1、Designation: D1321 16aStandard 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 p
2、arentheses 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. Scope*1.1 This test method covers the empirical estimation of thecons
3、istency 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 bituminous material, Te
4、st 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 damage. Mercury, ori
5、ts 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 information. Users s
6、hould 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.1.3.1 ExceptionThe values given in parentheses are forinformation only.1.4 This standard does not purport to ad
7、dress 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 Meth
8、od 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 Spe
9、cification 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 d
10、efined 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 specifi
11、ed 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. Summary
12、 of Test Method4.1 The sample is heated to at least 17 C (30 F) above itsexpected congealing point or melting point, poured into a1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.1
13、0.0A on Physical/Chemical Properties.Current edition approved July 1, 2016. Published July 2016. Originally approvedin 1954. Last previous edition approved in 2016 as D1321 16. DOI: 10.1520/D1321-16A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servic
14、e at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29
15、59. United States1container, 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 under a load of 100 g.5. Significance and Use5.1 Petroleum
16、 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 and for measuring the extent ofpenetration at the conclu
17、sion 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 Fig. 1 represents a composite drawingillustrating the
18、 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 instrument shall be provided with levelingscrews and a s
19、pirit level to maintain the plunger shaft 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
20、. Alternatively,a stop watch graduated in 0.1 s intervals may 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,
21、25 minover the entire length of the cone. The axis of the cone 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 har
22、dness C57to 60. After tapering, the point shall be ground off 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
23、shall be finished to a smoothness of 0.2 m (8 in.)(rms). The 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 willmeasu
24、re and certify the accuracy of penetration needles in accordancewith 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 (
25、18 in. 6116 in.) wall thickness.To prevent slippage of very hard 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
26、 specimen.6.5 Test Room or Cabinet, capable of being maintained 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 5). The water bath should be made of glass or othersuitable transparent material, or
27、 have a window to permit ahorizontal view of the specimen. It 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 equippe
28、d with a rigid perforated testshelf about 51 mm below the water 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 theFIG. 1 Pe
29、netrometer FIG. 2 Standard NeedleD1321 16a2requirements for Thermometer 64C or 64F as prescribed inSpecification E1 or Thermometer S64C or S64F as prescribedin Specification E2251.6.7.1 Thermometric devices such as resistance temperaturedetectors (RTDs), thermistors, or other liquid-in-glass ther-mo
30、meters of equal or better accuracy, and covering theappropriate temperature range, may be used.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 su
31、pport is placed on aninsulating material, such as corks or rubber stoppers during thecooling period.7. 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 Test Method D87, respectively),
32、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.Place the test specimen container on the plate and then pour
33、 themelted wax into it in such a way that a convex meniscus isformed. Allow the container and contents to cool in the roomat 23.9 C 6 2.2 C for 1 h. After 1 h of cooling, shave anyexcess wax from the top of the container and remove the brassplate. Place the smooth wax surface up. Condition the speci
34、-men in the bath at the test temperature 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 permissible to wedge thespecimen in the container.NOTE 4The sample temperature prior to pouring into the testspe
35、cimen container can impact the wax tunneling severity. For goodpractice, it is suggested that sample is cooled to 17 C to 20 C above itsmelting point prior to pouring into the test specimen container.8. Procedure8.1 Reverse the penetrometer base and place the penetrom-eter head over the edge of the
36、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 6). Level the penetrometerand the perforated shelf in the water bath.NOTE 5Alternatively, the penetrometer may be place
37、d 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 circulation above and below the test specimen are maintained andprovided further that the temperature of the small bath is measuredimmediately
38、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 F). One of the above alternatives will berequired if the penetrometer is the adjustable table type.8.2 Place the specimen container on the p
39、erforated 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 (1 in.) above the top surface of the specimen andmaintain it at the test tempera
40、ture.NOTE 6The 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, 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
41、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 of theneedle nearly touches the surface of the specimen. S
42、ecurelylock 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 ensuring the bath temperature is within the properspecificati
43、ons, 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 the indicator shaft untilit is stopped by the needle shaft and read the penetration fromthe indicator scale.8.5 Make four tests at points ab
44、out 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, position the needle as described in8.4, and proceed with
45、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 and Bias310.1 The precision of this test method as deter
46、mined 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 materialwould, in the long run, in the normal and correct o
47、peration ofthe test method, exceed the following values in only one casein twenty.25 C Repeatability 5 1.72 100.005 24 x !# (1)40 C Repeatability 5 0.09905x !1.1175(2)where:x = penetration.10.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators
48、work-ing in different laboratories on identical test material would, inthe long run, exceed the following values in only one case intwenty.3Supporting data at 25 C and 40 C have been filed at ASTM InternationalHeadquarters and may be obtained by requesting Research Report RR:D02-1205(25 C) and Resea
49、rch Report RR:D02-1835 (40 C).D1321 16a325 C Reproducibility 5 4.81 100.004 42 x !# (3)40 C Reproducibility 5 0.1746x !1.1175(4)where:x = penetration.10.1.3 The repeatability and reproducibility, calculated fromthe above equations for selected penetration values are shownin 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 be defined onlyin terms of a test method.1
