HG/T 3073-1999 Determination of specific surface area of precipitated hydrated silicon dioxide in rubber compounding ingredients - Nitrogen adsorption method
Some standard content:
Record number: 4077--1999
HG/T3073-1999
The first part of this standard is a non-equivalent adoption of the international standard ISO4652-1:1994 "Rubber compounding agent - Carbon black - Determination of specific surface area by nitrogen adsorption", which is a revision of the A method in the recommended chemical industry standard HG/T3073-1989 "Rubber compounding agent precipitated hydrated silica specific surface area determination nitrogen adsorption method". The main differences between the first part of this standard and ISO4652-1:1994 are: - ISO4652-1 stipulates four methods for determining the specific surface area of carbon black for rubber. This standard equivalently adopts one of them, A method (using Ni-Count-1 instrument), that is, the static adsorption method, while retaining the dynamic adsorption method currently used in my country. This standard adds sampling.
The main difference between this standard and HG/T3073-1989 is that this standard specifies two determination methods as the first and second parts, of which the first part is the arbitration method. This standard adds "Foreword" and "ISO Foreword" - This standard stipulates the use of the standard reference carbon black calibration instrument in ISO/TR6809-96. This standard will replace HG/T3073-1989 from the date of implementation. This standard was proposed by the Technical Supervision Department of the former 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 Technical Committee for Standardization of Rubber and Rubber Products. The drafting unit of this standard: Carbon Black Industry Research and Design Institute. The main drafters of this standard: Xue Lei, Zhou Yongmei. This standard was first issued as the national standard GB10529-89 in March 1989, and was adjusted to the chemical industry standard in December 1997, and renumbered as HG/T3073-1989, and the original GB10529-89 was abolished. 45
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing international standards is normally carried out by ISO technical committees. Any member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO may also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft international standards adopted by technical committees are circulated to member bodies for voting. Publication as an international standard requires an affirmative vote by at least 75 % of the member bodies casting a vote.
International Standard ISO 4652-1 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials for the rubber industry (including latex).
This standard is a technical revision of the first edition, which cancels and replaces it (ISO 4652-1: 1981). The general title of ISO 4652 is: Rubber compounding ingredients — Carbon black — Determination of specific surface area — Nitrogen adsorption method. It includes the following parts:
Part 1: Single point method
Part 2: BET multi-point method
Appendix A is an integral part of ISO4652.
Chemical Industry Standard of the People's Republic of China
Rubber compounding ingredients—Silica, precipitated, hydrated
Determination of specific surface area-Nitrogen adsorption method
Rubber compounding ingredients—Silica, precipitated, hydratedDetermination of specific surface area-Nitrogen adsorptionmethod1Scope
HG/T3073—1999
neq Iso4652-i:1994
Replaces HG/T3073-1989
This standard specifies the method for determining the specific surface area of precipitated hydrated silica by static adsorption method or dynamic adsorption method. This standard is applicable to the determination of specific surface area of various types of precipitated hydrated silica. 2 Reference standards
The clauses contained in the following standards constitute the clauses of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. HG/T3061-1999 Technical conditions for precipitated hydrated silica in rubber compounding ingredients (neqISO5794-1:1994) ISO/TR6809:1996 Rubber compounding ingredients-carbon black-standard reference carbon black Part I Static adsorption method
3 Principle
Put a quantitative degassed precipitated hydrated silica sample in a nitrogen flow at liquid nitrogen temperature, and after the nitrogen adsorbed on the surface of the precipitated hydrated silica reaches equilibrium, determine its adsorption amount, and calculate the specific surface area of the sample based on its adsorption amount. 4 Reagents and materials
4.1 Pure nitrogen: in steel cylinders or other nitrogen sources, first-class products. 4.2 Liquid nitrogen.
4.3 High vacuum grease No. 1.
4.4 Fine glass wool.
4.5 Benzene: chemically pure.
4.6 Acetone: chemically pure.
4.7 Ethanol: chemically pure.
5 Instruments and equipments
General laboratory instruments and equipments and
5.1 Nitrogen adsorption specific surface area measuring instrument: Ni-Count-1 (see Figures 1 and 2) or other single-point nitrogen adsorption specific surface area measuring instruments.
Approved by the State Administration of Petroleum and Chemical Industry on August 12, 1999 and implemented on October 1, 2000
Pressure gauge evacuation valve and pipeline
Container and pipeline for calibration volume
Flow control valve
Pressure regulator
HG/T3073-1999
(0~103)kPa
Precision pressure gauge (0~775)mmHg
Vacuum indicator
Electric heater (3 pieces)
Connect to nitrogen vapor pressure thermometer
Connect to vacuum pump
Vacuum Branch pipe
Liquid nitrogen dewar flask
Figure 1 Schematic diagram of four-sample tube Ni-Count-1 specific surface area measuring instrument Pure nitrogen
Filling connection
Ring-shaped copper wire on the edge of the dewar flask
Precision pressure gauge (0~25)kPa
(0~186)mmHg
Volume container
Thermometer sensing element
Liquid nitrogen dewar flask
Figure 2 Nitrogen vapor pressure thermometer
Note: The system has been filled with pure nitrogen, and the pressure is 13~20kPa (100~150mmHg). 5.2 Temperature-controlled heating electric furnace: The temperature can be maintained at (160±10)℃. 5.3 Vacuum pump: Ultimate pressure 1.3×10-2Pa. 48
5.4 Dewar flask: Capacity is about 265cm3.
5.5 Liquid nitrogen container: capacity 30dm2.
HG/T3073—1999
5.6 Nitrogen vapor pressure thermometer (see Figure 2) or oxygen vapor pressure thermometer. 5.7 Sample tube: see Figure 3.
Stainless steel wire
Sample funnel
5.8 Analytical balance: accuracy 0.1mg.
6 Test conditions
Glass sample tube
Figure 3 Sample funnel and glass sample tube
2/5 spherical ground
Pipeline 8×1
Filling rod or tube with closed ends, $5
Glass wool group
6.1 The test should be carried out at relative humidity (50±5)%, room temperature (23±2)℃, or relative humidity (65±5)%, room temperature (27±2)℃. 6.2 Reagents and instruments should be kept at laboratory temperature and humidity for 24h before use. 6.3 The laboratory should be free of smoke to avoid affecting the test results. 7 Sampling 1
Carry out according to the provisions of HG/T3061.
Instructions for use:
1] ISO4652-1:1994 does not have such provisions. 49
8 Sample preparation
HG/T3073—1999
8.1 Granular samples do not need to be crushed and can be degassed directly on the instrument or on a special vacuum device outside the machine. 8.2 If powdered samples need to be compacted, they can be compacted and then degassed on the instrument or on a special vacuum device outside the machine. 9 Preparation and calibration of instruments
9.1 The volume of the Ni-Count-1 specific surface area measuring instrument (including the pipeline leading to the vacuum valve and the pressure gauge) at room temperature 27°C and pressure 66.7kPa is 139.5cm (calibrated by the manufacturer). If the internal volume has been adjusted to 139.5cm, the accurate specific surface area will be obtained based on the functional relationship chart of surface area and pressure (provided with the instrument). 9.2 Use the standard reference carbon black in ISO/TR6809 to test to confirm the internal volume of the instrument. 9.3 The preparation of the Naconte-1 specific surface area measuring instrument should be carried out according to the instrument manual. This includes filling the nitrogen vapor pressure thermometer with nitrogen and flushing and evacuating the calibration volume tube and vacuum branch pipe with the valve closed until the air is exhausted. 9.4 The temperature of the electric furnace is controlled at (160 ± 10) ° C. To prevent air from entering the system, it should be evacuated at any time and filled with nitrogen for purification. 9.5 The calibration and accuracy of the instrument are checked with the standard reference carbon black specified in ISO/TR6809. Measurement steps
10.1 Refer to the provisions in Table 1 and select the appropriate sample size. Table 1 Reference table of precipitated hydrated silica sample dosage Category
Specific surface area, m2/g
161~190
136~160
106~135
71~105
10.2 Weigh a ball of glass wool of appropriate size (accurate to 0.1 mg), and record its mass (m1). Sample quantity, g
0.84~0.27
1.00~0.84
1.20~1.00
1.50~1.20
2.25~1.50
10.3 Weigh a clean sample tube with a filled glass rod (accurate to 0.1 mg), and record its mass (m2). 10.4 Roughly weigh the sample (mass before degassing). Put the sample into the sample tube, push the glass wool ball onto the sample, and put in the filling rod. 10.5 Apply high vacuum grease to the spherical ground mouth of the sample tube (be careful not to get into the tube). Install the sample tube on the instrument. 10.6 Perform vacuum degassing at (160±10)℃. During degassing, use nitrogen to purify the sample several times instantly, that is: close the valve to the vacuum pump, open the valve from nitrogen to the vacuum tube, and then re-evacuate. 10.7 Close the vacuum valve and use the vacuum indicator to check whether there is gas released from the sample. Keep the pressure no more than 0.1kPa. After 5 minutes, if there is no change in the vacuum indicator, it proves that the sample is degassed. 10.8 Close the valve to isolate the degassed sample from the vacuum tube and remove the temperature-controlled heating furnace. 10.9 Fill the purified container, pressure gauge and pipeline with nitrogen until the pressure is 66.7 kPa (500 mmHg) at room temperature of 27°C. If it exceeds or falls below this room temperature, 0.222 kPa (1.67 mmHg) should be added or subtracted for every 1°C increase or decrease. 10.10 Open the valve of the calibration volume tube leading to the sample tube to allow nitrogen to enter the sample tube. 10.11
Put the Dewar flask filled with liquid nitrogen on the sample tube. 10.12 When the sample is adsorbed, it should be carefully observed. When the pressure gauge pointer is stable and unchanged, it proves that the adsorption has reached equilibrium. Record the pressure gauge reading, accurate to 0.1 kPa (1 mmHg). The height of the liquid nitrogen surface must be kept unchanged during the entire adsorption process. 10.13 Put the Dewar flask on the sensing element of the nitrogen (or oxygen) vapor pressure thermometer. After the nitrogen (or oxygen) vapor pressure thermometer is stable, observe and record its reading, accurate to 0.1 kPa. HG/T3073—1999
10.14 Pass nitrogen into the sample tube until the pressure gauge reading is about 1.3 kPa (10 mmHg) higher than the atmospheric pressure, close the valve, and gently remove the sample tube.
10.15 Open the valve leading to the sample tube, connect to the atmosphere, and record the pressure gauge reading, accurate to 0.1 kPa, and close the valve. 10.16 Use a little solvent to wipe the high vacuum grease on the spherical ground mouth of the sample tube with absorbent cotton, and wipe off the water droplets on the outside of the sample tube, unscrew the vacuum valve to evacuate the main pipe and branch pipe.
10.17 Weigh the sample tube (including the dried and degassed sample, glass wool and filled glass rod, accurate to 0.1 mg), and record the mass (m3). 10.18 The pressure measured in 10.13 plus the atmospheric pressure is the vapor pressure Pz of nitrogen (which can be directly obtained by looking up the table using an oxygen pressure gauge). Then look up Table 2 to obtain the liquid nitrogen temperature correction factor B.
11Results show
Specific surface area Sm (m2/g) is calculated according to formula (1): S[1-F(V,-Va-V,
Wherein: S--.-Surface area under equilibrium pressure (see Table 3), m; m-
Degassed carbon black sample volume (m=ms-m1-m2), g; F correlation factor (see Table 3);
VVolume of sample tube after adding filling rod, cm;
Vat—Volume of sample tube neck above liquid nitrogen surface, cm\; Vgw—Volume of glass wool (density calculated as 2.3g/cm), cm;-Density of precipitated hydrated silica, density calculated as 2.0g/cm; B. Liquid nitrogen temperature correction factor (see Table 2). The calculation result is accurate to 0.1m2/g.||tt ||12 Correction factor
Use standard reference carbon black (see Table 4) to determine the specific surface area. If the difference between the measured value and the recognized value of the standard reference carbon black exceeds ±1.2 m2/g, calculate the correction factor of the instrument according to formula (2). Correction factor =
13 Test report
The test report should include the following:
a Information required for complete identification of the sample;
b Standard number based on which this test is based (specify static adsorption method); c Test conditions;
d Calculation results;
Recognized value
Measured value
e If standard reference carbon black is selected, indicate the correction factor and the standard reference carbon black used. (2)
Nitrogen vapor pressure
Correction factor
0. 964 47
0. 966 77
0. 967 34
0. 972 50
HG/T3073—1999
Table 2 Liquid nitrogen temperature correction factor
Nitrogen vapor pressurebZxz.net
Correction factor
0. 987 97
Nitrogen vapor pressure
Correction factor
0. 997 71
0. 998 28
1. 001 72
1. 003 44
1. 004 01
1. 006 30
1. 008 02
Nitrogen vapor pressure
Correction factor
Liquid nitrogen temperature correction factor B is derived from the following formula: HG/T3073—1999
Table 2 (end)
Nitrogen vapor pressure
Correction factor
1+0.0573×
Where: Pn——vapor pressure of pure nitrogen at liquid nitrogen temperature, measured by nitrogen vapor pressure thermometer, kPa; nitrogen vapor pressure
98.7--—the atmospheric pressure when the surface area S (see Table 3) under equilibrium pressure is measured by the calibrated instrument, kPa. If the pressure is expressed in mmHg, the above formula is: 1+0.0573×
『PN-740
Correction factor
Equilibrium pressure
Correlation factor
0. 008 28
0. 009 06
HG/T3073—1999
Values of S and F corresponding to equilibrium pressure
Surface area
Equilibrium pressure
Correlation factor
0. 012 20
Surface area
Equilibrium pressure
Correlation factor
0. 017 61
0. 021 68
HG/T3073—1999
Table 3 (continued)
Surface area
Equilibrium pressure
Correlation factor
0. 025 29
0. 026 84
Surface area00~0.84
1.20~1.00
1.50~1.20
2.25~1.50
10.3 Weigh a clean sample tube with a filled glass rod (accurate to 0.1 mg) and record its mass (m2). 10.4 Roughly weigh the sample (mass before degassing). Place the sample in the sample tube, push the glass wool ball onto the sample, and put in the filling rod. 10.5 Apply high vacuum grease to the spherical ground mouth of the sample tube (be careful not to enter the tube). Install the sample tube on the instrument. 10.6 Vacuum degas at (160±10)℃. When degassing, use nitrogen to purify the sample several times instantly, that is, close the valve to the vacuum pump, open the valve to the nitrogen to the vacuum tube, and then re-evacuate. 10.7 Close the vacuum valve and use a vacuum indicator to check whether there is gas released from the sample. Keep the pressure no more than 0.1 kPa. If the vacuum indicator does not change after 5 minutes, it proves that the sample is completely degassed. 10.8 Close the valve to isolate the degassed sample from the vacuum tube and remove the temperature-controlled heating electric furnace. 10.9 Fill the purified container, pressure gauge and pipeline with nitrogen until the pressure is 66.7 kPa (500 mmHg) at room temperature of 27°C. If it exceeds or falls below this room temperature, 0.222 kPa (1.67 mmHg) should be added or subtracted for every 1°C increase or decrease. 10.10 Open the valve of the calibrated volume tube leading to the sample tube to allow nitrogen to enter the sample tube. 10.11
Put the Dewar flask containing liquid nitrogen on the sample tube. 10.12 When the sample is adsorbed, it should be carefully observed. When the pressure gauge pointer is stable, it proves that the adsorption has reached equilibrium. Record the pressure gauge reading, accurate to 0.1 kPa (1 mmHg). The height of the liquid nitrogen surface must be kept constant during the entire adsorption process. 10.13 Put the Dewar flask on the sensing element of the nitrogen (or oxygen) vapor pressure thermometer. After the nitrogen (or oxygen) vapor pressure thermometer stabilizes, observe and record its reading, accurate to 0.1kPa. HG/T3073—1999
10.14 Pass nitrogen into the sample tube until the pressure gauge reading is about 1.3kPa (10mmHg) higher than the atmospheric pressure, close the valve, and gently remove the sample tube.
10.15 Open the valve leading to the sample tube, connect to the atmosphere, and record the pressure gauge reading, accurate to 0.1kPa, and close the valve. 10.16 Use a little solvent to wipe off the high vacuum grease on the spherical ground mouth of the sample tube with absorbent cotton, and wipe off the water droplets on the outside of the sample tube, unscrew the vacuum valve to evacuate the main pipe and branch pipes.
10.17 Weigh the sample tube (including the dried and degassed sample, glass wool and filled glass rod, accurate to 0.1 mg), and record the mass (m3). 10.18 The pressure measured in 10.13 plus the atmospheric pressure is the nitrogen vapor pressure Pz (which can be directly obtained by looking up the table using an oxygen pressure gauge), and then look up Table 2 to obtain the liquid nitrogen temperature correction factor B.
11Results show
Specific surface area Sm (m2/g) is calculated according to formula (1): S[1-F(V,-Va-V,
Wherein: S--.-Surface area under equilibrium pressure (see Table 3), m; m-
Degassed carbon black sample volume (m=ms-m1-m2), g; F correlation factor (see Table 3);
VVolume of sample tube after adding filling rod, cm;
Vat—Volume of sample tube neck above liquid nitrogen surface, cm\; Vgw—Volume of glass wool (density calculated as 2.3g/cm), cm;-Density of precipitated hydrated silica, density calculated as 2.0g/cm; B. Liquid nitrogen temperature correction factor (see Table 2). The calculation result is accurate to 0.1m2/g.||tt ||12 Correction factor
Use standard reference carbon black (see Table 4) to determine the specific surface area. If the difference between the measured value and the recognized value of the standard reference carbon black exceeds ±1.2 m2/g, calculate the correction factor of the instrument according to formula (2). Correction factor =
13 Test report
The test report should include the following:
a Information required for complete identification of the sample;
b Standard number based on which this test is based (specify static adsorption method); c Test conditions;
d Calculation results;
Recognized value
Measured value
e If standard reference carbon black is selected, indicate the correction factor and the standard reference carbon black used. (2)
Nitrogen vapor pressure
Correction factor
0. 964 47
0. 966 77
0. 967 34
0. 972 50
HG/T3073—1999
Table 2 Liquid nitrogen temperature correction factor
Nitrogen vapor pressure
Correction factor
0. 987 97
Nitrogen vapor pressure
Correction factor
0. 997 71
0. 998 28
1. 001 72
1. 003 44
1. 004 01
1. 006 30
1. 008 02
Nitrogen vapor pressure
Correction factor
Liquid nitrogen temperature correction factor B is derived from the following formula: HG/T3073—1999
Table 2 (end)
Nitrogen vapor pressure
Correction factor
1+0.0573×
Where: Pn——vapor pressure of pure nitrogen at liquid nitrogen temperature, measured by nitrogen vapor pressure thermometer, kPa; nitrogen vapor pressure
98.7--—the atmospheric pressure when the surface area S (see Table 3) under equilibrium pressure is measured by the calibrated instrument, kPa. If the pressure is expressed in mmHg, the above formula is: 1+0.0573×
『PN-740
Correction factor
Equilibrium pressure
Correlation factor
0. 008 28
0. 009 06
HG/T3073—1999
Values of S and F corresponding to equilibrium pressure
Surface area
Equilibrium pressure
Correlation factor
0. 012 20
Surface area
Equilibrium pressure
Correlation factor
0. 017 61
0. 021 68
HG/T3073—1999
Table 3 (continued)
Surface area
Equilibrium pressure
Correlation factor
0. 025 29
0. 026 84
Surface area00~0.84
1.20~1.00
1.50~1.20
2.25~1.50
10.3 Weigh a clean sample tube with a filled glass rod (accurate to 0.1 mg) and record its mass (m2). 10.4 Roughly weigh the sample (mass before degassing). Place the sample in the sample tube, push the glass wool ball onto the sample, and put in the filling rod. 10.5 Apply high vacuum grease to the spherical ground mouth of the sample tube (be careful not to enter the tube). Install the sample tube on the instrument. 10.6 Vacuum degas at (160±10)℃. When degassing, use nitrogen to purify the sample several times instantly, that is, close the valve to the vacuum pump, open the valve to the nitrogen to the vacuum tube, and then re-evacuate. 10.7 Close the vacuum valve and use a vacuum indicator to check whether there is gas released from the sample. Keep the pressure no more than 0.1 kPa. If the vacuum indicator does not change after 5 minutes, it proves that the sample is completely degassed. 10.8 Close the valve to isolate the degassed sample from the vacuum tube and remove the temperature-controlled heating electric furnace. 10.9 Fill the purified container, pressure gauge and pipeline with nitrogen until the pressure is 66.7 kPa (500 mmHg) at room temperature of 27°C. If it exceeds or falls below this room temperature, 0.222 kPa (1.67 mmHg) should be added or subtracted for every 1°C increase or decrease. 10.10 Open the valve of the calibrated volume tube leading to the sample tube to allow nitrogen to enter the sample tube. 10.11
Put the Dewar flask containing liquid nitrogen on the sample tube. 10.12 When the sample is adsorbed, it should be carefully observed. When the pressure gauge pointer is stable, it proves that the adsorption has reached equilibrium. Record the pressure gauge reading, accurate to 0.1 kPa (1 mmHg). The height of the liquid nitrogen surface must be kept constant during the entire adsorption process. 10.13 Put the Dewar flask on the sensing element of the nitrogen (or oxygen) vapor pressure thermometer. After the nitrogen (or oxygen) vapor pressure thermometer stabilizes, observe and record its reading, accurate to 0.1kPa. HG/T3073—1999
10.14 Pass nitrogen into the sample tube until the pressure gauge reading is about 1.3kPa (10mmHg) higher than the atmospheric pressure, close the valve, and gently remove the sample tube.
10.15 Open the valve leading to the sample tube, connect to the atmosphere, and record the pressure gauge reading, accurate to 0.1kPa, and close the valve. 10.16 Use a little solvent to wipe off the high vacuum grease on the spherical ground mouth of the sample tube with absorbent cotton, and wipe off the water droplets on the outside of the sample tube, unscrew the vacuum valve to evacuate the main pipe and branch pipes.
10.17 Weigh the sample tube (including the dried and degassed sample, glass wool and filled glass rod, accurate to 0.1 mg), and record the mass (m3). 10.18 The pressure measured in 10.13 plus the atmospheric pressure is the nitrogen vapor pressure Pz (which can be directly obtained by looking up the table using an oxygen pressure gauge), and then look up Table 2 to obtain the liquid nitrogen temperature correction factor B.
11Results show
Specific surface area Sm (m2/g) is calculated according to formula (1): S[1-F(V,-Va-V,
Wherein: S--.-Surface area under equilibrium pressure (see Table 3), m; m-
Degassed carbon black sample volume (m=ms-m1-m2), g; F correlation factor (see Table 3);
VVolume of sample tube after adding filling rod, cm;
Vat—Volume of sample tube neck above liquid nitrogen surface, cm\; Vgw—Volume of glass wool (density calculated as 2.3g/cm), cm;-Density of precipitated hydrated silica, density calculated as 2.0g/cm; B. Liquid nitrogen temperature correction factor (see Table 2). The calculation result is accurate to 0.1m2/g.||tt ||12 Correction factor
Use standard reference carbon black (see Table 4) to determine the specific surface area. If the difference between the measured value and the recognized value of the standard reference carbon black exceeds ±1.2 m2/g, calculate the correction factor of the instrument according to formula (2). Correction factor =
13 Test report
The test report should include the following:
a Information required for complete identification of the sample;
b Standard number based on which this test is based (specify static adsorption method); c Test conditions;
d Calculation results;
Recognized value
Measured value
e If standard reference carbon black is selected, indicate the correction factor and the standard reference carbon black used. (2)
Nitrogen vapor pressure
Correction factor
0. 964 47
0. 966 77
0. 967 34
0. 972 50
HG/T3073—1999
Table 2 Liquid nitrogen temperature correction factor
Nitrogen vapor pressure
Correction factor
0. 987 97
Nitrogen vapor pressure
Correction factor
0. 997 71
0. 998 28
1. 001 72
1. 003 44
1. 004 01
1. 006 30
1. 008 02
Nitrogen vapor pressure
Correction factor
Liquid nitrogen temperature correction factor B is derived from the following formula: HG/T3073—1999
Table 2 (end)
Nitrogen vapor pressure
Correction factor
1+0.0573×
Where: Pn——vapor pressure of pure nitrogen at liquid nitrogen temperature, measured by nitrogen vapor pressure thermometer, kPa; nitrogen vapor pressure
98.7--—the atmospheric pressure when the surface area S (see Table 3) under equilibrium pressure is measured by the calibrated instrument, kPa. If the pressure is expressed in mmHg, the above formula is: 1+0.0573×
『PN-740
Correction factor
Equilibrium pressure
Correlation factor
0. 008 28
0. 009 06
HG/T3073—1999
Values of S and F corresponding to equilibrium pressure
Surface area
Equilibrium pressure
Correlation factor
0. 012 20
Surface area
Equilibrium pressure
Correlation factor
0. 017 61
0. 021 68
HG/T3073—1999
Table 3 (continued)
Surface area
Equilibrium pressure
Correlation factor
0. 025 29
0. 026 84
Surface area15 Open the valve leading to the sample tube, connect to the atmosphere, and record the pressure gauge reading, accurate to 0.1kPa, and close the valve. 10.16 Use a little solvent to wipe off the high vacuum grease on the spherical ground mouth of the sample tube with absorbent cotton, and wipe off the water droplets on the outside of the sample tube, unscrew the vacuum valve to evacuate the main pipe and branch pipes.
10.17 Weigh the sample tube (including the dried and degassed sample, glass wool and filled glass rod, accurate to 0.1mg), and record the mass (m3). 10.18 The pressure measured in 10.13 plus the atmospheric pressure is the vapor pressure of nitrogen Pz (which can be directly obtained by looking up the table using an oxygen pressure gauge), and then look up Table 2 to obtain the liquid nitrogen temperature correction factor B.
11Results show
Specific surface area Sm (m2/g) is calculated according to formula (1): S[1-F(V,-Va-V,
Wherein: S--.-Surface area under equilibrium pressure (see Table 3), m; m-
Degassed carbon black sample volume (m=ms-m1-m2), g; F correlation factor (see Table 3);
VVolume of sample tube after adding filling rod, cm;
Vat—Volume of sample tube neck above liquid nitrogen surface, cm\; Vgw—Volume of glass wool (density calculated as 2.3g/cm), cm;-Density of precipitated hydrated silica, density calculated as 2.0g/cm; B. Liquid nitrogen temperature correction factor (see Table 2). The calculation result is accurate to 0.1m2/g.||tt ||12 Correction factor
Use standard reference carbon black (see Table 4) to determine the specific surface area. If the difference between the measured value and the recognized value of the standard reference carbon black exceeds ±1.2 m2/g, calculate the correction factor of the instrument according to formula (2). Correction factor =
13 Test report
The test report should include the following:
a Information required for complete identification of the sample;
b Standard number based on which this test is based (specify static adsorption method); c Test conditions;
d Calculation results;
Recognized value
Measured value
e If standard reference carbon black is selected, indicate the correction factor and the standard reference carbon black used. (2)
Nitrogen vapor pressure
Correction factor
0. 964 47
0. 966 77
0. 967 34
0. 972 50
HG/T3073—1999
Table 2 Liquid nitrogen temperature correction factor
Nitrogen vapor pressure
Correction factor
0. 987 97
Nitrogen vapor pressure
Correction factor
0. 997 71
0. 998 28
1. 001 72
1. 003 44
1. 004 01
1. 006 30
1. 008 02
Nitrogen vapor pressure
Correction factor
Liquid nitrogen temperature correction factor B is derived from the following formula: HG/T3073—1999
Table 2 (end)
Nitrogen vapor pressure
Correction factor
1+0.0573×
Where: Pn——vapor pressure of pure nitrogen at liquid nitrogen temperature, measured by nitrogen vapor pressure thermometer, kPa; nitrogen vapor pressure
98.7--—the atmospheric pressure when the surface area S (see Table 3) under equilibrium pressure is measured by the calibrated instrument, kPa. If the pressure is expressed in mmHg, the above formula is: 1+0.0573×
『PN-740
Correction factor
Equilibrium pressure
Correlation factor
0. 008 28
0. 009 06
HG/T3073—1999
Values of S and F corresponding to equilibrium pressure
Surface area
Equilibrium pressure
Correlation factor
0. 012 20
Surface area
Equilibrium pressure
Correlation factor
0. 017 61
0. 021 68
HG/T3073—1999
Table 3 (continued)
Surface area
Equilibrium pressure
Correlation factor
0. 025 29
0. 026 84
Surface area15 Open the valve leading to the sample tube, connect to the atmosphere, and record the pressure gauge reading, accurate to 0.1kPa, and close the valve. 10.16 Use a little solvent to wipe off the high vacuum grease on the spherical ground mouth of the sample tube with absorbent cotton, and wipe off the water droplets on the outside of the sample tube, unscrew the vacuum valve to evacuate the main pipe and branch pipes.
10.17 Weigh the sample tube (including the dried and degassed sample, glass wool and filled glass rod, accurate to 0.1mg), and record the mass (m3). 10.18 The pressure measured in 10.13 plus the atmospheric pressure is the vapor pressure of nitrogen Pz (which can be directly obtained by looking up the table using an oxygen pressure gauge), and then look up Table 2 to obtain the liquid nitrogen temperature correction factor B.
11Results show
Specific surface area Sm (m2/g) is calculated according to formula (1): S[1-F(V,-Va-V,
Wherein: S--.-Surface area under equilibrium pressure (see Table 3), m; m-
Degassed carbon black sample volume (m=ms-m1-m2), g; F correlation factor (see Table 3);
VVolume of sample tube after adding filling rod, cm;
Vat—Volume of sample tube neck above liquid nitrogen surface, cm\; Vgw—Volume of glass wool (density calculated as 2.3g/cm), cm;-Density of precipitated hydrated silica, density calculated as 2.0g/cm; B. Liquid nitrogen temperature correction factor (see Table 2). The calculation result is accurate to 0.1m2/g.||tt ||12 Correction factor
Use standard reference carbon black (see Table 4) to determine the specific surface area. If the difference between the measured value and the recognized value of the standard reference carbon black exceeds ±1.2 m2/g, calculate the correction factor of the instrument according to formula (2). Correction factor =
13 Test report
The test report should include the following:
a Information required for complete identification of the sample;
b Standard number based on which this test is based (specify static adsorption method); c Test conditions;
d Calculation results;
Recognized value
Measured value
e If standard reference carbon black is selected, indicate the correction factor and the standard reference carbon black used. (2)
Nitrogen vapor pressure
Correction factor
0. 964 47
0. 966 77
0. 967 34
0. 972 50
HG/T3073—1999
Table 2 Liquid nitrogen temperature correction factor
Nitrogen vapor pressure
Correction factor
0. 987 97
Nitrogen vapor pressure
Correction factor
0. 997 71
0. 998 28
1. 001 72
1. 003 44
1. 004 01
1. 006 30
1. 008 02
Nitrogen vapor pressure
Correction factor
Liquid nitrogen temperature correction factor B is derived from the following formula: HG/T3073—1999
Table 2 (end)
Nitrogen vapor pressure
Correction factor
1+0.0573×
Where: Pn——vapor pressure of pure nitrogen at liquid nitrogen temperature, measured by nitrogen vapor pressure thermometer, kPa; nitrogen vapor pressure
98.7--—the atmospheric pressure when the surface area S (see Table 3) under equilibrium pressure is measured by the calibrated instrument, kPa. If the pressure is expressed in mmHg, the above formula is: 1+0.0573×
『PN-740
Correction factor
Equilibrium pressure
Correlation factor
0. 008 28
0. 009 06
HG/T3073—1999
Values of S and F corresponding to equilibrium pressure
Surface area
Equilibrium pressure
Correlation factor
0. 012 20
Surface area
Equilibrium pressure
Correlation factor
0. 017 61
0. 021 68
HG/T3073—1999
Table 3 (continued)
Surface area
Equilibrium pressure
Correlation factor
0. 025 29
0. 026 84
Surface area025 29
0. 026 84
Surface area025 29
0. 026 84
Surface area
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