CN109856298A - The mass spectrograph caliberating device and method of the measurement of mixed gas containing high-temperature vapor - Google Patents
The mass spectrograph caliberating device and method of the measurement of mixed gas containing high-temperature vapor Download PDFInfo
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- CN109856298A CN109856298A CN201910138235.XA CN201910138235A CN109856298A CN 109856298 A CN109856298 A CN 109856298A CN 201910138235 A CN201910138235 A CN 201910138235A CN 109856298 A CN109856298 A CN 109856298A
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Abstract
A kind of mass spectrograph caliberating device of the measurement of mixed gas containing high-temperature vapor, comprising: standard gas preparation facilities interconnected and measuring device, in which: standard gas preparation facilities is connect with mass spectrograph.The present invention mixes known proportion with high-temperature vapor without steam calibrating gas to prepare the mixing standard gas containing high-temperature vapor, can mix the ratio of each component in standard gas by adjusting the amount for the vapor for entering pressure vessel, adjustment；The present invention is able to carry out the mass spectrograph measurement calibration of the mixed gas containing high-temperature vapor under normal pressure and high pressure, vdiverse in function；The present invention obtains the component of each gas by two kinds of calculations, is mutually authenticated each other, improves the accuracy and confidence level of measurement；The present invention normal mixture body be produce in times of requiring, prepare with by way of with survey, ensure that preferable gas stabilization.
Description
Technical field
The present invention relates to a kind of technology in mass spectrograph calibration field, specifically a kind of mixed gas containing high-temperature vapor
The mass spectrograph caliberating device and method of measurement.
Background technique
After Fukushima, Japan accident, people are to the Hydrogen distribution under emergency conditions inside npp safety shell, and migration feelings
Condition is studied more and more.When carrying out containment hydrogen Related Experimental Study, need to steam the high water of high temperature and pressure in container
The each component concentration of the mixed gas of Gas content measures.The mass spectrograph used at different conditions should use different standards
Gas is calibrated, and ingredient, pressure and the temperature of standard gas should be identical as object gas as far as possible.The prior art is mostly used at single group
The method that other high-purity gas are passed through in part standard gas is customized, and can specifically be divided into static volumetric method and Devince By Dynamic Gas Ration Method.It should
Technology has the following problems: the stability of flow in order to guarantee high-purity calibrating gas that every kind is passed through causes flow control system to set
Count sufficiently complex；In order to make different gas enter a container, the pressure difference between each single standard gas cannot mistake
Greatly, to limit the use of this programme；Mixed calibrating gas is under same stagnation pressure and same temperature, in mixed gas
The states of matter of all gas must be consistent, cannot condense, however for vapor higher for boiling point, it is difficult to ensure that
It is not coagulated in mixed process；The gas having in itself in mixing vessel will affect the constituent content of calibrating gas, in turn
Reduce calibration effect.In addition to the foregoing problems, existing mass spectrograph calibration technique can not also be suitable for high temperature and pressure and become condition
Moisture vapor mixed gas calibration.
Summary of the invention
The present invention In view of the above shortcomings of the prior art, proposes a kind of matter of measurement of mixed gas containing high-temperature vapor
Spectrometer caliberating device and method prepare steam-laden standard mixture by the current method now made and carry out multi-state and mix
Close Demarcate Gas.
The present invention is achieved by the following technical solutions:
The present invention includes: standard gas preparation facilities interconnected and measuring device, in which: standard gas preparation facilities and mass spectrograph
Connection.
The standard gas preparation facilities includes: standard gas tank, pressure vessel, temperature control equipment, water softening device and steam
Generator, in which: standard gas tank and steam generator pass through ventilation pipe respectively and be connected with pressure vessel, water softening device and steam
Generator is connected, and the temperature control equipment for pressure vessel and ventilation pipe to be heated and kept the temperature is set to pressure vessel
With ventilation pipe surface.
The pressure vessel is hollow cavity, which is provided with air inlet, exhaust outlet, sample tap, the detection of the first oxygen concentration
Mouth, sensor installation port and the installation of TC mouth, in which: air inlet is set to the top of pressure vessel, and exhaust outlet is set to pressure
The bottom of force container, sample tap, sensor installation port, the installation of TC mouth and the first oxygen concentration detection mouth are radially disposed at pressure
On container, sample tap is connected by sampling line with mass spectrograph.
The pressure vessel is equipped with the second oxygen concentration detection mouth further preferably with common with the first oxygen concentration detection mouth
Ensure that the gas inside pressure vessel has been sufficiently mixed, the second oxygen concentration detection mouth and the first oxygen concentration detection mouth pass through pressure
The central cross section of container is symmetrical arranged and sample tap, sensor installation port and the installation of TC mouth are located at the detection of the first oxygen concentration
Near mouth and the second oxygen concentration detection mouth.
The inside of the pressure vessel, which is preferably provided with, stirs and make muddy device to guarantee that the standard gas in pressure vessel uniformly mixes.
The temperature control equipment includes: heating warmer, temperature controller and temperature measurement equipment, in which: heating
Warmer is set in the outside wall surface of ventilation pipe and pressure vessel, and temperature measurement equipment probes into ventilation pipe and pressure vessel
Portion is simultaneously set near its inner surface, and temperature measurement equipment and heating warmer are connected with temperature controller respectively.
The measuring device includes: oxygen concentration detection device and high-precision pressure sensor, in which: oxygen concentration detection is set
Standby to be connected with oxygen concentration detection mouth, high-precision pressure sensor is connected with sensor installation port.
The present invention relates to a kind of method using above-mentioned apparatus, by heating warmer by ventilation pipe, pressure vessel and
Sampling line is heated to preset temperature and maintains, then the high temperature and high pressure steam that steam generator and water softening device are generated jointly
It is passed through pressure vessel, and by the air formed in standard gas tank and Z gas according to the mixed gas injection pressure container of preset ratio, so
The oxygen purity in pressure vessel is measured using oxygen concentration detection device afterwards and air, Z gas and water is obtained by calculation
The actual ratio of steam extracts the standard gas in pressure vessel finally by sampling line and is passed into mass spectrograph, completes calibration.
The volume fraction of the airThe volume fraction of Z gasVapor
Volume fraction w=1-y-z, in which: x is oxygen purity, n1For the ratio of gas in standard gas tank shared by air, n2For Z gas
The ratio of gas in shared standard gas tank.
The actual ratio can also be measured respectively by obtaining oxygen concentration detection device and high-precision pressure sensor
Pressure vessel in oxygen partial pressure and stagnation pressure, then measure by temperature measurement equipment the temperature of mixed gas, finally utilize reason
Think that the equation of gas state finds out the ratio of three kinds of gas respectively.
The Z gas is the stable single standard gas of chemical property or chemical property stabilization and the known mixing of ratio
Calibrating gas.
Technical effect
Compared with prior art, the present invention mixes known proportion to prepare without steam calibrating gas with high-temperature vapor
Mixing standard gas containing high-temperature vapor can mix each in standard gas by adjusting the amount for the vapor for entering pressure vessel, adjustment
The ratio of component；The present invention is able to carry out the mass spectrograph measurement mark of the mixed gas containing high-temperature vapor under normal pressure and high pressure
It is fixed, it is vdiverse in function；The present invention obtains the component of each gas by two kinds of calculations, is mutually authenticated each other, improves survey
The accuracy and confidence level of amount；The present invention normal mixture body be produce in times of requiring, prepare with by way of with survey, guarantee
Preferable gas stabilization.
Detailed description of the invention
Fig. 1 is the device of the invention structural schematic diagram；
Fig. 2 is method flow schematic diagram of the invention；
Fig. 3 is the structural schematic diagram of the pressure vessel of embodiment 1；
Fig. 4 is the structural schematic diagram of the pressure vessel of embodiment 2；
In figure: standard gas preparation facilities A, measuring device B, temperature control equipment 0, standard gas tank 1, pressure vessel 2, heating and thermal insulation
Device 3, temperature controller 4, temperature measurement equipment 5, water softening device 6, steam generator 7, regulating valve 8, the second shut-off valve 9,
One ventilation pipe~third ventilation pipe 101~103, mass spectrograph 12, air inlet 201, exhaust outlet 202, takes water supply pipe 11
Sample mouth 203, sensor installation port 205, the installation of TC mouth 206, stirs and make muddy device 207, the second oxygen at first oxygen concentration detection mouth 204
Concentration Testing mouth 208,13, three mouthfuls of pipes 14 of sampling line, oxygen concentration detection device 15,16, first sections of high-precision pressure sensor
Only valve 17.
Specific embodiment
Embodiment 1
As shown in Figure 1, the present embodiment includes: standard gas preparation facilities A and measuring device B interconnected, in which: standard gas system
Standby device A is connect with mass spectrograph 12.
The standard gas preparation facilities A includes: standard gas tank 1, pressure vessel 2, temperature control equipment 0,6 and of water softening device
Steam generator 7, in which: standard gas tank 1 is connected by the first ventilation pipe 101 with pressure vessel 2, and steam generator 7 passes through the
Two ventilation pipes 102 are connected with pressure vessel 2, and water softening device 6 is connected with steam generator 7, temperature control equipment 0 respectively with
Pressure vessel 2, ventilation pipe 101 are connected with the second ventilation pipe 102.
As shown in figure 3, the pressure vessel 2 is hollow cavity, air inlet 201, exhaust outlet 202, sampling which is provided with
Mouthful the 203, first oxygen concentration detection mouth 204, sensor installation port 205, the installation of TC mouth 206 and stir and make muddy device 207, in which: into
Port 201 is set to the top of pressure vessel 2, and exhaust outlet 202 is set to the bottom of pressure vessel 2, sample tap 203, sensor
Installing port 205, the installation of TC mouth 206 and the first oxygen concentration detection mouth 204 are radially disposed on pressure vessel 2, sample tap 203
It is connected by sampling line 13 with mass spectrograph 12, stirs and make muddy the inside that device 207 is set to pressure vessel 2.
The device 207 of stiring and make muddy includes: three fan blades for being set to enclosure interior, in which: one end of three fan blades is fixed
Size in the center for stiring and make muddy device 207 and the angle of every two fan blades composition is identical.
The air inlet 201 is connected with the first ventilation pipe 101 and the second ventilation pipe 102 respectively by three mouthfuls of pipes 14
So that the high-temperature vapor that mixed gas and steam generator 7 that standard gas tank 1 is discharged are discharged mixes in advance before entering pressure vessel 2
It closes.
The pressure vessel 2 uses stainless steel material and maximum pressure-bearing range is 1~1.5MPa.
The position spacing of the sample tap 203, sensor installation port 205 and the first oxygen concentration detection mouth 204 is less than
200mm is to reduce influence of the local pressure variation to measurement result caused by the flowing of 2 internal cause gas of pressure vessel.
The temperature control equipment 0 includes: heating warmer 3, temperature controller 4 and temperature measurement equipment 5, in which:
Heating warmer 3 is in contact with ventilation pipe and pressure vessel 2, one end of temperature measurement equipment 5 respectively with the first ventilation pipe
101, the second ventilation pipe 102 is connected with the installation of TC mouth 206 is higher than the Water vapor condensation temperature of pressure instantly with monitoring temperature
Degree, the other end are connected with temperature controller 4.
Instantly the pressure refers to: the pressure for the mixed gas that high-precision pressure sensor 16 is measured.
Electric-heating belt is arranged particular by the outer wall of ventilation pipe and pressure vessel 2 in the heating warmer 3
Mode realize heating and thermal insulation.
The insulating layer that the outside of electric-heating belt in the present embodiment is equipped with a thickness of 50~100mm, the preferred rock of the insulating layer
Cotton material.
Temperature controller 4 in the present embodiment is IC control, and temperature testing equipment 5 is thermocouple.
First ventilation pipe 101 is equipped with the second shut-off valve 9.
Second ventilation pipe 102 is equipped with regulating valve 8.
The measuring device B includes: that oxygen concentration detection device 15, high-precision pressure sensor 16 and data acquisition are set
It is standby, in which: oxygen concentration detection device 15 is connected by water supply pipe 11 with oxygen concentration detection mouth, high-precision pressure sensor 16
Be connected with sensor installation port 205, data acquisition equipment respectively with oxygen concentration detection device 15 and high-precision pressure sensor 16
It is connected.
The range of the high-precision pressure sensor 16 is 0~10bar, and precision is ± 0.5%FS hereinafter, its core
Material be titanium-sapphire diaphragm.
The water softening device 6 is connected with water supply pipe 11.
As shown in Fig. 2, the present embodiment is related to a kind of method using above-mentioned apparatus, specifically includes the following steps:
1) pass through heating warmer 3 for the first ventilation pipe 101, the second ventilation pipe 102, pressure vessel 2 and probe tube
Line 13 is heated to 100~200 degrees Celsius and maintains；
2) high temperature and high pressure steam needed for generating calibration by steam generator 7 and water softening device 6, the pressure of steam exist
1~7bar；
3) by the air and helium that are formed in standard gas tank 1 according to preset ratio n1:n2Mixed gas and above-mentioned high temperature it is high
Press steam injection pressure container；
4) opening stirs and make muddy device 207 and stirs and make muddy marked gas；
5) the oxygen purity x in pressure vessel 2 is measured followed by oxygen concentration detection device 15；
6) component of each gas: mode one is mutually authenticated with two kinds of calculations: according to oxygen purity x, calculating
The volume fraction of airThe volume fraction of heliumThe volume fraction w=1-y- of vapor
z；Mode two: the oxygen in pressure vessel 2 measured respectively by oxygen concentration detection device 15 and high-precision pressure sensor 16
Partial pressure and stagnation pressure, then pass through the temperature that temperature measurement equipment 5 measures mixed gas, finally distinguished using The Ideal-Gas Equation
Find out the ratio of three kinds of gas；
7) standard gas in pressure vessel 2 is extracted by sampling line 13 and is input to mass spectrograph 12；
8) volume fraction of air, helium and vapor is inputted into mass spectrograph 12, obtains sensitivity corresponding with three kinds of gases
Coefficient completes calibration.
Embodiment 2
As shown in figure 4, the present embodiment is compared with Example 1, pressure vessel 2 which is provided with air inlet 201, exhaust outlet 202,
Sample tap 203, the first oxygen concentration detection mouth 204, the second oxygen concentration detection mouth 208, sensor installation port 205 and the installation of TC
Mouth 206, in which: air inlet 201 is set to the top of pressure vessel 2, and exhaust outlet 202 is set to the bottom of pressure vessel 2, sampling
Mouth 203, sensor installation port 205, the installation of TC mouth 206, the first oxygen concentration detection mouth 204 and the second oxygen concentration detection mouth
208 are radially disposed on pressure vessel 2, and the second oxygen concentration detection mouth 208 and the first oxygen concentration detection mouth 204 pass through pressure vessel
2 central cross section be symmetrical arranged and sample tap 203, sensor installation port 205 and the installation of TC mouth 206 to be located at the first oxygen dense
It spends between detection mouth 204 and the second oxygen concentration detection mouth 208, sample tap 203 is connected by sampling line 13 with mass spectrograph 12.
The exhaust outlet 202 is connected with third ventilation pipe 103, which is further provided with first
Shut-off valve 17 closes exhaust outlet 202 to control exhaust outlet 202 in high pressure gas calibration, in atmosphere gas calibration, the row of opening
Port 202.
The present embodiment is related to a kind of method using above-mentioned apparatus, specifically includes the following steps:
1) pass through heating warmer 3 for the first ventilation pipe 101, the second ventilation pipe 102, pressure vessel 2 and probe tube
Line 13 is heated to 100~200 degrees Celsius and maintains；
2) high temperature and high pressure steam needed for generating calibration by steam generator 7 and water softening device 6, the pressure of steam exist
1~7bar；
3) by the air and helium that are formed in standard gas tank 1 according to preset ratio n1:n2Mixed gas be passed through 5 in pressure vessel 2
~10 minutes in wiping pressure container 2 per se with gas；
4) it opens regulating valve 8 and is passed through high temperature and high pressure steam to pressure vessel；
5) two oxygen concentration detection devices 15 are opened, respective oxygen purity X is obtained1And X2, it is ensured that the two end value
Error between 0~1%, and take the average value X of two end values；
6) component of each gas: mode one is mutually authenticated with two kinds of calculations: according to oxygen purity x, calculating
The volume fraction of airThe volume fraction of heliumThe volume fraction w=1-y- of vapor
z；Mode two: the oxygen partial pressure in pressure vessel that is measured respectively by oxygen concentration detection device and high-precision pressure sensor and
Stagnation pressure, then pass through the temperature that temperature measurement equipment 5 measures mixed gas, finally three are found out respectively using The Ideal-Gas Equation
The ratio of kind gas；
7) standard gas in pressure vessel 2 is extracted by sampling line 13 and is input to mass spectrograph 12；
8) volume fraction of air, helium and vapor is inputted into mass spectrograph 12, obtains sensitivity corresponding with three kinds of gases
Coefficient completes calibration.
The each component ratio of the standard gas can be adjusted by adjusting the amount for each gas for being passed through pressure vessel 2.
When the concentration of the object of measurement and pressure and temp change, set-up procedure 1) and 4) in temperature and logical
The pressure and temp of the vapor entered, and then meet the calibration under different condition.
Above-mentioned specific implementation can by those skilled in the art under the premise of without departing substantially from the principle of the invention and objective with difference
Mode carry out local directed complete set to it, protection scope of the present invention is subject to claims and not by above-mentioned specific implementation institute
Limit, each implementation within its scope is by the constraint of the present invention.
Claims (10)
1. a kind of mass spectrograph caliberating device of the measurement of mixed gas containing high-temperature vapor characterized by comprising interconnected
Standard gas preparation facilities and measuring device, in which: standard gas preparation facilities is connect with mass spectrograph；
The standard gas preparation facilities includes: standard gas tank, pressure vessel, temperature control equipment, water softening device and steam generation
Device, in which: standard gas tank and steam generator pass through ventilation pipe respectively and be connected with pressure vessel, water softening device and steam generation
Device is connected, and temperature control equipment is in contact with pressure vessel and ventilation pipe.
2. the apparatus according to claim 1, characterized in that the pressure vessel is hollow cavity, which is provided with air inlet
Mouth, exhaust outlet, sample tap, the first oxygen concentration detection mouth, sensor installation port and the installation of TC mouth, in which: air inlet setting
In the top of pressure vessel, exhaust outlet is set to the bottom of pressure vessel, sample tap, sensor installation port, the installation of TC mouth
It is radially disposed on pressure vessel with the first oxygen concentration detection mouth, sample tap is connected by sampling line with mass spectrograph.
3. the apparatus of claim 2, characterized in that the air inlet by three mouthfuls of pipes respectively with standard gas tank and steaming
The ventilation pipe of vapour generator is connected so that the mixed gas of standard gas tank discharge and the high-temperature vapor of steam generator discharge exist
It is pre-mixed before into pressure vessel.
4. the apparatus of claim 2, characterized in that the inside of the pressure vessel is equipped with and stirs and make muddy device to guarantee to press
Standard gas in force container uniformly mixes.
5. the apparatus of claim 2, characterized in that the pressure vessel is further provided with the detection of the second oxygen concentration
Mouth to ensure that the gas inside pressure vessel has been sufficiently mixed with the first oxygen concentration detection mouth jointly, the second oxygen concentration detection mouth
The central cross section for passing through pressure vessel with the first oxygen concentration detection mouth is symmetrical arranged and sample tap, sensor installation port and thermoelectricity
Even installing port is located near the first oxygen concentration detection mouth and the second oxygen concentration detection mouth.
6. the apparatus according to claim 1, characterized in that the temperature control equipment includes: heating warmer, temperature
Controller and temperature measurement equipment, in which: heating warmer is set in the outside wall surface of ventilation pipe and pressure vessel, and temperature is surveyed
Amount equipment is probeed into inside ventilation pipe and pressure vessel and is set near its inner surface, temperature measurement equipment and heating warmer
It is connected respectively with temperature controller.
7. the apparatus according to claim 1, characterized in that the measuring device includes: oxygen concentration detection device and height
Accuracy pressure sensor, in which: oxygen concentration detection device is connected with oxygen concentration detection mouth, high-precision pressure sensor and sensor
Installing port is connected.
8. a kind of method using any of the above-described claim described device, which is characterized in that will be ventilated by heating warmer
Pipeline, pressure vessel and sampling line are heated to preset temperature and maintain, then steam generator and water softening device are produced jointly
Raw high temperature and high pressure steam is passed through pressure vessel, and by the air formed in standard gas tank and Z gas according to the gaseous mixture of preset ratio
Then body injection pressure container using oxygen concentration detection device measures the oxygen purity in pressure vessel and by calculating
To air, the actual ratio of Z gas and vapor, the standard gas in pressure vessel is extracted finally by sampling line and is input to mass spectrum
Instrument completes calibration；
The Z gas is hybrid standard known to the stable single standard gas of chemical property or chemical property stabilization and ratio
Gas.
9. according to the method described in claim 8, it is characterized in that, the volume fraction of the airZ
The volume fraction of gasThe volume fraction w=1-y-z of vapor, in which: x is oxygen purity, n1For air institute
Account for the ratio of gas in standard gas tank, n2For the ratio of gas in standard gas tank shared by Z gas.
10. according to the method described in claim 8, it is characterized in that, the actual ratio by obtain oxygen concentration detection device
The oxygen partial pressure and stagnation pressure in pressure vessel measured respectively with high-precision pressure sensor, then measured by temperature measurement equipment
The temperature of mixed gas finally finds out the ratio of three kinds of gas respectively using The Ideal-Gas Equation.
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Cited By (5)
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| CN111220775A (en) * | 2020-01-20 | 2020-06-02 | 中国特种设备检测研究院 | Saturated or supersaturated flue gas moisture content measurement calibrating device |
| CN111929420A (en) * | 2020-07-07 | 2020-11-13 | 中煤陕西榆林能源化工有限公司 | Method and device for measuring combustible gas in steam |
| CN112185595A (en) * | 2020-09-30 | 2021-01-05 | 中国核动力研究设计院 | Online measurement system and method for steam concentration of gas-phase mixture |
| CN113813619A (en) * | 2021-10-14 | 2021-12-21 | 聚光科技(杭州)股份有限公司 | Steam generation device and method |
| CN114062277A (en) * | 2021-12-10 | 2022-02-18 | 杭州晟冠科技有限公司 | Calibration device and method for monitoring system of dissolved gas in photoacoustic spectroscopy transformer oil |
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| CN114062277A (en) * | 2021-12-10 | 2022-02-18 | 杭州晟冠科技有限公司 | Calibration device and method for monitoring system of dissolved gas in photoacoustic spectroscopy transformer oil |
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