting the specimen. It maybe necessary to place a weight on the base of the penetrometerto counterbalance the head (Note 5). Level the penetrometerand the perforated shelf in the water bath.NOTE 4Alternatively, the penetrometer may be placed in the waterbath. Likewise, a small
33、bath may be placed on the penetrometer standprovided the test temperature (within 0.1C (60.2F) and the requiredwater circulation above and below the test specimen are maintained andprovided further that the temperature of the small bath is measuredimmediately before testing each specimen using the t
34、hermometer specifiedin 6.7. Emergent stem corrections shall be applied when the correctionequals or exceeds 0.05C (0.1F). One of the above alternatives will berequired if the penetrometer is the adjustable table type.8.2 Place the specimen container on the perforated test shelfwith the smooth wax su
35、rface that had contacted the brass plateat the top. Make certain that the container or test shelf cannotteeter during testing. Adjust the water level so that it is at least25 mm (1 in.) above the top surface of the specimen andmaintain it at the test temperature.NOTE 5The test may be performed at an
36、y temperature in the rangefrom 25 to 55C (77 to 130F). Temperatures 25, 35, 45, or 50C (77, 95,113, or 122F) normally are used.8.3 Place a 50-g weight above the penetrometer needle,making a total load of 100 6 0.15 g for the needle and allattachments. Observe that the release mechanism does not drag
37、on the shaft and that the indicator on the scale is in the “zero”position. Adjust either the indicator assembly or the table,depending upon the type of instrument, until the tip of theneedle nearly touches the surface of the specimen. Securelylock the movable assembly in this position.8.4 Then, by m
38、eans of the slow-motion adjustment, bringthe needle tip to just touch the surface of the specimen,watching the reflection of the needle tip as an aid to accuratesetting.After ensuring the bath temperature is within the properspecifications, release the needle shaft and hold it free for 5.06 0.1 s, t
39、iming this interval automatically or with a stop watchgraduated to 0.1 s. Then gently depress the indicator shaft untilit is stopped by the needle shaft and read the penetration fromthe indicator scale.8.5 Make four tests at points about equally spaced (not lessthan 12.7 mm (12 in.) apart) on a circ
40、umference at least 3.2 mm(18 in.) from the side of the container. Before each test, wipethe needle carefully toward its point with a clean, dry cloth toremove all adhering wax, position the needle as described in8.4, and proceed with the test.9. Report9.1 Record as a single test value the average sc
41、ale readingfor the four penetrations on the prepared specimen and reportto the nearest penetration reading (see 3.1.1). Also report theactual test temperature used.10. Precision and Bias310.1 The precision of this test method as determined bystatistical examination of interlaboratory results is as f
42、ollows:10.1.1 RepeatabilityThe difference between successiveresults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould, in the long run, in the normal and correct operation ofthe test method, exceed the following values in only on
43、e casein twenty.Repeatability 5 1.72 100.005 24 x!# (1)where:x = penetration.10.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, exceed the following values
44、 in only one case intwenty.Reproducibility 5 4.81 100.004 42 x!# (2)wherex = penetration.10.1.3 The repeatability and reproducibilities for the differ-ent penetration values calculated from the above equations areshown in Table 1.10.2 BiasThe procedure in Test Method D 1321 for mea-suring the needle
45、 penetration of petrolatum waxes has no biasbecause the value of the needle penetration can be defined onlyin terms of a test method.11. Keywords11.1 hardness; needle penetration; penetration; petroleumwax3Supporting data have been filed at ASTM International Headquarters and maybe obtained by reque
46、sting Research Report RR: D02-1205.D1321043SUMMARY OF CHANGESSubcommittee D02.10 has identified the location of selected changes to this standard since the last issue(D 132102a) that may impact the use of this standard.(1) Added Test Method D87to the Referenced Documents.(2) Added a Discussion to 3.
47、1.1.(3) Revised 4.1.(4) Added tolerance limits to the dimensions cited in 6.4 and6.8.(5) Revised 6.8 to permit the use of insulating materials otherthan cork.(6) Revised 7.1, 8.2, 8.4, and 9.1.(7) Deleted former Note 6.ASTM International takes no position respecting the validity of any patent rights
48、 asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any ti
49、me by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on S
