GB/T 3780.6-1998 Test method for tinting strength of carbon black for rubber
Some standard content:
GB/T 3780.6-1998
This standard is the test method standard for carbon black products for rubber. It is revised from GB/3780.6-1991 according to the American Society for Testing and Materials standard ASTMD3265-96. This standard is equivalent to ASTM D3265-96.
The main difference between this standard and ASTM D3265-96 is that ASTM D3265 stipulates that only one sample ink slurry should be prepared, while this standard stipulates that two sample ink slurries should be prepared and the average value should be taken. ASTM D3265 stipulates three methods for preparing ink slurries: coating film method, roller dispersion film method and glass slide film method. According to the actual situation in my country, this standard adopts the corrugated glass slide film method and coating film method. The main differences between this standard and GB/T3780.6-1991 are as follows: on the basis of the original glass slide film method, the polyester film method is added, and the glass slide film method is specified as the arbitration method. The repeatability is revised from 1.3 to 2.3. The reproducibility is revised from 3.3 to 4.2. In Appendix A, the standard carbon black is revised from A, BC, D, and SRB to A., B, CD, E, F. and SRB2, and the tinting strength value is also changed.
This standard replaces GB/T 3780.6-1991 from the date of implementation. Appendix A of this standard is the appendix of the standard. This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Carbon Black Sub-Technical Committee of the National Rubber and Rubber Products Standardization Technical Committee. The drafting unit of this standard: China Carbon Black Industry Research and Design Institute of the Ministry of Chemical Industry. The main drafters of this standard: Biti, Wang Dingyou, Kai Bi. This standard was first issued in June 1983 and first subscribed in January 1991. National Standard of the People's Republic of China
Test method for tinting strength of carbon black used in rubher products
Carbon black used in rubher products'Tiniing strength test methodGB/T 3780.61998
Replaced by GR/T 3780.61991
The tinting strength of carbon black mainly depends on the size of carbon black particles and is also related to the structure of carbon black and the size distribution of the polymer. Therefore, it can be used to characterize the particle size and distribution of different carbon black particles. 1 Scope
This standard specifies the test method for measuring the tinting strength of carbon black using a reflectometer with industrial coloring reference carbon black ITRB as the benchmark. This standard is applicable to all types of carbon black used in rubber. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in the technical specification. When this standard is issued, the versions shown are all valid. All standards will be revised. Parties using this standard should explore the possibility of using the latest versions of the following standards. GB3778--1994 Carbon for Rubber
GB8170~198? Numerical Rounding Rules
3 Method Summary
White powder (ZnO) and liquid plasticizer (cyclohexane oil) are mixed with industrial coloring reference carbon black and sample carbon black respectively, and the ink slurry is ground and smoothed into a thick and flat film. The reflectivity of the two ink slurries is measured by a suitable photoelectric reflectometer, and the tinting strength of the sample carbon black is calculated by the ratio of the H reflectivity.
4 Reagents
4.1 Plasticizer: Cyclic soybean oil o-0.920.99g/cm% 4.2 Solvent: No. 100 solvent gasoline, ethanol or acetone. 4.3 Oxidizing agent: analytically pure,
4.4 Industrial color reference carbon black ITRB.
4.5 Standard reference carbon black (see Appendix A). 5 Instruments and materials
Conventional laboratory instruments and equipment
5.1 Analytical flat plate with an accuracy of 0.1 mg
5.2 Automatic half-plate grinder,
5.3 Photoelectric reflectometer, which can measure the difference in the immersion rate between gray gradients. 5.4 Ink knife, conical, 100~150mm long, 5.5 Syringe 510.02)cn.
Approved by the State Administration of Quality and Technical Supervision on November 4, 1998 and implemented on June 1, 1999
GB/T 3780. 6—1998
5.6 Glass plate: 750mm×500mm×10mm. 5.7 Thin soft paper: hygroscopic, lint-free.
5.8 Ink slurry sampler
5.8-1 Glass slide film making method
5.8.1.1 Optical glass slide: 75 mm× 50 mm×(1.22±0.05) mm. 5.8.1.2 Separation rod: g6 mm, length 230 mm. 5.8.1.3 Slide sample preparation solution (as shown in Figure 1).
1.5 A pair of copper strips with a thickness of 0.5 mm are pasted on the glass plate. 2.3, 6, 8—Glass slide 1—Ink slurry; 7 Glass plate Slide sampler
5.8-2 Coating film making method
5.8.2.1 Coating film making device: groove depth 0.10 mm 5.8.2.2 Glass plate: 250 mm×80 mmX5 mm. 6 Test conditions
The test is carried out at room temperature (23.2)℃, relative humidity (5015) or room temperature (27±2)℃, relative humidity (65+5)%. 7 Test steps
7.1 Take appropriate amount of zinc oxide, ITRB and carbon black sample and place them in an oven at (125+2)℃ and burn for 1 hour. Move them to a flammable device and cool to room temperature. Note: Zinc oxide, ITRB and carbon black samples should be dried under the same conditions. 7.2 Accurately weigh two portions of 0.1000g carbon black sample, ITRB and corresponding portions of 3.7500g zinc oxide. Note: For N500, N690 and V700 series, weigh 0.2000g zinc oxide per portion, or 3.7500g. Divide the test result by 2. 7.3 Use a syringe to suck 2.20cm of epoxidized blood oil at the center of the lower plate of the grinder. Note: If 2.20 cm of epoxidized soybean oil is used, the flow of the slurry is easy to control, and 2.00 cm is allowed. 7.4 Place ammonium sulfide and carbon black in the center of the epoxidized oil, mix them thoroughly with a blender knife, and move the ink adhering to the blender knife to the upper plate of the grinder to minimize the loss of slurry. 7.5 Close the 1: plate of the grinder, adjust the pressure to 0.017 MPa, and start grinding for 25 turns. 7.6 Stop the machine, beat the flat drum, and use the ink blender knife to move the ink adhering to the flat plate to the center of the lower plate. Collect the whole static slurry and move it to the center of the lower plate. As the lower plate moves slightly, the ink slurry expands into a flat ring. Continue grinding for 25 turns. Repeat this three times for a total of 100 turns. 7.7 Place the slurry on a smooth, clean glass plate or sulfuric acid paper. Instructions for use:
17ASTMD3265 stipulates that only one sample slurry should be prepared. GB/T3780.61998
7.8 Prepare another sample carbon black ink slurry and industrial coloring reference carbon black ink slurry according to the above procedure. 7.9 Clean the grinding machine plate with solvent and soft paper, and prepare the accumulated slurry film by any of the following methods alone! 7.10.1 Glass slide film preparation method (referee method) 7.10.1.1 Take a small amount of slurry on a clean optical glass slide (5.8.1.1) with ink. 7.10.1.2 Put one end of the slide with the slurry on the sample preparation device (5.8.1.3) (see Figure 1): Use a glass rod horizontally mounted on a steel bar to pull it parallel to the open end and the closed end for 1-2 times to make it evenly distributed on the slide. Prepare a slurry film with a width of 50 mm and a thickness of 0.5 mm. Place the slide on a porcelain plate for later use.
7.10.2 Coating film method
7.10.2.1 Wipe the glass plate with a thin soft paper (5.8.2.2). 7.10.2.2 Use a knife to put some ink slurry on the top of the glass plate. Use a coating film applicator (5.8.2.1) to properly and steadily press (2~3)5 to scrape the slurry from the top to the bottom to form a slurry film. 7.10.2-3 Use ink applicator to take a small amount and put it on the starting end of the slurry film. It is not necessary to remove the ink slurry on the newly attached film applicator. Return the film applicator to the starting end of the slurry film: repeat 7.10.2.2--times 7.10.2.4 The width of the slurry film is about 50 mm, and the surface is uniform and smooth. Otherwise, use ink adjustment pad to collect the ink slurry: re-prepare according to the provisions of 7.10.2.1~7.10.2.3. 7.11 Determination of reflectivity of carbon black ink
7.11.1 Glass slide film method
7.11.1.1 Adjust the reflectometer according to the instrument manual. Without the color filter, put the reflective head on the back of the industrial color reference carbon black ink slurry slide, turn on the measurement switch, rotate the correction switch to adjust the reflectivity to 80 scale - measure the reflectivity of different parts of the middle of the slide. Generally, read the reading after stabilization (15~30)s. 7.11.1-2 If the reflectivity measured at four different locations is between 79.5 and 80.5, it means that the requirements are met. At the same time, measure the reflectivity of another portion of ITRB slurry.
7.11.1.3 If the reflectivity of the two portions of ITRB slurry is between 79.5 and 80.5, use a blending knife to mix the two portions of ink slurry evenly, and then repeat the operation according to the requirements of 7.11.1.1 to 7.11.1.2. 7.11.1.4 If both portions of slurry do not meet the requirements, prepare another portion of accumulated slurry according to the requirements of 7.10.1, measure its reflectivity according to the requirements of 7.11.1.1 to 7.11.1.2, and then select two portions that meet the requirements from the three portions of slurry, and repeat the operation according to the requirements of 7.11.1.3. 7.11.1.5 Turn off the test switch, remove the carbon black slurry cut sheet, place the carbon black slurry carrier to be tested, turn on the test switch, measure the reflectivity of four different parts of the slurry carrier, and measure the reflectivity of one sample at the same time, record each reading, and take the average value.
7.11.2 Coating film method
7.11.2.1 Place one ITRI ink slurry under the reflectivity head. Make the slurry face the light hole of the reflectometer. Ignore the wall slurry within 20 μm from the top of the slurry film.
7.11.2.2 After adjusting (15-20) seconds, use the positive switch to adjust the reflectivity value to 80, then measure the reflectivity of four different parts, and record each reading. If the four readings are between 7.5 and 8.5, it can be considered to meet the requirements. At the same time, measure the reflectivity of another ITRI ink slurry. 7.11.2.3 If the reflectivity of the two 1TRB slurries is between 79.5 and 80.5, the two slurries can be mixed evenly with an ink mixer, and then the operation is repeated according to the requirements of 7.11.2.1 to 7.11.2.2. 7.11.2.4 If the two slurries do not meet the requirements, another slurry must be prepared according to the requirements of 7-10.2, and its reflectivity must be determined according to the requirements of 7.11.2.1 to 7.11.2.2. Then, two slurries that meet the requirements are selected from the three slurries, and the operation is repeated according to 7.11.2.3. 7.11.2.5 Place a sample slurry under the reflection head of the reflectometer, so that the slurry faces the light hole of the reflectometer. 20 mm from the top of the slurry film. Note: 1-ASTM133265 specifies two methods for preparing slurries, namely, the layer film method, the roller dispersion method, and the glass slide film method. The paste inside shall not be considered.
GB/T 3780. 6—1998
7. 11.2. 6 After positioning (15~201)s, measure the reflectivity of four different parts and measure the reflectivity of another sample at the same time. Record each reading. Take the average value and
8 Calibration of the instrument
8. 1 According to the procedure of 7.10. 1 or 7.10.2, prepare duplicates of five standard pastes for calibration of color strength according to the quality of ITRB carbon black specified in the table below.
Standard ink paste tinting strength value,
8.2 According to the steps of 7.11.1 or 7.11.2, measure the color strength and take the average value of the duplicate test results. 8.3 The difference between the measured value of the standard slurry and its corresponding standard value should be within ±0.8, otherwise the least square method should be used to calculate the standard value by comparing the measured value to the standard value: Plot the measured value against the standard value. 8.4 The sample carbon black data should be calibrated by equation 1 or calculated from the graph. 8.5 If necessary, the standard reference carbon black can be used for calibration. 9 Result expression
Color intensity T (expressed as a percentage) is calculated according to equation (1): $×100
Formula rft: R ---ITRB reflectivity of instrument slurry; reflectivity of sample ink slurry.
The calculated result should have one more significant digit than that specified in GB 3778, and the long average value should be taken. Then the numerical value should be rounded off according to GB 817. 10 Precision
10.1 Repeatability: The difference between two test results in one experiment is less than 2.0%, 10.2 Reproducibility: The difference between two test results in different laboratories is less than 4.2%. 11 Test report
The test report shall include the following contents:
a) Sample identification number and place of origin;wwW.bzxz.Net
h) Name or number of the standard on which this test is based:
l) Test results;
|) Any abnormalities in the test.
Standard close ratio carbon black
Coloring strength value
(N326)
110. 5±1.5
GB/T3780.6—1998
Appendix A
(Standard Appendix)
Standard reference carbon black coloring strength standard value
(N330)
98. 5-1. 5
(N121)
119.511.5
(N762)
41.2-.1.5
55.2±1. 5
(N683)
$5. 8= 1. 5
(N330)
102.5±1.55 If necessary, the standard reference carbon black can be used for calibration. 9 Result expression
Color intensity T (expressed as a percentage) is calculated according to formula (1): $×100
Formula rft: R---ITRB reflectivity of the instrument slurry; reflectivity of the sample ink slurry.
The calculated result is one more significant digit than that specified in GB 3778, and the long average is taken. Then the numerical value is rounded according to GB 817. 10 Precision
10.1 Repeatability: The difference between two test results in the same experiment is less than 2.0%, 10.2 Reproducibility: The difference between two test results in different laboratories is less than 4.2%. 11 Test report
The test report includes the following contents:
a) Sample identification number and place of origin;
h) The name or number of the standard based on which this test is conducted:
l) Test results;
) Test abnormality.
Standard close ratio carbon black
Coloring strength value
(N326)
110. 5±1.5
GB/T3780.6—1998
Appendix A
(Standard Appendix)
Standard reference carbon black coloring strength standard value
(N330)
98. 5-1. 5
(N121)
119.511.5
(N762)
41.2-.1.5
55.2±1. 5
(N683)
$5. 8= 1. 5
(N330)
102.5±1.55 If necessary, the standard reference carbon black can be used for calibration. 9 Result expression
Color intensity T (expressed as a percentage) is calculated according to formula (1): $×100
Formula rft: R---ITRB reflectivity of the instrument slurry; reflectivity of the sample ink slurry.
The calculated result is one more significant digit than that specified in GB 3778, and the long average is taken. Then the numerical value is rounded according to GB 817. 10 Precision
10.1 Repeatability: The difference between two test results in the same experiment is less than 2.0%, 10.2 Reproducibility: The difference between two test results in different laboratories is less than 4.2%. 11 Test report
The test report includes the following contents:
a) Sample identification number and place of origin;
h) The name or number of the standard based on which this test is conducted:
l) Test results;
) Test abnormality.
Standard close ratio carbon black
Coloring strength value
(N326)
110. 5±1.5
GB/T3780.6—1998
Appendix A
(Standard Appendix)
Standard reference carbon black coloring strength standard value
(N330)
98. 5-1. 5
(N121)
119.511.5
(N762)
41.2-.1.5
55.2±1. 5
(N683)
$5. 8= 1. 5
(N330)
102.5±1.5
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