1、Designation: D1321 10Standard 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 revision. A number in pa
2、rentheses 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. Scope*1.1 This test method covers the empirical estimation of theconsistenc
3、y 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 penetration of bituminous material, Test M
4、ethod D5. Conemethods applicable to greases and to petrolatum are described in TestMethods 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 damage. Mercury, orits v
5、apor, 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 information. Users shoul
6、d 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 address all of thesa
7、fety 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 Method for Penetration
8、 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 Specification for AST
9、M 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 defined conditions.
10、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 specified cone or needle
11、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. Summary of Test Method4.1
12、 The sample is heated to at least 17C (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 astan
13、dard 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 jurisdiction of ASTM Committee D0
14、2 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10.0A on Physical/Chemical Properties.Current edition approved May 1, 2010. Published June 2010. Originallyapproved in 1954. Last previous edition approved in 2004 as D132104. DOI:10.1520/D1321-10.2For referenc
15、ed 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.1*A Summary of Changes section appears at the end of this standard.Copyrig
16、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. 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 sh
17、allbe 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 Fig. 1 represents a composite drawingillustrating the two available types of instrument, o
18、ne 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 instrument shall be provided with levelingscrews and a spirit level to maintain the plunger s
19、haft in a truevertical position. 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 graduate
20、d in 0.1-s intervals may be used.6.3 Needle and PlungerThe 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
21、 cone. The axis of the coneshall be coincident with the shaft 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, th
22、e point shall be groundoff to a truncated cone, the smaller 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
23、0.2 m (8 in.) (rms). The finalweight of the needle shall 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
24、 needles in accordancewith these permissible variations.6.4 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
25、 wax, a few screw threads or grooves shall be cut intothe 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
26、at23.9 6 2.2C (75 6 4F).6.6 Water Bath, of at least 10-L 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 p
27、ossible 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 water level to
28、 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 to 55C or 77 to 131F and conforming to the requirementsfor Thermometer 64C or 64F as prescribed in Specification E1or Thermometer
29、 S64C or S64F as prescribed in SpecificationE2251.6.8 Brass Plate, 63.5 6 1.6 mm by 38 6 1.6 mm by 6.4 61.6 mm (212 6116 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 st
30、oppers during the cooling period.7. Preparation of Test Specimen7.1 Heat the wax sample to at least 17C (30F) above itsexpected congealing point or melting point (as determined byTest Method D938 or Test Method D87, respectively), usingcare to prevent local overheating. Make sure the sample isFIG. 1
31、 PenetrometerFIG. 2 Standard NeedleD1321 102homogeneous and free from air bubbles. In the test room orcabinet maintained at 23.9 6 2.2C (75 6 4F), place the brassplate on a stable support, such as stoppers or corks, and wet theupper surface of the plate with a mixture of equal volumes ofglycerin and
32、 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 contentsto 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. Plac
33、e 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 the wallsof the test specimen container; in such cases, it is permissible to wedge thespecimen in the container.8. Procedure8.1 R
34、everse 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 counterbalance the head (Note 5). Level the penetrometerand the pe
35、rforated 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 0.1C (60.2F) and the requiredwater circulation above and below the test specimen are maintained a
36、ndprovided 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 0.05C (0.1F). One of the above alternatives will berequired if the pene
37、trometer 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 testing. Adjust the water level so that it is at least25 mm (
38、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 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 needl
39、e,making a total load of 100 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 indicator assembly or the table,depending upon the type of instrument, until the tip o
40、f 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 specimen,watching the reflection of the needle tip as an aid to accuratesetting.After ensu
41、ring the bath temperature is within the properspecifications, release the needle shaft and hold it free for 5.06 0.1 s, timing 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 f
42、romthe 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 needle carefully toward its point with a clean, dry cloth toremove all adhering wax, po
43、sition 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 penetration reading (see 3.1.1). Also report theactual test temperature used.10. Precision a
44、nd 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 operator with the same apparatusunder constant operating conditions on identical test mate
45、rialwould, 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 ReproducibilityThe difference between two singleand independent results obtained by different o
46、perators 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.10.1.3 The repeatability and reproducibilities for the differ-ent penetration values calc
47、ulated from the above equations areshown in Table 1.3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1205.TABLE 1 Repeatability and Reproducibility Calculated forDifferent Values of PenetrationPenetration, x Repeatability Rep
48、roducibility10 2 520 2 630 2 740 3 750 3 860 4 970 4 1080 5 1190 5 12100 6 13125 8 17150 11 22175 14 29200 19 37D1321 10310.2 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 be defined onlyin
49、terms of a test method.11. Keywords11.1 hardness; needle penetration; penetration; petroleumwaxSUMMARY OF CHANGESSubcommittee D02.10 has identified the location of selected changes to this standard since the last issue(D132104) that may impact the use of this standard.(1) Added Specification E2251.(2) Revised 6.7.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determ
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