ASTM D1321-23

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. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D1321 − 16a D1321 − 23
Standard Test Method for
Needle Penetration of Petroleum Waxes
This standard is issued under the fixed designation D1321; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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 the consistency of waxes derived from petroleum by measurement of the
extent of penetration of a standard needle. This test method is applicable to waxes having a penetration of not greater than 250.
NOTE 1—This test method is similar to the needle method for determining the penetration of bituminous material, Test Method D5. Cone methods
applicable to greases and to petrolatum are described in Test Methods D217 and Test Method D937, respectively.
1.2 WARNING—Mercury has been designated by many regulatory agencies as a hazardous materialsubstance that can cause
central nervous system, kidney and liver damage. serious medical issues. Mercury, or its vapor, may has been demonstrated to be
hazardous to health and corrosive to materials. Caution should be taken Use caution when handling mercury and mercury
containing mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s
website—http://www.epa.gov/mercury/faq.htm—for additional information. Users should be aware (SDS) for additional informa-
tion. The potential exists that selling mercury and/or mercury containing products into your state or country may be prohibited by
law.or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their
location.
1.3 The values stated in SI units are to be regarded as the standard.
1.3.1 Exception—The 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 responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D5 Test Method for Penetration of Bituminous Materials
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.10 on Properties of Petroleum Waxes and Alternative Wax-like Materials.
Current edition approved July 1, 2016Dec. 1, 2023. Published July 2016December 2023. Originally approved in 1954. Last previous edition approved in 2016 as
D1321 – 16.D1321 – 16a. DOI: 10.1520/D1321-16A. 10.1520/D1321-23.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*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
D1321 − 23
D87 Test Method for Melting Point of Petroleum Wax (Cooling Curve)
D217 Test Methods for Cone Penetration of Lubricating Grease
D937 Test Method for Cone Penetration of Petrolatum
D938 Test Method for Congealing Point of Petroleum Waxes, Including Petrolatum
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
E1 Specification for ASTM Liquid-in-Glass Thermometers
E2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.1.2 penetration, n—of petroleum wax, the depth in tenths of a millimetre to which a standard needle penetrates into the wax
under defined conditions.
3.1.2.1 Discussion—
As an example, a penetration reading of 85 from the indicator scale corresponds to a penetration depth of 8.5 mm.
3.1.3 penetrometer, n—an instrument that measures the consistency or hardness of semiliquid to semisolid materials by measuring
the depth to which a specified cone or needle under a given force falls into the material.
3.1.3.1 Discussion—
In this test method, a standard penetrometer needle (6.3) is used to determine the hardness of petroleum wax. The penetration force
is determined by the total mass (100 g) of the needle, plunger, and 50 g weight.
4. Summary of Test Method
4.1 The sample is heated to at least 17 °C (30 °F) above its expected congealing point or melting point, poured into a container,
and then air cooled under controlled conditions. The sample then is conditioned at test temperature in a water bath. Penetration
is measured with a penetrometer, which applies a standard needle to the sample for 5 s under a load of 100 g.
5. Significance and Use
5.1 Petroleum waxes differ in hardness. Needle penetration is a measurement of hardness. Hardness may have a significant effect
upon other physical properties.
6. Apparatus
6.1 Penetrometer, for applying the standard needle to the surface of the sample specimen and for measuring the extent of
penetration at the conclusion of the test. The penetrometer shall be constructed in such a manner that the accurate placement of
the tip of the needle at the level surface of the specimen may be made while maintaining a “zero” reading on the indicator. The
apparatus shown in Fig. 1 represents a composite drawing illustrating the two available types of instrument, one with an adjustable
table and the other with an adjustable needle assembly; the use of either type of instrument is permissible. The loaded needle must
fall, when released, without appreciable friction. The instrument shall be provided with leveling screws and a spirit level to
maintain the plunger shaft in a true vertical position. The indicator scale shall be calibrated in tenths of a millimetre division and
shall have a range of at least 250 tenths of millimetres.
6.2 Timing Device—An automatic timing release mechanism attached to the penetrometer may be used. Alternatively, a stop watch
graduated in 0.1 s intervals may be used.
6.3 Needle and Plunger—The 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°, 55 min to 9°, 25 min over the
entire length of the cone. The axis of the cone shall be coincident with the shaft axis within 0.13 mm (0.005 in.) maximum runout
(total indicator reading). The tapered section of the needle shall be made from fully hardened and tempered stainless steel, Grade
440-C or equal, Rockwell hardness C57 to 60. After tapering, the point shall be ground off to a truncated cone, the smaller base
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°, and the
edge shall be sharp and free from burrs. The conical surface and the truncation shall be finished to a smoothness of 0.2 μm (8 μin.)
(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.
D1321 − 23
FIG. 1 Penetrometer
FIG. 2 Standard Needle
NOTE 2—The National Institute of Standards and Technology will measure and certify the accuracy of penetration needles in accordance with these
permissible 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 ⁄16 in.) inside
1 1 1 1
diameter, 31.8 mm 6 1.6 mm (1 ⁄4 in. 6 ⁄16 in.) height, and 3.2 mm 6 1.6 mm ( ⁄8 in. 6 ⁄16 in.) wall thickness. To prevent
slippage of very hard wax, a few screw threads or grooves shall be cut into the center part of the inside wall of the cylinder. 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 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) (Note 5).
The water bath should be made of glass or other suitable transparent material, or have a window to permit a horizontal view of
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 to support
it on a perforated conditioning shelf not less than 51 mm (2 in.) from the bottom of the bath. The bath also shall be equipped with
a rigid perforated test shelf about 51 mm below the water level to support the specimen during the pen
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