CN107340204B - Method for measuring multiple isotherms during a complete charge - Google Patents
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- CN107340204B CN107340204B CN201710506861.0A CN201710506861A CN107340204B CN 107340204 B CN107340204 B CN 107340204B CN 201710506861 A CN201710506861 A CN 201710506861A CN 107340204 B CN107340204 B CN 107340204B
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- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000007789 gas Substances 0.000 claims abstract description 90
- 238000001179 sorption measurement Methods 0.000 claims abstract description 43
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 41
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 238000009849 vacuum degassing Methods 0.000 claims abstract description 8
- 238000009736 wetting Methods 0.000 claims abstract description 4
- 238000012360 testing method Methods 0.000 claims description 9
- 238000007872 degassing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 5
- 238000011056 performance test Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 238000002474 experimental method Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009530 blood pressure measurement Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
Abstract
The invention relates to the field of performance test of adsorption materials, in particular to a method capable of measuring multiple isotherms in a complete inflation pressurization process, which comprises the steps of vacuum degassing; filling high-purity nitrogen into the reference cavity, the sample cavity and other areas in the device vacuum system, and recording related data; determining the number of moles of gas entering the vacuum system of the apparatus and calculating the volume of gas flowing through the mass flow controller; measuring the initial mass of a dried sample, wetting the sample in a steam environment, measuring the mass of the wet sample, filling the wet sample into a sample cavity, and carrying out vacuum degassing on the device for five minutes; acetylene is filled into the reference cavity, and the temperature T 0 of the reference cavity is recorded; the gas expands into the sample cavity and reaches an equilibrium state, the temperature T 1 of the reference cavity is recorded, the temperature of the constant temperature tank is regulated to be increased to T 2, the temperature of the constant temperature tank is regulated to be continuously increased to T 3, and meanwhile related data is recorded; until the equilibrium air pressure of the sample cavity reaches 500bar; excess adsorption calculation; the gas adsorption data points for each equilibrium gas pressure were plotted as curves.
Description
Technical Field
The invention relates to the field of performance test of adsorption materials, in particular to a method for researching the temperature dependence in acetylene adsorption under high pressure in a wet sample, and for measuring acetylene adsorption, which can be used for measuring multiple isotherms in a complete inflation pressurization process.
Background
The basic method for measuring gas adsorption by the capacity method is that a vacuum system comprises a container I and a container II, a certain amount of adsorbent sample is placed in the container I, the container I is emptied of gas and kept at a certain temperature, then a known amount of gas is introduced into the container I through a container II with a certain volume, after the adsorbent adsorbs a certain amount of gas, the gas pressure in the container I and the container II reaches equilibrium, and the adsorption amount can be calculated according to the change of the gas pressure before and after adsorption. And gradually increasing the pressure of the gas in the container II to the vacuum system, repeating the steps to obtain the gas adsorption quantity under different equilibrium pressures, drawing data points of the gas adsorption quantity under each equilibrium state pressure on a two-dimensional graph and connecting the two-dimensional graph to form a curve, wherein the ordinate is the gas adsorption quantity, and the abscissa is the equilibrium state pressure, so that an adsorption isotherm under a certain temperature condition can be obtained.
In the prior art, the dynamic volumes of acetylene molecules are often different from the gases such as helium, nitrogen, etc. used for device volume determination, which results in inaccurate estimates of sample density for certain materials, such as materials with larger distributions of pore sizes or materials with pore sizes close to the gas molecules, and thus require more accurate testing devices, especially in terms of determination of vacuum system volumes. In addition, some adsorption experiments need to be performed on wet samples, and the major difficulty in experiments in the prior art is that small changes in water content in different individual test experiments can significantly affect the adsorption capacity of the adsorbent samples to acetylene, so that the adsorption capacity obtained by the experiments is not dependent on temperature only, and thus causes large errors, and the method capable of measuring multiple isotherms in one complete inflation pressurization process can solve the problems.
Disclosure of Invention
In order to solve the problems, the invention is a simple method for carrying out adsorption experiments by a pressure measurement method, namely, adsorption isotherms at different temperatures are measured under the condition of a closed system, the water content can be kept constant at all temperatures, and in addition, the measurement time can be greatly reduced because no degassing of samples is needed between independent tests under different temperature conditions.
The technical scheme adopted by the invention is as follows:
The method capable of measuring multiple isotherms in a complete inflation pressurization process mainly comprises an air storage tank I, an air storage tank II, an electromagnetic valve I, a mass flow controller, an electromagnetic valve II, a reference cavity, an electromagnetic valve III, a barometer, a thermocouple, an electromagnetic valve IV, a vacuum pump, an electromagnetic valve V, a sample cavity, a constant temperature tank and an air pipe, wherein one end of the electromagnetic valve I is connected with the air storage tank I through the air pipe of the valve I, the other end of the electromagnetic valve II is connected with the mass flow controller, the electromagnetic valve II, the reference cavity, the electromagnetic valve IV and a vacuum pump through the electromagnetic valve III, the thermocouple is connected with the outside of the reference cavity, the sample cavity is connected with the reference cavity through the electromagnetic valve V, the reference cavity, the thermocouple, the electromagnetic valve V and the sample cavity are positioned in the constant temperature tank so as to keep consistent and controllable, acetylene gas for testing is filled in the air storage tank I, the barometer and the thermocouple are respectively used for monitoring the temperature and the temperature of gas in the reference cavity, the vacuum pump is used for controlling the vacuum pump, and the vacuum pump is used for controlling the pressure and the vacuum pump to be different from the electromagnetic valve I to the vacuum pump, and the vacuum pump to be in the vacuum pump type II, and the vacuum pump type can be changed to the volume error of the electromagnetic valve I and the electromagnetic valve II can be equal to the volume error of the electromagnetic valve II and the vacuum pump to the electromagnetic valve II and the vacuum valve V.
The method capable of measuring multiple isotherms in a complete inflation pressurization process comprises the following steps:
Under the condition that no sample exists in the device, a vacuum system seals and starts the vacuum pump, and the electromagnetic valve I, the electromagnetic valve II, the electromagnetic valve III, the electromagnetic valve IV and the electromagnetic valve V are started to carry out vacuum degassing on the device;
Closing the electromagnetic valve IV, opening the electromagnetic valve V, and opening a valve on the gas storage tank II, so that high-purity nitrogen is filled into the reference cavity, the sample cavity and other areas in the device vacuum system, and in the process, the mass flow controller sets a certain parameter to control the gas flow rate and records related data;
Determining the number of moles of gas entering the vacuum system of the device from the flow data of the mass flow controller and calculating the volume of gas flowing through the mass flow controller The relation between the air pressure P and the total volume V tot of the vacuum system is/>Where T N and P N are the temperature and pressure under normal conditions, T is the temperature of the vacuum system volume, estimate/>The slope of the curve enables determination of V tot＝VS+VR+Vother, where V S is the volume of the sample chamber, V R is the volume of the reference chamber, and V other is the volume of other areas within the device vacuum system;
Fourthly, taking a sample to be measured, drying the sample in other devices in a vacuum heating mode, measuring the initial mass m 0 of the dried sample, wetting the sample in a steam environment, measuring the wet sample mass m 1, filling the wet sample into the sample cavity, starting the vacuum pump, starting the electromagnetic valve I, the electromagnetic valve II, the electromagnetic valve III, the electromagnetic valve IV and the electromagnetic valve V, and carrying out five-minute preliminary vacuum degassing on the device;
Closing the electromagnetic valve IV and the electromagnetic valve V, opening a valve on the air storage tank I, filling acetylene gas into the reference cavity, closing the electromagnetic valve I after the acetylene gas reaches an equilibrium state, and recording the temperature T 0 of the reference cavity and the reading of the barometer at the moment;
Opening the electromagnetic valve V to enable gas to expand into the sample cavity and enable the gas to reach an equilibrium state with the sample, namely, no gas is continuously absorbed, recording the temperature T 1 of the reference cavity at the moment and the barometer reading, adjusting the constant temperature tank to raise the temperature to T 2, recording the barometer reading at the moment after the equilibrium state is reached, adjusting the constant temperature tank to continuously raise the temperature to T 3, recording the barometer reading at the moment after the equilibrium state is reached, and enabling data points corresponding to three isotherms of T 1、T2 and T 3 to be simultaneously determined in a single gas injection process;
Seventhly, repeating the fifth step and the sixth step until the balance air pressure of the sample cavity reaches 500bar, and carrying out the operation of filling acetylene gas into the reference cavity from the gas storage tank I for N times, namely, a complete inflation and pressurization process;
Calculation of excess adsorption, i-th excess adsorption after the operation of filling acetylene gas into the reference chamber, by the difference between the total mass of gas entering the sample chamber and the mass of gas occupying the volume of the vacuum system Where i is an integer between 1 and N,/>For the ith operation of filling acetylene gas into the reference cavity and reaching the density of acetylene under the pressure and temperature conditions after balancing, the mass of acetylene transferred from the reference cavity into the sample cavity is determined byCalculation of/>, whereAnd/>The density of acetylene in the reference cavity during the filling period and the balance period in the ith acetylene filling operation is obtained by looking up the table of the air pressure and the temperature conditions measured in the fifth step and the sixth step respectively;
Ninth, excess adsorption mass normalized to sample mass Wherein m 0 is the initial mass of the sample, T j is T 1、T2 or T 3, and the excess adsorption quantity under each temperature condition, namely the mole number of adsorbed gas, is obtainedWherein M gas is the molar mass of acetylene;
And ten, the data of the gas adsorption quantity under each equilibrium state air pressure obtained under a certain temperature T j are stippled on a two-dimensional graph and connected into a curve, the ordinate is the mole number of the adsorbed gas, and the abscissa is the equilibrium state air pressure, so that the adsorption isotherm under the T j condition can be obtained, and the adsorption isotherms under a plurality of temperature conditions can be obtained at one time in a complete pressurizing process of acetylene gas without carrying out degassing operation on a sample for a plurality of times, thereby saving time.
The beneficial effects of the invention are as follows:
the invention is different from the traditional pressure measuring method used in the high-pressure adsorption test in that the temperature of the gas in the acetylene adsorption test is controllable and variable; because the continuous isotherm measurement needs to be deaerated after each single adsorption test, more time is needed, compared with the continuous isotherm measurement experiment, the method can greatly reduce the measurement time, and is an adsorption measurement method capable of obtaining multiple isotherms at one time in a complete inflation pressurization process; the water content in the system of the device of the present invention remains constant at all temperature conditions, which allows negligible variation of the sample water content with temperature under conditions where the vacuum volume of the system is sufficiently small.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic diagram of the present invention.
In the figure, the air storage tank I, the air storage tank II, the electromagnetic valve I, the mass flow controller 4, the electromagnetic valve II, the reference cavity 6, the electromagnetic valve III, the barometer 8, the thermocouple 9, the electromagnetic valve IV, the electromagnetic valve 11, the vacuum pump 12, the electromagnetic valve V, the sample cavity 13 and the constant temperature tank 14 are shown.
Detailed Description
As shown in FIG. 1, the measuring device mainly comprises an air storage tank I1, an air storage tank II2, an electromagnetic valve I3, a mass flow controller 4, an electromagnetic valve II5, a reference cavity 6, an electromagnetic valve III7, a barometer 8, a thermocouple 9, an electromagnetic valve IV10, a vacuum pump 11, an electromagnetic valve V12, a sample cavity 13, a thermostatic bath 14 and an air pipe, wherein one end of the electromagnetic valve I3 is connected with the air storage tank I1 and the air storage tank II2 through a valve air pipe, the other end is sequentially connected with the mass flow controller 4, the electromagnetic valve II5, the reference cavity 6, the electromagnetic valve IV10 and the vacuum pump 11 through the electromagnetic valve III7, the thermocouple 9 is connected outside the reference cavity 6, the sample cavity 13 is connected with the reference cavity 6 through the electromagnetic valve V12, the reference cavity 6, the thermocouple 9, the electromagnetic valve V12 and the sample cavity 13 are positioned in the constant temperature tank 14 to keep the temperature consistent and controllable, acetylene gas for testing is filled in the gas storage tank I1, high-purity nitrogen is filled in the gas storage tank II2, the barometer 8 and the thermocouple 9 are respectively used for monitoring the pressure and the temperature of the gas in the reference cavity 6, the vacuum pump 11 is used for vacuumizing the device, the mass flow controller 4 controls the flow rate of the gas entering the reference cavity 6, the gas flow rate can be adjusted between 0 and 30ln/min, the error is +/-0.2%, and the types of the electromagnetic valve I3, the electromagnetic valve II5, the electromagnetic valve III7, the electromagnetic valve IV10 and the electromagnetic valve V12 are Burket types 2400, and are specially designed so that the internal volume of the device cannot change in the process of changing between opening and closing.
The method capable of measuring multiple isotherms in a complete inflation pressurization process comprises the following steps:
under the condition that no sample exists in the device, a vacuum system seals and starts the vacuum pump 11, and the electromagnetic valves I3, II5, III7, IV10 and V12 are opened to perform vacuum degassing on the device;
Closing the electromagnetic valve IV10, opening the electromagnetic valve V12, and opening the valve on the gas storage tank II2 to enable high-purity nitrogen to be filled into the reference cavity 6, the sample cavity 13 and other areas in the device vacuum system, wherein in the process, the mass flow controller 4 sets a certain parameter to control the gas flow rate and records related data;
determining the number of moles of gas entering the vacuum system of the device from the flow data of the mass flow controller 4 and calculating the volume of gas flowing through the mass flow controller 4 The relation between the air pressure P and the total volume V tot of the vacuum system is/>Where T N and P N are the temperature and pressure under normal conditions, T is the temperature of the vacuum system volume, estimate/>The slope of the curve enables determination of V tot＝VS+VR+Vother, where V S is the volume of the sample chamber 13, V R is the volume of the reference chamber 6, and V other is the volume of other areas within the device vacuum system;
Fourthly, taking a sample to be measured, drying the sample in other devices in a vacuum heating mode, measuring the initial mass m 0 of the dried sample, wetting the sample in a steam environment, measuring the wet sample mass m 1, filling the wet sample into the sample cavity 13, starting the vacuum pump 11, starting the electromagnetic valves I3, II5, III7, IV10 and V12, and performing five-minute preliminary vacuum degassing on the device;
Fifthly, closing the electromagnetic valve IV10 and the electromagnetic valve V12, opening a valve on the air storage tank I1 to enable acetylene gas to be filled into the reference cavity 6, closing the electromagnetic valve I3 after the equilibrium state is reached, and recording the temperature T 0 of the reference cavity 6 and the reading of the barometer 8 at the moment;
Opening the electromagnetic valve V12 to enable gas to expand into the sample cavity 13 and reach an equilibrium state with the sample, namely no gas is continuously absorbed, recording the temperature T 1 of the reference cavity 6 at the moment and the reading of the barometer 8, adjusting the constant temperature tank 14 to raise the temperature to T 2, recording the reading of the barometer 8 at the moment after the equilibrium state is reached, adjusting the constant temperature tank 14 to continuously raise the temperature to T 3, and recording the reading of the barometer 8 at the moment after the equilibrium state is reached, so that data points corresponding to three isotherms of T 1、T2 and T 3 can be simultaneously determined in a single gas injection process;
Seventhly, repeating the fifth step and the sixth step until the equilibrium air pressure of the sample cavity 13 reaches 500bar, and performing the operation of filling acetylene gas from the gas storage tank I1 into the reference cavity 6 for a total of N times, namely, a complete inflation and pressurization process;
Calculation of excess adsorption, i-th excess adsorption after the operation of filling acetylene gas into the reference chamber 6, is calculated by the difference between the total mass of gas entering the sample chamber 13 and the mass of gas occupying the volume of the vacuum system Where i is an integer between 1 and N,/>For the ith operation of filling acetylene gas into the reference chamber 6 and achieving the density of acetylene under the pressure and temperature conditions after equilibrium, the mass of acetylene transferred from the reference chamber 6 into the sample chamber 13 is determined byCalculation of/>, whereAnd/>The density of acetylene in the reference cavity 6 during the filling period and the balance period in the ith acetylene filling operation is obtained by looking up the table of the air pressure and the temperature conditions measured in the fifth step and the sixth step respectively;
Ninth, excess adsorption mass normalized to sample mass Wherein m 0 is the initial mass of the sample, T j is T 1、T2 or T 3, and the excess adsorption quantity under each temperature condition, namely the mole number of adsorbed gas, is obtainedWherein M gas is the molar mass of acetylene;
And ten, the data of the gas adsorption quantity under each equilibrium state air pressure obtained under a certain temperature T j are stippled on a two-dimensional graph and connected into a curve, the ordinate is the mole number of the adsorbed gas, and the abscissa is the equilibrium state air pressure, so that the adsorption isotherm under the T j condition can be obtained, and the adsorption isotherms under a plurality of temperature conditions can be obtained at one time in a complete pressurizing process of acetylene gas without carrying out degassing operation on a sample for a plurality of times, thereby saving time.
In the complete pressurizing process of filling acetylene gas, the vacuum system of the device is not required to be opened, so that the water content in the vacuum system is unchanged, and the difference of the results of independent experiments caused by different water contents is reduced.
Claims (1)
1. The method capable of measuring multiple isotherms in a complete inflation pressurization process mainly comprises an air storage tank I (1), an air storage tank II (2), an electromagnetic valve I (3), a mass flow controller (4), an electromagnetic valve II (5), a reference cavity (6), an electromagnetic valve III (7), a barometer (8), a thermocouple (9), an electromagnetic valve IV (10), a vacuum pump (11), an electromagnetic valve V (12), a sample cavity (13), a thermostatic bath (14) and an air pipe, wherein one end of the electromagnetic valve I (3) is connected with the air storage tank I (1) and the air storage tank II (2) through a valve air pipe, the other end is connected with the mass flow controller (4), the electromagnetic valve II (5), the reference cavity (6), the electromagnetic valve IV (10) and the vacuum pump (11) through the electromagnetic valve III (7), the thermocouple (9) is connected with the reference cavity (6), the sample cavity (13) is connected with the reference cavity (6) through the electromagnetic valve V (12), the thermocouple (6), the electromagnetic valve V (12) and the temperature of the electromagnetic valve V (13) is kept consistent in the sample cavity (14), acetylene gas for testing is filled in the gas storage tank I (1), high-purity nitrogen is filled in the gas storage tank II (2), the barometer (8) and the thermocouple (9) are respectively used for monitoring the pressure and the temperature of the gas in the reference cavity (6), the vacuum pump (11) is used for vacuumizing the device, the mass flow controller (4) is used for controlling the flow rate of the gas entering the reference cavity (6) and can be adjusted between 0ml/min and 30ml/min, the error is +/-0.2%, the types of the electromagnetic valve I (3), the electromagnetic valve II (5), the electromagnetic valve III (7), the electromagnetic valve IV (10) and the electromagnetic valve V (12) are Burket and are specially designed so that the internal volume of the electromagnetic valve I (3), the electromagnetic valve III (10) and the electromagnetic valve V (12) cannot change in the changing process between opening and closing,
The method is characterized in that: the method capable of measuring multiple isotherms in a complete inflation pressurization process comprises the following steps:
Under the condition that no sample exists in the device, a vacuum system seals and starts the vacuum pump (11), and the electromagnetic valve I (3), the electromagnetic valve II (5), the electromagnetic valve III (7), the electromagnetic valve IV (10) and the electromagnetic valve V (12) are started to carry out vacuum degassing on the device;
closing the electromagnetic valve IV (10), opening the electromagnetic valve V (12), and opening a valve on the gas storage tank II (2) to enable high-purity nitrogen to be filled into the reference cavity (6), the sample cavity (13) and other areas in the device vacuum system, wherein in the process, the mass flow controller (4) sets a certain parameter to control the gas flow rate and records related data;
Determining the number of moles of gas entering the vacuum system of the device from the flow data of the mass flow controller (4) and calculating the volume of gas flowing through the mass flow controller (4) The relation between the air pressure P and the total volume V tot of the vacuum system is/>Where T N and P N are the temperature and pressure under normal conditions, T is the temperature of the vacuum system volume, estimate/>The slope of the curve enables determination of V tot＝VS+VR+Vother, where V S is the volume of the sample chamber (13), V R is the volume of the reference chamber (6), and V other is the volume of other areas within the device vacuum system;
Taking a sample to be measured, drying the sample in other devices in a vacuum heating mode, measuring the initial mass m 0 of the dried sample, wetting the sample in a steam environment, measuring the wet sample mass m 1, filling the wet sample into the sample cavity (13), starting the vacuum pump (11), starting the electromagnetic valve I (3), the electromagnetic valve II (5), the electromagnetic valve III (7), the electromagnetic valve IV (10) and the electromagnetic valve V (12), and performing five-minute preliminary vacuum degassing on the device;
Closing the electromagnetic valve IV (10) and the electromagnetic valve V (12), opening a valve on the air storage tank I (1) to enable acetylene gas to be filled into the reference cavity (6), closing the electromagnetic valve I (3) after the equilibrium state is reached, and recording the temperature T 0 of the reference cavity (6) and the reading of the barometer (8) at the moment;
opening the electromagnetic valve V (12) to enable gas to expand into the sample cavity (13) and reach an equilibrium state with the sample, namely no gas is continuously absorbed, recording the temperature T 1 of the reference cavity (6) and the reading of the barometer (8), adjusting the constant temperature tank (14) to raise the temperature to T 2, recording the reading of the barometer (8) after the equilibrium state is reached, adjusting the constant temperature tank (14) to continuously raise the temperature to T 3, and recording the reading of the barometer (8) after the equilibrium state is reached, so that data points corresponding to three isotherms of T 1、T2 and T 3 can be simultaneously determined in a single gas injection process;
Seventhly, repeating the fifth step and the sixth step until the equilibrium air pressure of the sample cavity (13) reaches 500bar, and carrying out the operation of filling acetylene gas into the reference cavity (6) from the air storage tank I (1) for N times, namely, a complete inflation and pressurization process;
calculation of excess adsorption, i-th excess adsorption after the operation of filling the reference chamber (6) with acetylene gas, by the difference between the total mass of the gas entering the sample chamber (13) and the mass of the gas occupying the volume of the vacuum system Where i is an integer between 1 and N,/>For the ith operation of filling acetylene gas into the reference chamber (6) and reaching the density of acetylene under the pressure and temperature conditions after equilibrium, the mass of acetylene transferred from the reference chamber (6) into the sample chamber (13) is determined byCalculation of/>, whereAnd/>The density of acetylene in the reference cavity (6) in the filling period and the balance period in the ith acetylene filling operation is obtained by looking up the table of the air pressure and the temperature conditions measured in the fifth step and the sixth step respectively;
Ninth, excess adsorption mass normalized to sample mass Wherein m 0 is the initial mass of the sample, T j is T 1、T2 or T 3, and the excess adsorption quantity under each temperature condition, namely the mole number of adsorbed gas, is obtainedWherein M gas is the molar mass of acetylene;
And ten, the data of the gas adsorption quantity under each equilibrium state air pressure obtained under a certain temperature T j are stippled on a two-dimensional graph and connected into a curve, the ordinate is the mole number of the adsorbed gas, and the abscissa is the equilibrium state air pressure, so that the adsorption isotherm under the T j condition can be obtained, and the adsorption isotherms under a plurality of temperature conditions can be obtained at one time in a complete pressurizing process of acetylene gas without carrying out degassing operation on a sample for a plurality of times, thereby saving time.
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