1、Designation: D1321 10 (Reapproved 2015)D1321 16Standard 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 las
2、t 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 U.S. Department of Defense.1. Scope Scope*1.1 This test method covers the
3、empirical estimation of the consistency of waxes derived from petroleum by measurement ofthe extent of penetration of a standard needle. This test method is applicable to waxes having a penetration of not greater than 250.NOTE 1This test method is similar to the needle method for determining the pen
4、etration of bituminous material, Test Method D5. Cone methodsapplicable to greases and to petrolatum are described in Test Methods D217 and Test Method D937, respectively.1.2 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause centralnervous system,
5、kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.h
6、tmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into your state or country may be prohibited by law.1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.3.1 Exceptio
7、nThe values given in parentheses are for information only.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicabili
8、ty of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D5 Test Method for Penetration of Bituminous MaterialsD87 Test Method for Melting Point of Petroleum Wax (Cooling Curve)D217 Test Methods for Cone Penetration of Lubricating GreaseD937 Test Method for Cone Penetratio
9、n of PetrolatumD938 Test Method for Congealing Point of Petroleum Waxes, Including PetrolatumE1 Specification for ASTM Liquid-in-Glass ThermometersE2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids3. Terminology3.1 Definitions:3.1.1 penetration, nof petroleum
10、 wax, the depth in tenths of a millimetre to which a standard needle penetrates into the waxunder defined conditions.3.1.1.1 DiscussionAs an example, a penetration reading of 85 from the indicator scale corresponds to a penetration depth of 8.5 mm.1 This test method is under the jurisdiction ofASTM
11、Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.10.0A on Physical/Chemical Properties.Current edition approved April 1, 2015June 1, 2016. Published June 2015July 2016. Originally approved in 1954. Last previous edition approved in
12、 20102015 asD1321 10.D1321 10 (2015). DOI: 10.1520/D1321-10R15.10.1520/D1321-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page o
13、n the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that user
14、s consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoh
15、ocken, PA 19428-2959. United States13.1.2 penetrometer, nan instrument that measures the consistency or hardness of semiliquid to semisolid materials bymeasuring the depth to which a specified cone or needle under a given force falls into the material.3.1.2.1 DiscussionIn this test method, a standar
16、d penetrometer needle (6.3) is used to determine the hardness of petroleum wax. The penetration forceis determined by the total mass (100 g) of the needle, plunger, and 50 g weight.4. Summary of Test Method4.1 The sample is heated to at least 17 C (30 F) above its expected congealing point or meltin
17、g point, poured into a container,and then air cooled under controlled conditions. The sample then is conditioned at test temperature in a water bath. Penetrationis measured with a penetrometer, which applies a standard needle to the sample for 5 s under a load of 100 g.5. Significance and Use5.1 Pet
18、roleum waxes differ in hardness. Needle penetration is a measurement of hardness. Hardness may have a significanteffect upon other physical properties.6. Apparatus6.1 Penetrometer, for applying the standard needle to the surface of the sample specimen and for measuring the extent ofpenetration at th
19、e conclusion of the test. The penetrometer shall be constructed in such a manner that the accurate placement ofthe tip of the needle at the level surface of the specimen may be made while maintaining a “zero” reading on the indicator. Theapparatus shown in Fig. 1 represents a composite drawing illus
20、trating the two available types of instrument, one with an adjustabletable and the other with an adjustable needle assembly; the use of either type of instrument is permissible. The loaded needle mustfall, when released, without appreciable friction. The instrument shall be provided with leveling sc
21、rews and a spirit level tomaintain the plunger shaft in a true vertical position. The indicator scale shall be calibrated in tenths of a millimetre division andshall have a range of at least 250 tenths of millimetres.6.2 Timing DeviceAn automatic timing release mechanism attached to the penetrometer
22、 may be used. Alternatively, a stopwatch graduated in 0.1 s intervals may be used.6.3 Needle and PlungerThe needle shall be approximately 83 mm in length and conform to the dimensions shown in Fig. 2.It shall be symmetrically tapered at one end to a cone whose angle shall be within the range from 8,
23、 55 min to 9, 25 min overFIG. 1 PenetrometerD1321 162the entire length of the cone. The axis of the cone shall be coincident with the shaft axis within 0.13 mm (0.005 in.) maximumrunout (total indicator reading). The tapered section of the needle shall be made from fully hardened and tempered stainl
24、ess steel,Grade 440-C or equal, Rockwell hardness C57 to 60. After tapering, the point shall be ground off to a truncated cone, the smallerbase of which shall be from 0.14 mm to 0.16 mm in diameter. The truncation shall be square with the needle axis within 2, andthe edge shall be sharp and free fro
25、m burrs. The conical surface and the truncation 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;a weight of 50 g 6 0.05 g is required for mounting on the plunger.NOTE 2The Nation
26、al Institute of Standards and Technology will measure and certify the accuracy of penetration needles in accordance with thesepermissible variations.6.4 Test Specimen Container, consisting of a brass cylinder open at both ends, having a 25.4 mm 6 1.6 mm (1 in. 6 116 in.)inside diameter, 31.8 mm 6 1.
27、6 mm (114 in. 6 116 in.) height, and 3.2 mm 6 1.6 mm (18 in. 6 116 in.) wall thickness. To preventslippage of very hard wax, a few screw threads or grooves shall be cut into the center part of the inside wall of the cylinder. Thecylinder shall be placed on a base plate of brass, wetted with an equal
28、 volume mixture of glycerin and water, when casting a testspecimen.6.5 Test Room or Cabinet, capable of being maintained at 23.9 C 6 2.2 C (75 F 6 4 F).6.6 Water Bath, of at least 10 L capacity, capable of being maintained at the test temperature within 60.1 C (60.2 F) (Note4). The water bath should
29、 be made of glass or other suitable transparent material, or have a window to permit a horizontal viewof the specimen. It shall be possible to immerse the test specimen in the bath to a depth of not less than 102 mm (4 in.) and tosupport it on a perforated conditioning shelf not less than 51 mm (2 i
30、n.) from the bottom of the bath. The bath also shall beequipped with a rigid perforated test shelf about 51 mm below the water level to support the specimen during the penetration bythe needle.6.7 Thermometer, for use in the water bath. An ASTM Precision Thermometer, total immersion, having a range
31、from 25 C to55 C or 77 F to 131 F and conforming to the requirements for Thermometer 64C or 64F as prescribed in Specification E1 orThermometer S64C or S64F as prescribed in Specification E2251.6.7.1 Thermometric devices such as resistance temperature detectors (RTDs), thermistors, or other liquid-i
32、n-glass thermometersof equal or better accuracy, and covering the appropriate temperature range, may be used.6.8 Brass Plate, 63.5 mm 6 1.6 mm by 38 mm 6 1.6 mm by 6.4 mm 6 1.6 mm (212 in. 6 116 in. by 112 in.6 116 in. by 14 in.6 116 in.) for supporting test specimen during preparation of the sample
33、. The specimen support is placed on an insulating material,such as corks or rubber stoppers during the cooling period.7. Preparation of Test Specimen7.1 Heat the wax sample to at least 17 C (30 F) above its expected congealing point or melting point (as determined by TestMethod D938 or Test Method D
34、87, respectively), using care to prevent local overheating. Make sure the sample is homogeneousand free from air bubbles. In the test room or cabinet maintained at 23.9 C 6 2.2 C (75 F 6 4 F), place the brass plate on astable support, such as stoppers or corks, and wet the upper surface of the plate
35、 with a mixture of equal volumes of glycerin andwater. Place the test specimen container on the plate and then pour the melted wax into it in such a way that a convex meniscusis formed. Allow the container and contents to cool in the room at 23.9 C 6 2.2 C for 1 h. Then shave any excess wax from the
36、top of the container and remove the brass plate. Place the smooth wax surface 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 walls of the test specimen container; in such cases, it is permissible
37、 to wedge thespecimen in the container.8. Procedure8.1 Reverse the penetrometer base and place the penetrometer head over the edge of the water bath and above the perforatedtest shelf used for supporting the specimen. It may be necessary to place a weight on the base of the penetrometer to counterba
38、lancethe head (Note 5). Level the penetrometer and the perforated shelf in the water bath.FIG. 2 Standard NeedleD1321 163NOTE 4Alternatively, the penetrometer may be placed in the water bath. Likewise, a small bath may be placed on the penetrometer stand providedthe test temperature (within 0.1 C (6
39、0.2 F) and the required water circulation above and below the test specimen are maintained and provided furtherthat the temperature of the small bath is measured immediately before testing each specimen using the thermometer specified in 6.7. Emergent stemcorrections shall be applied when the correc
40、tion equals or exceeds 0.05 C (0.1 F). One of the above alternatives will be required if the penetrometeris the adjustable table type.8.2 Place the specimen container on the perforated test shelf with the smooth wax surface that had contacted the brass plate atthe top. Make certain that the containe
41、r or test shelf cannot teeter during testing. Adjust the water level so that it is at least 25 mm(1 in.) above the top surface of the specimen and maintain it at the test temperature.NOTE 5The test may be performed at any temperature in the range from 25 C to 55 C (77 F to 130 F). Temperatures 25 C,
42、 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 all attachments.Observe that the release mechanism does not drag on the shaft and that the indicator on the scale is in
43、the “zero” position. Adjusteither the indicator assembly or the table, depending upon the type of instrument, until the tip of the needle nearly touches thesurface of the specimen. Securely lock the movable assembly in this position.8.4 Then, by means of the slow-motion adjustment, bring the needle
44、tip to just touch the surface of the specimen, watching thereflection of the needle tip as an aid to accurate setting. After ensuring the bath temperature is within the proper specifications,release the needle shaft and hold it free for 5.0 s 6 0.1 s, timing this interval automatically or with a sto
45、p watch graduated to 0.1 s.Then gently depress the indicator shaft until it is stopped by the needle shaft and read the penetration from the indicator scale.8.5 Make four tests at points about equally spaced (not less than 12.7 mm (12 in.) apart) on a circumference at least 3.2 mm(18 in.) from the s
46、ide of the container. Before each test, wipe the needle carefully toward its point with a clean, dry cloth to removeall adhering wax, position the needle as described in 8.4, and proceed with the test.9. Report9.1 Record as a single test value the average scale reading for the four penetrations on t
47、he prepared specimen and report to thenearest penetration reading (see 3.1.1). Also report the actual test temperature used.10. Precision and Bias310.1 The precision of this test method as determined by statistical examination of interlaboratory results is as follows:10.1.1 RepeatabilityThe differen
48、ce between successive results obtained by the same operator with the same apparatus underconstant operating conditions on identical test material would, in the long run, in the normal and correct operation of the testmethod, exceed the following values in only one case in twenty.Repeatability51.72 1
49、00.00524 x!# (1)25 C Repeatability51.72 100.00524 x!# (1)40 C Repeatability50.09905x!1.1175 (2)where:where:x = penetration.10.1.2 ReproducibilityThe difference between two single and independent results obtained by different operators working indifferent laboratories on identical test material would, in the long run, exceed the following values in only one case in twenty.3 Supporting data at 25 C and 40 C have been filed atASTM International Headquarters and may be obtained by requesting R
