CN107367440A - A kind of method for acetylene absorption measurement - Google Patents
A kind of method for acetylene absorption measurement Download PDFInfo
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- CN107367440A CN107367440A CN201710506863.XA CN201710506863A CN107367440A CN 107367440 A CN107367440 A CN 107367440A CN 201710506863 A CN201710506863 A CN 201710506863A CN 107367440 A CN107367440 A CN 107367440A
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Abstract
The present invention relates to sorbing material performance test field, a kind of method for acetylene absorption measurement, by drying the nano material sample of gas disposal will be gone to be put into sample cavity;Vavuum pump, magnetic valve are opened to device vacuum outgas;High pure nitrogen is filled with other regions in reference cavity, sample cavity and device vacuum system, records related data;The number of moles of gas into device vacuum system is determined by mass flow controller data, and calculates the gas volume for flowing through mass flow controller;Nitrogen in unlatching vavuum pump, magnetic valve withdrawing device;Acetylene gas is filled with reference cavity;Acetylene gas is expanded into the sample cavity in reference cavity, records barometer and thermocouple reading;Acetylene gas in unlatching vavuum pump, magnetic valve withdrawing device;Record the barometer and thermocouple reading under each equilibrium state air pressure;Gas absorption amount is calculated, is represented with molal quantity;Gas absorption amount data point under each equilibrium state air pressure of gained is drawn as curve, just obtains adsorption isotherm.
Description
Technical field
The present invention relates to sorbing material performance test field, particularly a kind of vacuum system for being capable of more accurate determining device
System volume, reduce error in calibration process, use quality flow controller measures total vacuum system volume, so as to avoid
Use a kind of method for acetylene absorption measurement of calibration sample.
Background technology
The basic skills that volumetric method surveys gas absorption is that vacuum system includes container I and container II, is placed in container I
A certain amount of sample of sorbent, and gas in container I is emptied and is maintained at certain temperature, then determine volume by one
Container II is passed through the gas of known quantity into container I, after to be adsorbed dose has adsorbed a certain amount of gas, in container I and container II
Air pressure reaches balance, and adsorbance can be calculated according to the change of air pressure before and after absorption.Gradually increase container II to vacuum system
The pressure of middle gas, and repeat the above steps, the gas absorption amount under different equilibrium air pressures is obtained, by each equilibrium state air pressure
Under the data point of gas absorption amount be drawn on X-Y scheme and connect into curve, ordinate is gas absorption amount, and abscissa is flat
Weigh state air pressure, just obtains the adsorption isotherm under some temperature conditions.
In the prior art, the dynamic volume of acetylene molecule is typically different than the helium determined as device volume, nitrogen etc.
Gas, inaccurate which results in the estimation of the sample rate to some materials, such as some bore hole sizes have the material of larger distribution
Or bore hole size and the close material of gas molecule, it is therefore desirable to more accurate test device, especially hold in vacuum system
In terms of long-pending determination.In addition, valve used in existing different types of test device can cause volumetric measurement to produce error, described one kind
Method for acetylene absorption measurement can solve problem, and magnetic valve of the present invention is the magnetic valve of particular design, it is characterized in that
Between open and close in change procedure, its internal capacity will not produce change.
The content of the invention
In order to solve the above problems, the present invention can reduce the systematic error in gas absorption measurement, can be tested
Air pressure range be 10-10Mbar to 500bar, it is the volumetric method absorption measuring method with higher experimental precision.
The technical solution adopted in the present invention is:
A kind of method for acetylene absorption measurement, measurement apparatus mainly include air accumulator I, air accumulator II, electromagnetism
Valve I, mass flow controller, electromagnetic valve II, reference cavity, electromagnetic valve II I, barometer, thermocouple, electromagnetic valve I V, vavuum pump, electromagnetism
Valve V, sample cavity and tracheae, described electromagnetic valve I one end by valve tracheae be connected to the air accumulator I and air accumulator II,
Tracheae connects the mass flow controller, electromagnetic valve II, reference cavity, electromagnetic valve I V, vavuum pump, the air pressure to the other end successively
Meter is located at outside the reference cavity by the electromagnetic valve II I connections reference cavity, the thermocouple, and the sample cavity passes through described
The magnetic valve V connections reference cavity, is equipped with the acetylene gas of test in the air accumulator I, equipped with height in the air accumulator II
Pure nitrogen gas, the barometer and thermocouple are respectively used to monitor the pressure and temperature with reference to intracavity gas, and the vavuum pump is used
Vacuumized in device, the sample cavity is in a thermostat with temperature needed for maintenance, the mass flow control
Device control enters the gas flow rate of the reference cavity, can be adjusted 0 between 30mln/min, error ± 0.2%, institute
Electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, magnetic valve V-type number is stated to be Burket2400 types and special set
Count between open and close in change procedure, its internal capacity will not produce change, and a kind of acetylene that is used for adsorbs survey
The method and step of amount is:
One, will go the nano material sample of gas disposal to be put into the sample cavity by drying;
Two, open the vavuum pump, and open the electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, electromagnetism
Valve V, vacuum outgas is carried out to device;
Three, close the electromagnetic valve I V, magnetic valve V, and open the valve on the air accumulator II so that high pure nitrogen fills
Enter other regions in the reference cavity, sample cavity and device vacuum system, in this process the mass flow control
Device sets certain state modulator gas flow rate and records related data;
Four, determine the number of moles of gas into device vacuum system by the data on flows of the mass flow controller,
And calculate the gas volume for flowing through the mass flow controllerWith air pressure P and vacuum system total measurement (volume) Vtot's
Relation isWherein TNAnd PNIt is the temperature and air pressure under normal condition, T is that vacuum system is held
Long-pending temperature, estimationSlope of a curve just can determine Vtot=VS+VR+Vother, wherein VSFor the sample cavity
Volume, VRFor the volume of the reference cavity, VotherFor the volume in other regions in device vacuum system;
Five, open the vavuum pump, and open the electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, electromagnetism
Valve V, nitrogen in withdrawing device;
Six, close the electromagnetic valve I V, magnetic valve V, and open the valve on the air accumulator I so that acetylene gas fills
Enter the reference cavity, the electromagnetic valve I is closed after equilibrium state to be achieved;
Seven, open the magnetic valve V so that acetylene gas is expanded into the sample cavity in the reference cavity, treats air pressure
The barometer reading and thermocouple reading are recorded after balance;
Eight, open the vavuum pump, and open the electromagnetic valve I, electromagnetic valve II, electromagnetic valve II I, electromagnetic valve I V, electromagnetism
Valve V, acetylene gas in withdrawing device;
Nine, repeat the above steps six to step 8, until air pressure reaches 500bar, if n times are repeated altogether, record each
The barometer reading and thermocouple reading under equilibrium state air pressure;
Ten, calculate gas absorption amount, are represented with molal quantity, after gas is expanded into the sample cavity by the reference cavity,
When air pressure reaches equilibrium state, the number of moles of gas of reduction is absorbed number of moles of gas;Under each equilibrium state air pressure, lead to
Real gas law is crossed to calculate gas absorption amount nads=ri[VR(r0/ri-1)-VS]+ri-1VS, wherein ri=Pi/(Z(Ti, Pi)
RTi) it is the molar density of gas, the integer that i is 1 to N, Z (Ti, Pi) it is gas in temperature TiWith air pressure PiUnder the conditions of compression system
Number, r0It is the molar density before gas expansion in reference cavity, riIt is that gas expands in the sample cavity and absorbed by sample
Molar density afterwards;The data point of gas absorption amount under each equilibrium state air pressure of gained is drawn on X-Y scheme and connected into
Curve, ordinate are the molal quantity of absorption, and abscissa is equilibrium state air pressure, just obtains adsorption isotherm.
The beneficial effects of the invention are as follows:
The present invention is capable of the vacuum system volume of more accurate determining device, reduces the error in calibration process, uses matter
Flow controller is measured to measure total vacuum system volume, reduces the uncertainty of experimental result, is also avoided using calibration sample
Product, it is the volumetric method absorption measuring method with higher experimental precision.
Brief description of the drawings
Further illustrated with reference to the figure of the present invention:
Fig. 1 is schematic diagram of the present invention.
In figure, 1. air accumulator I, 2. air accumulator II, 3. electromagnetic valve Is, 4. mass flow controllers, 5. electromagnetic valve IIs, 6. join
Examine chamber, 7. electromagnetic valve II I, 8. barometers, 9. thermocouples, 10. electromagnetic valve I V, 11. vavuum pumps, 12. magnetic valve V, 13. sample cavities.
Embodiment
If Fig. 1 is schematic diagram of the present invention, measurement apparatus mainly includes air accumulator I1, air accumulator II2, electromagnetic valve I 3, quality
Flow controller 4, electromagnetic valve II 5, reference cavity 6, electromagnetic valve II I7, barometer 8, thermocouple 9, electromagnetic valve I V10, vavuum pump 11, electricity
Magnet valve V12, sample cavity 13 and tracheae, described one end of electromagnetic valve I 3 are connected to the air accumulator I1 and the storage by valve tracheae
Tracheae connects the mass flow controller 4, electromagnetic valve II 5, reference cavity 6, electromagnetic valve I V10, true successively for gas tank II2, the other end
Empty pump 11, the barometer 8 are located at the reference cavity 6 by the electromagnetic valve II I7 connections reference cavity 6, the thermocouple 9
Outside, the sample cavity 13 is equipped with the second of test by the magnetic valve V12 connections reference cavity 6 in the air accumulator I1
Alkynes gas, high pure nitrogen is housed in the air accumulator II2, the barometer 8 and thermocouple 9 are respectively used to monitor the reference cavity 6
The pressure and temperature of interior gas, the vavuum pump 11 are used to vacuumize device, and the sample cavity 13 is located at a constant temperature
The gas flow rate of the reference cavity 6 is entered with temperature needed for maintenance, the control of mass flow controller 4 in groove, can
Adjusted 0 between 30mln/min, error ± 0.2%, the electromagnetic valve I 3, electromagnetic valve II 5, electromagnetic valve II I7, magnetic valve
IV10, magnetic valve V12 models be Burket2400 types and particular design into the change procedure between open and close,
Its internal capacity will not produce change, and a kind of method and step for acetylene absorption measurement is:
One, will go the nano material sample of gas disposal to be put into the sample cavity 13 by drying;
Two, open the vavuum pump 11, and open the electromagnetic valve I 3, electromagnetic valve II 5, electromagnetic valve II I7, magnetic valve
IV10, magnetic valve V12, vacuum outgas is carried out to device;
Three, close the electromagnetic valve I V10, magnetic valve V12, and open the valve on the air accumulator II2 so that high-purity
Nitrogen is filled with other regions in the reference cavity 6, sample cavity 13 and device vacuum system, in this process the quality
Flow controller 4 sets certain state modulator gas flow rate and records related data;
Four, determine the number of moles of gas into device vacuum system by the data on flows of the mass flow controller 4,
And calculate the gas volume for flowing through the mass flow controller (4)With air pressure P and vacuum system total measurement (volume) Vtot
Relation beWherein TNAnd PNIt is the temperature and air pressure under normal condition, T is vacuum system
The temperature of volume, estimationSlope of a curve just can determine Vtot=VS+VR+Vother, wherein VSFor the sample cavity
13 volume, VRFor the volume of the reference cavity 6, VotherFor the volume in other regions in device vacuum system;
Five, open the vavuum pump 11, and open the electromagnetic valve I 3, electromagnetic valve II 5, electromagnetic valve II I7, magnetic valve
IV10, magnetic valve V12, nitrogen in withdrawing device;
Six, close the electromagnetic valve I V10, magnetic valve V12, and open the valve on the air accumulator I1 so that acetylene gas
Body is filled with the reference cavity 6, and the electromagnetic valve I 3 is closed after equilibrium state to be achieved;
Seven, open the magnetic valve V12 so that acetylene gas is expanded into the sample cavity 13 in the reference cavity 6, treats
The reading of barometer 8 and thermocouple 9 reading is recorded after air pressure balance;
Eight, open the vavuum pump 11, and open the electromagnetic valve I 3, electromagnetic valve II 5, electromagnetic valve II I7, magnetic valve
IV10, magnetic valve V12, acetylene gas in withdrawing device;
Nine, repeat the above steps six to step 8, until air pressure reaches 500bar, if n times are repeated altogether, record each
The reading of the barometer 8 and the reading of thermocouple 9 under equilibrium state air pressure;
Ten, calculate gas absorption amount, are represented with molal quantity, gas is expanded into the sample cavity 13 by the reference cavity 6
Afterwards, when air pressure reaches equilibrium state, the number of moles of gas of reduction is absorbed number of moles of gas;Each equilibrium state air pressure
Under, gas absorption amount n is calculated by real gas lawads=ri[VR(r0/ri-1)-VS]+ri-1VS, wherein ri=Pi/(Z
(Ti, Pi)RTi) it is the molar density of gas, the integer that i is 1 to N, Z (Ti, Pi) it is gas in temperature TiWith air pressure PiUnder the conditions of
The compressed coefficient, r0It is the molar density before gas expansion in reference cavity, riIt is that gas expands and passed through in the sample cavity 13
Cross the molar density after sample absorbs;The data point of gas absorption amount under each equilibrium state air pressure of gained is drawn in X-Y scheme
Go up and connect into curve, ordinate is the molal quantity of absorption, and abscissa is equilibrium state air pressure, just obtains adsorption isotherm.
To sum up, by the present invention in that with mass flow controller and the magnetic valve of particular design, can more accurately survey
Total vacuum system volume is measured, and reduces the uncertainty of Adsorption experimental results.
Claims (1)
1. a kind of method for acetylene absorption measurement, measurement apparatus mainly includes air accumulator I (1), air accumulator II (2), electromagnetism
Valve I (3), mass flow controller (4), electromagnetic valve II (5), reference cavity (6), electromagnetic valve II I (7), barometer (8), thermocouple
(9), electromagnetic valve I V (10), vavuum pump (11), magnetic valve V (12), sample cavity (13) and tracheae, described electromagnetic valve I (3) one end lead to
Valve tracheae is crossed to be connected to the air accumulator I (1) tracheae connects the quality stream successively with the air accumulator II (2), the other end
Amount controller (4), electromagnetic valve II (5), reference cavity (6), electromagnetic valve I V (10), vavuum pump (11), the barometer (8) pass through institute
Electromagnetic valve II I (7) the connections reference cavity (6) is stated, the thermocouple (9) is located at the reference cavity (6) outside, the sample cavity (13)
The reference cavity (6) is connected by the magnetic valve V (12), the acetylene gas of test, institute are housed in the air accumulator I (1)
State and high pure nitrogen is housed in air accumulator II (2), the barometer (8) and thermocouple (9) are respectively used to monitor in the reference cavity (6)
The pressure and temperature of gas, the vavuum pump (11) are used to vacuumize device, and the sample cavity (13) is located at a perseverance
The gas flow speed of the reference cavity (6) is entered with temperature needed for maintenance, mass flow controller (4) control in warm groove
Rate, it can be adjusted 0 between 30mln/min, error ± 0.2%, the electromagnetic valve I (3), electromagnetic valve II (5), magnetic valve
III (7), electromagnetic valve I V (10), magnetic valve V (12) model be Burket2400 types and particular design into open and close
Between closing in change procedure, its internal capacity will not produce change,
It is characterized in that:It is described it is a kind of for acetylene absorption measurement method and step be:
One, will go the nano material sample of gas disposal to be put into the sample cavity (13) by drying;
Two, open the vavuum pump (11), and open the electromagnetic valve I (3), electromagnetic valve II (5), electromagnetic valve II I (7), electromagnetism
Valve IV (10), magnetic valve V (12), vacuum outgas is carried out to device;
Three, close the electromagnetic valve I V (10), magnetic valve V (12), and open the valve on the air accumulator II (2) so that high
Pure nitrogen gas is filled with other regions in the reference cavity (6), sample cavity (13) and device vacuum system, in this process institute
Mass flow controller (4) is stated to set certain state modulator gas flow rate and record related data;
Four, determine the number of moles of gas into device vacuum system by the data on flows of the mass flow controller (4), and
The gas volume of the mass flow controller (4) is flowed through in calculatingWith air pressure P and vacuum system total measurement (volume) Vtot's
Relation isWherein TNAnd PNIt is the temperature and air pressure under normal condition, T is that vacuum system is held
Long-pending temperature, estimationSlope of a curve just can determine Vtot=VS+VR+Vother, wherein VSFor the sample cavity
(13) volume, VRFor the volume of the reference cavity (6), VotherFor the volume in other regions in device vacuum system;
Five, open the vavuum pump (11), and open the electromagnetic valve I (3), electromagnetic valve II (5), electromagnetic valve II I (7), electromagnetism
Valve IV (10), magnetic valve V (12), nitrogen in withdrawing device;
Six, close the electromagnetic valve I V (10), magnetic valve V (12), and open the valve on the air accumulator I (1) so that acetylene
Gas is filled with the reference cavity (6), and the electromagnetic valve I (3) is closed after equilibrium state to be achieved;
Seven, open the magnetic valve V (12) so that and acetylene gas is expanded into the sample cavity (13) in the reference cavity (6),
The barometer (8) reading and thermocouple (9) reading are recorded after air pressure balance;
Eight, open the vavuum pump (11), and open the electromagnetic valve I (3), electromagnetic valve II (5), electromagnetic valve II I (7), electromagnetism
Valve IV (10), magnetic valve V (12), acetylene gas in withdrawing device;
Nine, repeat the above steps six to step 8, until air pressure reaches 500bar, if n times are repeated altogether, record each balance
The barometer (8) reading and thermocouple (9) reading under state air pressure;
Ten, calculate gas absorption amount, are represented with molal quantity, gas is expanded into the sample cavity (13) by the reference cavity (6)
Afterwards, when air pressure reaches equilibrium state, the number of moles of gas of reduction is absorbed number of moles of gas;Each equilibrium state air pressure
Under, gas absorption amount n is calculated by real gas lawads=ri[VR(r0/ri-1)-VS]+ri-1VS, wherein ri=Pi/(Z
(Ti, Pi)RTi) it is the molar density of gas, the integer that i is 1 to N, Z (Ti, Pi) it is gas in temperature TiWith air pressure PiUnder the conditions of
The compressed coefficient, r0It is the molar density before gas expansion in reference cavity, riIt is that gas expands simultaneously in the sample cavity (13)
Molar density after sample absorbs;The data point of gas absorption amount under each equilibrium state air pressure of gained is drawn in two dimension
On figure and curve is connected into, ordinate is the molal quantity of absorption, and abscissa is equilibrium state air pressure, just obtains adsorption isotherm.
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Cited By (3)
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CN109142130A (en) * | 2018-09-16 | 2019-01-04 | 金华职业技术学院 | A kind of adsorbent test method |
CN109238905A (en) * | 2018-09-16 | 2019-01-18 | 金华职业技术学院 | A kind of gas absorption test device |
CN112945794A (en) * | 2021-02-02 | 2021-06-11 | 南昌师范学院 | Used for detecting SO of activated carbon fiber pair2Method for adsorption amount |
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CN109142130A (en) * | 2018-09-16 | 2019-01-04 | 金华职业技术学院 | A kind of adsorbent test method |
CN109238905A (en) * | 2018-09-16 | 2019-01-18 | 金华职业技术学院 | A kind of gas absorption test device |
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CN112945794A (en) * | 2021-02-02 | 2021-06-11 | 南昌师范学院 | Used for detecting SO of activated carbon fiber pair2Method for adsorption amount |
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