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This document is developed in accordance with the rules given in GB/T 1.1-2020 Directives for standardization - Part 1: Rules for the structure and drafting of standardizing documents.
This document replaces GB/T 4985-2010 Standard test method for needle penetration of petroleum waxes. In addition to structural adjustments and editorial changes, the following main technical changes have been made with respect to GB/T 4985-2010:
a) The contents of Fischer-Tropsch wax, synthetic wax and bio-wax have been added (see Clause 1);
b) The content of automatic penetrometer has been added (see 5.1.3);
c) The "laboratory or test chamber: capable of being maintained at 23.9°C ± 2.2°C" to "laboratory or test chamber: capable of being maintained at 24.0°C ± 2.0°C" (see 5.5; 5.5 of 2010 edition);
d) The content of reagent has been added (see 5.9);
e) The contents of automatic penetrometer test steps have been added (see 7.2);
f) The contents of quality control have been added (see Clause 9);
g) The repeatability at test temperature of 25°C has been changed (see 10.1.2, 9.1.1 of 2010 edition), the repeatability at 35°C (see 10.1.2) and the repeatability at 40°C have been added (see 10.1.2), the reproducibility at test temperature of 25°C has been changed (see 10.1.3; 9.1.2 of 2010 edition), the reproducibility at 35°C (see 10.1.3) and the reproducibility at 40°C have been added (see 10.1.3);
h) The repeatability and reproducibility for typical penetration in Table 1 have been changed (see Table 1; Table 1 of 2010 edition).
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. The issuing body of this document shall not be held responsible for identifying any or all such patent rights.
This document was proposed by and is under the jurisdiction of the National Technical Committee on Petroleum Products and Lubricants of Standardization Administration of China (SAC/TC 280).
The previous editions of this document and documents replaced by this document are as follows:
——It was first issued as GB 4985-1985 in 1985, first revised in 1998, and second revised in 2010;
——This edition is the third revision.
Standard test method for needle penetration of petroleum waxes
WARNING — Persons using this document shall be familiar with normal laboratory practice. This document may involve certain hazardous materials, equipment and operations, but it does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the users of this document to prepare corresponding safety and protection measures and to determine the applicability of regulatory limitations prior to use.
1 Scope
This document describes a method for evaluating wax hardness by measuring the depth of penetration of a standard needle into a wax specimen.
This document is applicable to petroleum waxes with penetration not greater than 250 1/10 mm, and may also be used to determine Fischer-Tropsch wax, synthetic wax and bio-wax. However, the precision for the determination of synthetic wax and bio-wax is not given in this document.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this standard and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 514-2005 Specification for liquid-in-glass thermometers for testing of petroleum products
GB/T 2539 Petroleum waxes — Determination of melting point-cooling curve method
NB/SH/T 0843 Standard practice for evaluating analytical measurement system performance of petrochemical industry (Statistical techniques)
SH/T 0132 Standard test method for congealing point of petroleum waxes
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
penetration of petroleum wax
depth of vertical penetration of standard needle into wax specimen, in 1/10 mm, under the specified conditions
Note: For example, the dial of the penetrometer shows 85, indicating a penetration of 85 1/10 mm and a penetration depth of 8.5 mm.
3.2
penetrometer
instrument (or device) for determining the consistency or hardness of solid or semi-solid specimens by measuring the depth at which a needle or cone of specified weight penetrates the specimen under the action of specified gravity
4 Principle
The specimen is heated to a minimum temperature of 17°C above the expected congealing point or melting point. The melted wax is poured into a shaper, cooled in air under specified conditions, and controlled at the test temperature in a water bath. The standard needle of the penetrometer is pierced into the specimen for 5 s under 100 g load, and its penetration is measured. The test temperature may be selected from 25°C to 55°C, which is usually 25°C, 35°C, 40°C, 45°C or 55°C.
5 Instruments and reagents
5.1 Penetrometer
5.1.1 Penetrometer: as shown in Figure 1. In this document, the hardness of the wax specimen is measured with a standard needle. The total load, totaling 100 g, includes the standard needle, sliding bars and 50 g weights.
5.1.2 Manual penetrometer: used to bring the standard needle into contact with the surface of the specimen and to measure the depth of penetration of the standard needle into the specimen upon completion of the test. If the indicator reading of manual penetrometer is "zero", the needle tip shall be able to be accurately placed on the surface of wax specimen by adjusting the adjusting device. One of the adjusting devices is an adjustable test bench, and the other is an adjustable needle assembly, either of which is optional. The instrument is equipped with horizontal adjustment screws and a level gauge to ensure that the sliding bar shaft is in a vertical position. The loaded standard needle during being releasing shall fall off without obvious resistance. The indicator shall be calibrated to 1/10 mm with a scale range of no less than 250 1/10 mm.
5.1.3 Automatic penetrometer: used to bring the standard needle into contact with the surface of the specimen. At the beginning of measurement, the penetration time is controlled by an automatic timing device, and the penetration is automatically measured and reported. The unit is 1/10 mm, and the measurement range shall be no less than 250 1/10 mm. The automatic penetrometer is equipped with an adjustable needle assembly, by which the needle tip is able to be accurately placed on the surface of the wax specimen. Horizontal adjustment screws and a level gauges are provided to ensure that the sliding bar shaft is in a vertical position. The loaded standard needle during being releasing shall fall off without obvious resistance. In addition, such penetrometer is equipped with an automatic timing device and an automatic device for measuring the penetration depth of the standard needle into specimens.
Foreword i
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Instruments and reagents
6 Specimen preparation
7 Test procedures
8 Result Report
9 Quality control
10 Precision and deviation
Bibliography
