This standard specifies the method for determining the absorption value of carbon black dibutyl phthalate (DBP) using an oil absorptometer. This method is an arbitration method. This standard is applicable to the determination of the absorption value of carbon black dibutyl phthalate (DBP) for rubber. GB/T 3780.2-1994 Determination of the absorption value of carbon black dibutyl phthalate GB/T3780.2-1994 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Determination of dibutylphthalate absorption number of carbon blackGB/T 3780.2-94
Generation 8 378:3
This standard adopts the international standard ISO4656/1:1985 "Carbon black - Determination of dibutylphthalate absorption number Part 1: Oil absorptometer method".
Part I Method A
1 Subject content and scope of application
This standard specifies the method for determining the absorption value of dibutylphthalate (DBP) of carbon black using an absorptometer. This method is an arbitration method. This standard is applicable to the determination of the absorption value of dibutylphthalate (DBP) of carbon black for rubber. 2 Reference standards
GB3778 Carbon black for rubber
GB/T 3780.8 Determination of heating loss of carbon black GB/T10723 Standard method for improving the reproducibility of carbon black test using ASTM standard reference carbon black GB/T15338 Confirmation of precision and deviation of carbon black test method 3 Principle
3.1 The degree of aggregation of carbon black particles affects the performance of carbon black vulcanized rubber. The voids of carbon black aggregates depend on the degree of aggregation of carbon black particles. The pore volume can be obtained from the volume of dibutyl phthalate absorbed by carbon black. Therefore, the absorption value of dibutyl phthalate of carbon black can be used as a measure of the degree of aggregation of carbon black particles. 3.2 Use a constant-speed burette to add dibutyl phthalate to the carbon black sample that is kept in motion by the rotating blade, so that the carbon black changes from a free-flowing powder to a semi-plastic mixture, thereby increasing the viscosity of the mixture and the torque of the rotor. When the torque reaches the preset value inferred from the torque change curve due to this viscosity change, the titration stops. Read the added volume of dibutyl phthalate directly. The volume of dibutyl phthalate absorbed per unit mass of carbon black is the absorption value of dibutyl phthalate of carbon black. 4 Reagents and materials
4. Density of dibutyl phthalate (D)BP) P2s 1.045 1.050 g/cm2. 4.2 Use the standard reference carbon black SRBs in GB/T15338. 5 Instrument
5.1 Carbon black oil absorption meter, including the following components: 5.1.1 Mixing machine.
5. 1. 2 Speed ​​burette; output 4 ± 0. 024 cm2/min. Approved by the State Administration of Technical Supervision on December 22, 1994 and implemented on September 1, 1995
5. 1. 3 Torque adjustment device.
5.1.4 Torque dynamic recorder.
5.2 Constant temperature drying oven: can be controlled at 105 + 2°C. 5.3 Balance: accurate to 0.01g.
5.4 Dryer.
5.5 Scraper.
GB/T3780.2—94
5. 6 Crusher or grinder: can crush granular carbon black. 6 Sampling
6.1 Follow the relevant provisions of GB3778. 7 Preparation of samples
7.1 According to the provisions of GB/T3780.8, dry the specified amount of carbon black sample in a constant temperature drying oven at 105±2C1 for 1 hour, take it out and place it in a desiccator to cool for use.
8 Test conditions
The test is best carried out under the following conditions;
Temperature 23±2℃ and relative humidity 50%±5%, arbitration conditions, a
Temperature 2 7±2℃ and relative humidity 65%±5%; b.
Reagents and instruments should be kept at the experimental temperature and humidity for at least 24h before use. 9 Steps
9.1 Adjust and calibrate the carbon black oil absorption meter and constant rate burette according to Appendix A and B 9.2 Use the standard reference carbon black SRBs in GB/T15338 to calibrate the carbon black oil absorption meter according to the operating steps specified in Articles 9.3 and 9.4 (see Table 1).
Table 13 Standard reference carbon black o-phthalate: medium acid monoester absorption value standard reference carbon black
A-4 N326
B-4N330
C-4N121
D-4 N762
E-4N660
F-4N683
Absorption value of dibutyl ortho-dicarboxylate, 10m/kgcm*/1Hlg）70.8(±0.63)
100. 0(±0. 92)
130. 8(+0. 97)
64. 8(± 0. 8R)
90. 1(±1. 49)
130. 0(+1.27)
Note: The rotor and mixing chamber with high light activity are not suitable for N650, N660, NG83 and N765, produce unstable torque near the end point, and sometimes even fail to reach the burning point. In this case, these carbons are crushed before weighing. 9.2.1 Each standard reference carbon black should be measured enough times to obtain a stable measurement value. If the difference between the two measurement results does not exceed 1,6×10-\m/kg, these two results are regarded as qualified values. Instructions for use:
1IS04656/1 Assuming a temperature of 125±2℃ or 105±2℃. 27 150) 4656/1 Last table 1,
GB/T 3780.2—94
9.2.2 If the measured value is still outside the allowable range after calibration and adjustment, the least square method can be used for regression calculation according to the provisions of GB/T 10723 to regress the measured value to the standard value. Another method is to draw a curve between the measured value and the standard value. The measured value of the tested sample should be calibrated with the above regression equation or curve. 9.2.3 The instrument needs to be calibrated with standard reference carbon black regularly, and a new equation needs to be recalculated or a new curve needs to be drawn if necessary. 9.3 Sample size
9.3.1 According to the carbon black type and sample size listed in Table 2, weigh the dried carbon black sample (accurate to 0.02 g). Table 2 Carbon black type and sample amount Carbon black type N472, N582 N630, N642 and N770 series (except N765) N800 and N900 series Other types of carbon black Test sample Note: Carbon black with high density cannot fill the mixing chamber (5.1.1). More sample can be weighed, which will generate a torque large enough to drive the torque limit switch. 9.4 Determination 9.4.1 Move the sample into the mixing chamber (5.1.1) of the oil absorptometer. 9.4.2 Start the carbon black oil absorption meter, then start the constant speed burette (5.1.2) to add dibutyl phthalate. When the added dibutyl phthalate makes the carbon black sample semi-plastic reach the pre-adjusted torque level, the instrument will automatically shut down. Record the volume of dibutyl phthalate consumed.
If there is no torque adjustment device, use a recorder to record the entire torque curve and calculate the volume of dibutyl phthalate consumed according to 70% of the maximum torque value.
9.4. 3 Remove the mixing chamber and carefully clean the rotor blades and the chamber with a scraper (5.5). Note: The cleaning method can be simplified as follows: Before removing the mixing chamber, add some dry carbon black and run the instrument. At the same time, turn on the "quick down" switch of the automatic burette to fill the burette with butyl phthalate. When the burette is full, the negative black oil absorption meter also stops rotating clockwise, and the mixing chamber can be cleaned at this time. 9.4.4 Reinstall the mixing chamber to measure the next sample. 10 Result expression
10.1 The absorption value of carbon black, monobutyl phthalate, D, is expressed as 10-5m/kg (cm*/100g), and is calculated using formula (1): Mx100
Where: V—. The volume of dibutyl phthalate consumed, cm*M sample amount, &.
The calculation result shall be accurate to 0.1×10-5m/kg. 11 Allowable error 1
The difference between two measurement results shall not exceed 1.6×10-m/kg (1.6×10-5cm/100g). 12 Test report
12.1 The test report shall include the following items: a: National standard number on which this test is based
Adoption instructions:
1 The international standard does not specify the allowable error.
The complete number and origin of the sample;
Weigh the sample amount;
The average value of the two measurement results;
Operation steps not specified in this standard;
Record abnormal phenomena that occur during the test.
13 Subject content and scope of application
GB/T 3780.294
Part II Method B
This standard specifies the manual method for determining the absorption value of carbon black dibutyl phthalate (DBP). This standard is applicable to the determination of the absorption value of carbon black dibutyl phthalate (DBP) for rubber. 14 Referenced Standards
GB3778 Carbon Black for Rubber
GB/T3780.8 Determination of Heating Loss of Carbon Black 15 Summary of Method
15. 1 Add dibutyl phthalate to a certain amount of sample at a certain speed, stir and roll on a glass plate with a glass sample to change the mixture from a free-flowing powder to a semi-plastic object, and the end point is when all the carbon black rolls onto the glass rod and no oil marks appear on the glass plate. 16 Reagents
16.1 Density of dibutyl phthalate (DBP) p251.045~1.050g/cm 17 Instruments
17.1 Microburette: minimum graduation value is 0.02 cm. 17.2 Analytical flat: accurate to 0.001g. 17.3 Glass plate: 170mm×140 mm
17.4 Glass rod: diameter ±7~8 mm
17.5 Constant temperature drying oven: can be controlled at 105±2℃. 17.6 Dryer,
17.7 Stopwatch: accurate to 0.2 s.
18.1 Execute according to the relevant provisions of GB3778. 19 Preparation of the sample
19.1 According to the provisions of GB/T3780.8, dry an appropriate amount of carbon black sample in a constant temperature drying oven at 105±2℃ for 1h, and then cool it in a desiccator for later use.
20 Test conditions
The test is best carried out under the following conditions:
a. Temperature 23±2℃ and relative humidity 50%±5%, arbitration conditions; b. Temperature 271:2℃ and relative humidity 65%±5%CB/T3780.2-..94
Reagents and instruments should be stolen from the laboratory before use. 21 Steps
21.1 Weigh 1.000g (accurate to 0.001g) of the dry sample (19.1), place it on a glass plate (17.3), and start to drop dibutyl phthalate at a faster rate.
21.2 When the amount added is equivalent to two-thirds of the carbon black oil absorption value, use glass (17.4) to gently mix so that dibutyl phthalate and carbon black are evenly infiltrated. Then continue to roll and crush all the granular carbon smoke. 21.3 Continue to add dibutyl phthalate at a slower speed and continue to roll. 21.4 When the mixture of carbon black and dibutyl phthalate appears in different shapes (such as natural gas tank carbon black, high wear-resistant furnace carbon black appears in small strips, semi-reinforced furnace carbon black appears in small blocks, and spray carbon black appears in granules), all the carbon black can be rolled onto the glass rod. At the same time, when no ink marks appear on the glass plate, it is the end point.
21.5 One operation should be completed within 4 to 6 minutes 22 The result is expressed as
The absorption value of dibutyl phthalate of carbon black is expressed as 10=\m/kg (cm/100g), and is calculated by formula (2): D
M×100
-the volume of dibutyl phthalate consumed, cm\, where: V—
M—the amount of sample, g.
The calculation result is accurate to 0.1×10-sm/kg. 23 The allowable difference
The result of two determinations The difference between the results should not exceed 5×105m/kg (cm2/100g). 24 Test report
The test report should include the following items:
The national standard number on which this test is based:
The complete number and origin of the sample:
The average value of the two test results:
Operation steps not specified in this standard;
Record abnormal phenomena that occur during the test.
A1 Equipment
A1. 1 Spring wire: range 0～150 V.
GB/T 3780.2—94
Appendix A
Adjustment and calibration of carbon black oil absorption meter
(Supplement)
A1.2 String: 450 tutn long, with rings at both ends (for type A oil absorption meter). A1.3 Torque shaft positioning gauge (for type A oil absorption meter). A1.4 Stopwatch.
Type A oil absorption meter
A2.1 Inspection
Fix the ring at one end of the string (A1.2) to the nut extending from the back of the differential dynamometer (see Figure A1), and lay the string around the differential dynamometer in a counterclockwise direction.
Put the hook under the spring scale into the ring at the other end of the string (see Figure A1). Torque shaft
Torque shaft
Locking grid
Stop ring
GB/T 3780.2—94
Adjust zero position
Spring type
Position diameter on the nut of the brake medium
Spring scale
Draw the outer chord line on the pulley
Rotate counterclockwise on the
Dynamometer
Support spring fast
Dynamometer connection ring
Figure A1A type oil suction gauge
Put the manual/automatic switch to the "automatic" position, start the oil suction gauge and set the torque limit switch to 5. Apply a constant upward pull on the spring balance until the torque indicator reaches zero and the machine stops. Read the force applied by the spring.
If the force indication is 80-90 N, this preset is appropriate. A2.2 Adjustment of the spring
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If the instrument has been disassembled after leaving the factory, the position of the dynamometer, the coupling ring and the height of the torque shaft should be checked. If necessary, reposition it by placing the positioning gauge (A1.3) between the dynamometer coupling ring and the spring support block. Adjust the dynamometer coupling ring up or down as needed to make it consistent with the positioning gauge size (see Figure A1). Invert the positioning gauge to check the appropriate height of the torque shaft. When checking, place the positioning gauge on the top of the torque shaft GB/T 3780.2-94
and the spring block, as shown in Figure A1. If necessary, loosen the dynamometer coupling ring and the retaining ring, and slide the torque shaft up and down to adjust its height.
If the reading of the spring scale is too high, this indicates excessive friction or improper adjustment of the torque spring. Check the lubrication of the entire system for gear wear, bearing lubrication or hardening of the grease of the gear set. If all these conditions are intact, adjust or replace the spring to make the torque spring adjustment reading 80 N ~ 90 N. A2.3 Adjustment of the buffer tank regulating valve
Check whether the buffer tank is filled with oil that meets the requirements. Adjust the buffer tank regulating valve to the time for the torque detection system to return to its original position is 11:1.1s.
A3B type oil absorption gauge adjustment
A3.1 Inspection
Hook the spring scale on the shaft equipped with an isoelastic spring (see Figure A2). Set the manual/auto switch to the "auto" position, start the oil absorption gauge, and adjust the torque selector to 5. Apply a constant upward pull to the spring balance until the torque indicator reaches the tower position and the instrument stops. Read the force applied by the spring balance. The indicator is set at the indicator number. Scale Figure A2 B-type oil absorption gauge If the indicated force is between 17.7 and 25 N, it meets the requirements. 2 Differential research and often different exemption from early practical medicine research
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Equal elastic paste
Tensile testing machine. Sample
43.2 Adjustment of equal elasticity
GB/T 3780. 2-94
If the reading of the elastic mass balance exceeds the above limits, check for other factors, such as gear wear, improper lubrication, hardening of bearing dry grease, etc., and correct it by adjusting the screw at the bottom of the spring or by moving the balance. A3.3 Adjustment of the buffer bypass valve
Check whether the buffer tank is filled with oil that meets the requirements. Adjust the buffer valve (the black knob behind the oil absorptometer) so that the time to fully return to the original position is 3±0.5s, that is, lift it up by hand and then release it to measure. Note: Other oil absorptometers are calibrated according to the manual of the corresponding instrument. Appendix B
Calibration of constant rate burette
(Supplement)
B1 Overview
B1.1 The constant rate burette is an integral part of the oil absorptometer device. If there is an error in the disk of dibutyl phthalate added to the carbon black by the burette, an incorrect dibutyl phthalate absorption value will result. B2 Reagents
B2.1 Dibutyl phthalate (DBP): density p25 1.045~1.050 g/cm. B3 Apparatus
B3.1 Stopwatch.
B3.2 Beaker: capacity 150 cm.
B3.3 Industrial balance: accurate to 0.01 liter. B3.4 Plastic tube, resistant to swelling by dibutyl phthalate. B4 Pre-calibration checks
B4.1 In the plastic tube (B3.4) or conduit, especially on the nozzle, make sure that no air is accumulated, as sudden accumulation of air can cause errors in the amount of reagent released.
B5 Calibration procedures
B5.1 Check that the O-ring and plastic tube cannot be softened by the reagent and assemble the burette. B5.2 Fill the burette with dibutyl phthalate (B2.1) and place it in the conduit, remove all air from the system, and then completely fill the burette with dibutyl phthalate. Turn the stopcock at the top of the burette to the "delivery" position. Start the burette output switch until a constant flow rate is obtained from the tube.
B5.3 Stop titration and adjust the digital counter reading to zero. B5.4 Weigh the beaker (B3.2) to an accuracy of 0.01 liter and place it under the discharge tube. Simultaneously start the burette and stopwatch (B3.1) and titrate accurately for 2 min. Close the burette and record the counter reading. Weigh and record the amount of dibutyl phthalate released. Repeat the above operation with a titration time of 4 min and 8 min.
B6 Evaluation of calibration results
B6.1 Calculate the volume V of dibutyl phthalate released using formula (B1), expressed in cm\. V-
Where: n——mass of the released reagent, g: β——density of the reagent, g/cm.
GB/T 3780. 2-94
B6.2 The constant-rate burette of the oil absorption meter shall meet the requirements of Table B1. Table B1 Burettes that meet the requirements for use
Additional notes:
Counter reading
8.00±0. 05
16.00±0.10
32.00±0.20
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 Industry Research and Design Institute of the Ministry of Chemical Industry. Small
This standard was drafted by the Carbon Black Industry Research and Design Institute of the Ministry of Chemical Industry. The main drafters of this standard are Yu Lian, Yu Guifen and Xue Lei. Reagent release amount
8.00±0.05
16.00±0.10
32.00±0.20
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