1、Designation: D1321 10 (Reapproved 2015)Standard Test Method forNeedle Penetration of Petroleum Waxes1This standard is issued under the fixed designation D1321; 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.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 This test method covers the empirical estim
3、ation 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 fordetermining the penetration of bitumin
4、ous material, Test Method D5.Cone methods applicable to greases and to petrolatum are described inTest Methods D217 and Test Method D937, respectively.1.2 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney and liver dama
5、ge. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional info
6、rmation. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to
7、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 Documents2.1 ASTM Standards:2D5 Test Me
8、thod for Penetration of Bituminous MaterialsD87 Test Method for Melting Point of Petroleum Wax(Cooling Curve)D217 Test Methods for Cone Penetration of LubricatingGreaseD937 Test Method for Cone Penetration of PetrolatumD938 Test Method for Congealing Point of PetroleumWaxes, Including PetrolatumE1 S
9、pecification for ASTM Liquid-in-Glass ThermometersE2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision Liquids3. Terminology3.1 Definitions:3.1.1 penetration, nof petroleum wax, the depth in tenthsof a millimetre to which a standard needle penetrates into thewax under
10、 defined conditions.3.1.1.1 DiscussionAs an example, a penetration 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 speci
11、fied cone or needle undera given force falls into the material.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. Summa
12、ry of Test Method4.1 The sample is heated to at least 17 C (30 F) 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 penetromete
13、r, which applies astandard needle to the sample for 5 s under 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.1This test method is under the jurisdictio
14、n 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 April 1, 2015. Published June 2015. Originallyapproved in 1954. Last previous edition approved in 2010 as D132
15、1 10. DOI:10.1520/D1321-10R15.2For 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.Copyright ASTM International, 1
16、00 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Apparatus6.1 Penetrometer, for applying the standard needle to thesurface of the sample specimen and for measuring the extent ofpenetration at the conclusion of the test. The penetrometer shallbe constructed in suc
17、h 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 Fig. 1 represents a composite drawingillustrating the two available types of instrument, one with anadjustable tab
18、le 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 instrument shall be provided with levelingscrews and a spirit level to maintain the plunger shaft in a truevertical p
19、osition. The indicator scale shall 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
20、 be used.6.3 Needle and PlungerThe needle shall be approximately83 mm in length and conform to the dimensions shown in Fig.2. It shall be symmetrically tapered at one end to a cone whoseangle shall be within the range from 8, 55 min to 9, 25 minover the entire length of the cone. The axis of the con
21、e shall becoincident with the shaft axis within 0.13 mm (0.005 in.)maximum runout (total indicator reading). The tapered sectionof the needle shall be made from fully hardened and temperedstainless steel, Grade 440-C or equal, Rockwell hardness C57to 60. After tapering, the point shall be ground off
22、 to atruncated cone, the smaller base of which shall be from0.14 mm to 0.16 mm in diameter. The truncation shall besquare with the needle axis within 2, and the edge shall besharp and free from burrs. The conical surface and thetruncation shall be finished to a smoothness of 0.2 m (8 in.)(rms). The
23、final weight of the needle shall be 2.5 g 6 0.05 g.The total weight of the plunger shall be 47.5 g 6 0.05 g; aweight of 50 g 6 0.05 g is required for mounting on theplunger.NOTE 2The National Institute of Standards and Technology willmeasure and certify the accuracy of penetration needles in accorda
24、ncewith these permissible variations.6.4 Test Specimen Container, consisting of a brass cylinderopen at both ends, having a 25.4 mm 6 1.6 mm (1 in. 6116 in.) inside diameter, 31.8 mm 6 1.6 mm (114 in. 6116 in.)height, and 3.2 mm 6 1.6 mm (18 in. 6116 in.) wall thickness.To prevent slippage of very h
25、ard wax, a few screw threads orgrooves shall be cut into the center part of the inside wall of thecylinder. The cylinder shall be placed on a base plate of brass,wetted with an equal volume mixture of glycerin and water,when casting a test specimen.6.5 Test Room or Cabinet, capable of being maintain
26、ed at23.9 C 6 2.2 C (75 F 6 4 F).6.6 Water Bath, of at least 10 L capacity, capable of beingmaintained at the test temperature within 60.1 C (60.2 F)(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
27、 shall be possible toimmerse the test specimen in the bath to a depth 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 wat
28、er level to support thespecimen during the penetration by the needle.6.7 Thermometer, for use in the water bath. An ASTMPrecision Thermometer, total immersion, having a range from25 C to 55 C or 77 F to 131 F and conforming to therequirements for Thermometer 64C or 64F as prescribed inSpecification
29、E1 or Thermometer S64C or S64F as prescribedin Specification E2251.6.8 Brass Plate, 63.5 mm 6 1.6 mm by 38 mm 6 1.6 mmby 6.4 mm 6 1.6 mm (212 in. 6116 in. by 112 in.6116 in. by14 in. 6116 in.) for supporting test specimen during prepara-tion of the sample. The specimen support is placed on aninsulat
30、ing material, such as corks or rubber stoppers during thecooling period.FIG. 1 PenetrometerFIG. 2 Standard NeedleD1321 10 (2015)27. Preparation of Test Specimen7.1 Heat the wax sample to at least 17 C (30 F) above itsexpected congealing point or melting point (as determined byTest Method D938 or Tes
31、t 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 C 6 2.2 C (75 F 6 4 F), placethe brass plate on a stable support, such as stoppers or corks,and wet the upper surface of th
32、e plate with a mixture of equalvolumes of glycerin and water. Place the test specimencontainer on the plate and then pour the melted wax into it insuch a way that a convex meniscus is formed. Allow thecontainer and contents to cool in the room at 23.9 C 6 2.2 Cfor 1 h. Then shave any excess wax from
33、 the top of thecontainer and remove the brass plate. Place the smooth waxsurface up. Condition the specimen in the bath at the testtemperature within 0.1 C (0.2 F) for 1 h.NOTE 3Very hard waxes occasionally will shrink away from the wallsof the test specimen container; in such cases, it is permissib
34、le to wedge thespecimen in the container.8. Procedure8.1 Reverse the penetrometer base and place the penetrom-eter head over the edge of the water bath and above theperforated test shelf used for supporting the specimen. It maybe necessary to place a weight on the base of the penetrometerto counterb
35、alance 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 bath may be placed on the penetrometer standprovided the test temperature (within 0.1 C (60.2 F) and the requiredwater ci
36、rculation 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 thermometer specifiedin 6.7. Emergent stem corrections shall be applied when the correctionequals or exceeds 0.05 C (0.1
37、 F). 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 surface that had contacted the brass plateat the top. Make certain that the container or test shelf cannotteeter during
38、 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 any temperature in the rangefrom 25 C to 55 C (77 F to 130 F). Temperatures 25 C, 35 C, 45 C,or 50 C (77 F, 95 F, 113 F
39、, or 122 F) normally are used.8.3 Place a 50 g weight above the penetrometer needle,making a total load of 100 g 6 0.15 g for the needle and allattachments. Observe that the release mechanism does not dragon the shaft and that the indicator on the scale is in the “zero”position. Adjust either the in
40、dicator 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 means of the slow-motion adjustment, bringthe needle tip to just touch the surface of the specim
41、en,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 5.0 s6 0.1 s, timing this interval automatically or with a stop watchgraduated to 0.1 s. Then gently depress
42、 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 circumference at least 3.2 mm(18 in.) from the side of the container. Before each test, wipethe n
43、eedle 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 scale readingfor the four penetrations on the prepared specimen and reportto the nearest penetr
44、ation 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 follows:10.1.1 RepeatabilityThe difference between successiveresults obtained by the same oper
45、ator 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 one casein twenty.Repeatability 5 1.72 100.005 24 x !# (1)where:x = penetration.10.1.2 Reproduc
46、ibilityThe 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 in only one case intwenty.Reproducibility 5 4.81 100.004 42 x !# (2)where:x = penetration.1
47、0.1.3 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 D1321 for mea-suring the needle penetration of petrolatum waxes has no biasbecause the value of the needle penetration can
48、 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 requesting Research Report RR:D02-1205.D1321 10 (2015)3ASTM International takes no position resp
49、ecting the validity of any patent rights 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 time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either
