This standard specifies the method for determining the softening point of rubber antioxidants and vulcanization accelerators using the ring and ball method. This standard is applicable to the determination of the softening point of rubber antioxidants and vulcanization accelerators. GB/T 11409.3-2003 Determination of the softening point of rubber antioxidants and vulcanization accelerators GB/T11409.3-2003 Standard download decompression password: www.bzxz.net

GB/T11409.3—2003
This standard is equivalent to 6.6\softening point in Japanese Industrial Standard JIS K6220:1995 "Test Methods for Rubber Compounds", and is revised from the national standard GB/T11409.3—1989 "Determination Method for Softening Point of Rubber Antioxidants and Vulcanization Accelerators". The main technical differences between this standard and JIS K6220:1995 are: glycerin is added to the heat transfer fluid used in the test of this standard in addition to water and silicone oil; the sample ring is slightly different from the JIS K6220:1995 standard. The main technical differences between this standard and GB/T11409.3--1989 are: silicone oil and water are added to the heat transfer fluid in addition to glycerin; the heating rate of the heat transfer fluid is increased from "(3±0.5)℃ per minute". Change to \5℃ per minute". This standard was proposed by the former State Bureau of Petroleum and Chemical Industry. From the date of implementation, this standard will replace GB/T11409.3-1989. This standard is under the jurisdiction of the Chemical Additives Sub-Technical Committee of the National Technical Committee for Standardization of Rubber and Rubber Products. The main drafting unit of this standard: Sinopec Nanjing Chemical Plant. The main drafter of this standard: Liang Zhishun.
This standard was first issued on March 27, 1989.89
National Standard of the People's Republic of China
Rubber Anti-aging Agents, Vulcanization Accelerators
Determination of Softening Point
Test method of softening point for rubberantiagers and yulcanizing acceleratorsGB/T11409.3—2003
Replaces GB/T11409.3—1989
Warning: Personnel using this standard should be familiar with formal laboratory operating procedures. This standard does not intend to involve all safety issues that may arise from the use of this standard. It is the responsibility of the user to formulate appropriate safety and health systems and ensure compliance with national regulations. 1 Scope
This standard specifies the method for determining the softening point of rubber antioxidants and vulcanization accelerators using the ring and ball method. This standard is applicable to the determination of the softening point of rubber antioxidants and vulcanization accelerators. 2 Method Summary
Place a steel ball of specified mass on a sample ring filled with a sample, heat this assembly at a constant heating rate, and the temperature when the sample softens and falls to a specified distance together under the action of the steel ball's gravity is the softening point of the sample. Instruments and Reagents
3.1 Softening Point Determination Apparatus (see Figure 1).
3.1.1 Sample Ring: A ring made of brass or stainless steel, with a shape and size See Figure 2. 3.1.2 Steel ball: a steel ball with a diameter of 9.53 mm and a mass of 3.5 g ± 0.05 g. 3.1.3 Steel ball positioner: made of metal, so that the steel ball is located in the center of the sample. 3.2 Thermometer: a full immersion or partial immersion thermometer with a length of about 300 mm and a graduation value of 0.5 °C. 3.3 Electric furnace and voltage regulator.
3.4 ​​Porcelain plate or glass plate.
3.5 Evaporator with handle: 50 ml,.
3.6 Flat knife.
3.7 Heat transfer fluid: silicone oil, water or glycerin.
Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on January 10, 200390
Implemented on July 1, 2003
4 Preparation of test sample
GB/T11409.3—2003
1—Thermometer; 2—Steel ball positioner; 3—Test sample ring; 4—Bottom plate; 5—Spacer tube; 6—Test sample ring support plate; 7—Steel ballFigure 1 Softening point tester
$20. 6±0. 1
$17.5±0.1
+15. 9±0. 1
+19.0±0.1
Figure 2 Test sample ring
4.1 Place the test sample ring on a porcelain plate or glass plate coated with an oil film. 4.2 Take about 10g of the sample, place it in a handle evaporator, heat and melt it on an electric furnace with a voltage regulator, and stir the sample continuously during heating to prevent local overheating. The heating temperature shall not be higher than the estimated softening point of the sample by about 40℃. Pour the sample into the sample ring until the surface of the sample is slightly higher than the ring surface.
4.3 After the sample is cooled at room temperature for 30 minutes, use a hot knife to scrape off the part of the sample that is higher than the ring surface so that the sample surface is flush with the ring surface. 91
5 Determination steps
GB/T 11409.3--2003
5.1 Place the sample ring containing the sample horizontally in the round hole of the support plate, put on the steel ball positioner, place the steel ball on the sample, and place the sample rack in the heating bath containing the heat transfer liquid. The temperature of the heating liquid is about 50℃ lower than the estimated softening point of the sample, and it is maintained for 10min to 15min. The surface of the heat transfer liquid bath is slightly lower than the depth mark on the connecting rod, and there shall be no bubbles in any part of the sample ring. Insert the thermometer vertically through the center hole of the upper support plate so that the bottom of the mercury ball of the thermometer is at the same horizontal position as the bottom of the ring. 5.2 Place the heating bath on an electric furnace to heat the heat transfer liquid so that the temperature rise rate is maintained at 5°C per minute. 5.3 The sample is softened by heat. Under the action of the gravity of the steel ball, the temperature at which the sample and the steel ball fall together and contact the bottom plate surface is the softening point of the sample. bzxZ.net
If a full immersion thermometer is used, the observed value should be corrected according to the following formula: T = t + 0.000 16 h (ti — ta) Where: T—softening point of the sample, °C; t—-temperature indicated by the thermometer, °C;
temperature of the air around the middle of the mercury ball exposed to the liquid surface (indicated by the auxiliary thermometer), C; t
h——the height of the mercury column exposed to the liquid surface, expressed in degrees of the thermometer; 0.00016---the apparent volume expansion coefficient of mercury. 92
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