CN102980936A - Water vapor measurement device and its method - Google Patents
Water vapor measurement device and its method Download PDFInfo
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- CN102980936A CN102980936A CN2012104345168A CN201210434516A CN102980936A CN 102980936 A CN102980936 A CN 102980936A CN 2012104345168 A CN2012104345168 A CN 2012104345168A CN 201210434516 A CN201210434516 A CN 201210434516A CN 102980936 A CN102980936 A CN 102980936A
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Abstract
The invention provides a water vapor measurement device. The device comprises: a first gas source communicated with a mass spectrometer; a second gas source communicated with the inside of a water container, wherein the water container has an inlet and an outlet, the inlet is communicated with the second gas source, and the outlet is communicated with the mass spectrometer; a first calculating module used for obtaining a water vapor concentration according to an ion signal intensity sent by the mass spectrometer and corresponding to a second gas; a model establishing module used for obtaining the measurement model of the water vapor concentration according to the water vapor concentration obtained by the first calculating module, and ion signal intensity sent by the mass spectrometer and corresponding to the water vapor; and a second calculating module used for obtaining the concentration of water vapor to be measured according to the ion signal intensity sent by the mass spectrometer and corresponding to the water vapor to be measured and the measurement model. The water vapor measurement device has the advantages of accuracy, rapidness, stability, low measurement cost and the like.
Description
Technical field
The present invention relates to gasmetry, particularly water vapor measurement mechanism and method.
Background technology
In part industrial process gas detects, need to measure the water vapour content in the mixed gas.At present, mass spectrometer can't be set up effective water vapor quantitative model owing to can't obtain effective water vapor gas in measuring fragment coefficient and modeling process.Following form has provided as creating the interface of quantitative curve.
Step | Title | O 2(I 16) | H 2O(I 18) | N 2(I 28) | CO 2I 44 |
1 | Background signal 1 | 0.00000e0 | 0.00000e0 | 0.00000e0 | 0.00000e0 |
2 | Fragment (H 2O) | 0.110000 | 1.000000 | 0 | 0 |
3 | Fragment (CO 2) | 0.090000 | 0 | 0.110000 | 1.000000 |
4 | Gas 1 | 0.00000e0 | 0.00000e0 | 0.00000e0 | 0.00000e0 |
Each row information interpretation is as follows in the form 1: what show in the 1st row is background (noise signal) signal of an ion, and instrument is measured this signal when passing into background gas (such as Ar).The 2nd row and the 3rd behavior fragment ion are capable, show respectively H
2O and CO
2The fragmention signal passes into respectively pure H at instrument
2O, and CO
2In time, measure, and measures the fragmention signal and be used for calculating the fragment coefficient.The 4th behavior gas is capable, records each quota ion signal intensity when passing into the one bottle of mixing gas that comprises all tested gases, is stored in the matrix, is used for calculating relative calibration factor R S.
The main deficiency that technique scheme exists is:
1, the gas of water is bad obtains, and can't set up the fragmention coefficient of water, can't effectively deduct the water vapor intersection and disturb.
2, mix the steam that accurately to make up water in the gas and do mixed mark, can not set up effective water vapor quantitative model.
3, because mass spectrometer adopts is inner normalization method, if can not measure water vapor, then cause in the detected sample gas water vapor concentration value to be shared equally other components by equal proportion, affect measurement accuracy.
In order to overcome above-mentioned deficiency, following solution has been proposed in the prior art: air is passed in the mass spectrometer, before passing into mass spectrometer, record temperature and the relative humidity of air, calculate contained water vapor concentration in the air, thus calibrating mass spectrometry.The main deficiency that this solution exists is:
1, air is at indoor moveable, and it is unstable to enter mass spectrometric water vapour content;
2, the air themperature fluctuation is larger on the impact of water vapor concentration calculated value, and air themperature is wayward;
3, quantitatively required m/z18 quota ion of water may be contained in some chemical plant, the potpourri that comprises in the air, and it is inaccurate to cause measuring fragment coefficient and quantitative model.
Summary of the invention
In order to solve the deficiency in the above-mentioned prior art scheme, the invention provides a kind of accurately, fast, stable, the device and method of measuring the low measurement water vapor of cost.
The objective of the invention is to be achieved through the following technical solutions:
A kind of water vapor measurement mechanism comprises mass spectrometer, and described measurement mechanism also comprises:
The first gas source of the gas, described the first gas source of the gas is communicated with mass spectrometer;
The second gas source of the gas, described the second gas source of the gas are communicated with the inner and described mass spectrometer of tank;
Tank, described tank has import and outlet, and described import is communicated with described the second gas source of the gas, and described outlet is communicated with described mass spectrometer;
The first computing module, the ion signal intensity corresponding to the second gas that described the first computing module is used for sending according to described mass spectrometer draws water vapor concentration;
What water vapor concentration, the mass spectrometer that model building module, described model building module are used for drawing according to the first computing module sent draws the measurement model of water vapor concentration corresponding to the ion signal intensity of water vapor;
The second computing module, described the second computing module is used for the ion signal intensity corresponding to water vapor to be measured that sends according to mass spectrometer, the concentration that described measurement model draws water vapor to be measured.
According to above-mentioned measurement mechanism, alternatively, described measurement mechanism further comprises:
Companion's thermal modules, described companion's thermal modules is arranged on the pipeline between described tank and the mass spectrometer.
According to above-mentioned measurement mechanism, preferably, the concentration of the water vapor in described the first gas and/or the second gas is lower than 0.01%.
According to above-mentioned measurement mechanism, preferably, described the first gas is nitrogen.
According to above-mentioned measurement mechanism, preferably, described the second gas is argon gas.
Purpose of the present invention also is achieved by the following technical programs:
A kind of water vapor measuring method, described measuring method may further comprise the steps:
(A1) the first gas, the second gas are passed into respectively in the mass spectrometer, obtain respectively the ion signal intensity I corresponding to the second gas
0, I
1
(A2) described the second gas is carrying water vapor and is entering in the described mass spectrometer, obtains the ion signal intensity I corresponding to the second gas
2, corresponding to the ion signal intensity of water vapor
And corresponding to the fragment coefficient of the fragmention signal intensity of water vapor;
(A4) utilize described measurement model to process the ion signal intensity corresponding to water vapor to be measured that described mass spectrometer records, thereby know the concentration of water vapor to be measured.
According to above-mentioned measuring method, alternatively, in described step (A1), also obtain in the first gas or the second gas ion signal intensity corresponding to water vapor
(A3) utilize described
The fragment coefficient is set up the water vapor concentration measurement model.
According to above-mentioned measuring method, preferably, in described step (A1) and/or the step (A2), calculate the relative standard deviation RSD value of all ion signal intensity I that within the some time, record, if less than threshold value, recording, described RSD value also preserves I.
According to above-mentioned measuring method, preferably, the described some time is in the final stage of ventilation.
According to above-mentioned measuring method, preferably, the described some time is not less than 1 minute, and described threshold value is not more than 3%.
According to above-mentioned measuring method, preferably, in described step (A2), described the second gas is passed in the water, thereby so that the second gas carries water vapor.
According to above-mentioned measuring method, alternatively, in described step (A2), carry the second gas of water vapor and accompanied heat.
According to above-mentioned measuring method, preferably, the concentration of the water vapor in described the first gas and/or the second gas is lower than 0.01%.
According to above-mentioned measuring method, preferably, described the first gas is nitrogen.
According to above-mentioned measuring method, preferably, described the second gas is argon gas.
Compared with prior art, the beneficial effect that has of the present invention is:
1, the second gas passes in the water, thereby so that carry water vapor, the recycling mass spectrometer is measured this water vapor concentration, and then so that above-mentioned water vapor becomes gas, as seen, the generation of this gas is not subjected to the impact of ambient air, humidity variation, variation of ambient temperature, and gas is more stable;
2, since the water vapor gas adopt totally-enclosed form (tank), be not subjected to the interference of other compound in the environment, the fragment coefficient is measured and model set up more accurate;
3, computing module and model building module can adopt software (can also be circuit or other implementation) automatically to control and calculate, and needn't additionally increase thermometer and hygronom, and easy and simple to handle, integrated cost is low, failure rate is low.
Description of drawings
With reference to accompanying drawing, disclosure of the present invention will be easier to understand.Those skilled in the art are understood that easily: these accompanying drawings only are used for illustrating technical scheme of the present invention, and are not to be intended to protection scope of the present invention is construed as limiting.Among the figure:
Fig. 1 is the structure diagram according to the measurement mechanism of the embodiment of the invention 1;
Fig. 2 is the process flow diagram according to the measuring method of the embodiment of the invention 1;
Fig. 3 is the process flow diagram according to the measuring method of the embodiment of the invention 2.
Embodiment
Fig. 1-3 and following declarative description optional embodiment of the present invention how to implement with instruction those skilled in the art and reproduce the present invention.In order to instruct technical solution of the present invention, simplified or omitted some conventional aspects.Those skilled in the art should understand that the modification that is derived from these embodiments or replace will be within the scope of the invention.Those skilled in the art should understand that following characteristics can make up to form a plurality of modification of the present invention in every way.Thus, the present invention is not limited to following optional embodiment, and is only limited by claim and their equivalent.
Embodiment 1:
Fig. 1 has schematically provided the structure diagram that is applied in the standard water vapour measurement device in the mass spectrometer of the embodiment of the invention, and as shown in Figure 1, described measurement mechanism comprises:
The first gas source of the gas, described the first gas source of the gas is communicated with mass spectrometer;
The second gas source of the gas, it is inner that described the second gas source of the gas is communicated with tank; Preferably, the concentration of the water vapor in described the first gas and/or the second gas is lower than 1%.As, the first gas is that concentration is 99.999% nitrogen, the second gas is that concentration is 99.999% argon gas.
Tank, described tank has import and outlet, and described import is communicated with described the second gas source of the gas, and described outlet is communicated with described mass spectrometer and standard water vapour measurement mouth;
The first computing module, the ion signal intensity corresponding to the second gas that described the first computing module is used for sending according to described mass spectrometer draws water vapor concentration; Described the first computing module adopts circuit or software to realize that specific implementation is prior art for a person skilled in the art, is not need to pay creative work.
What water vapor concentration, the mass spectrometer that model building module, described model building module are used for drawing according to the first computing module sent draws the measurement model of water vapor concentration corresponding to the ion signal intensity of water vapor; Described model building module adopts circuit or software to realize that specific implementation is prior art for a person skilled in the art, is not need to pay creative work.
The second computing module, described the second computing module is used for the ion signal intensity corresponding to water vapor to be measured that sends according to mass spectrometer, the concentration that described measurement model draws water vapor to be measured.Described the second computing module adopts circuit or software to realize that specific implementation is prior art for a person skilled in the art, is not need to pay creative work.
According to above-mentioned measurement mechanism, alternatively, in order to guarantee the stable of water vapour content in the gas transmission pipeline, the pipeline between described tank and mass spectrometer arranges companion's thermal modules.
Fig. 2 has schematically provided the process flow diagram that is applied in the standard water vapour measurement method in the mass spectrometer of the embodiment of the invention, has specifically used above-mentioned measurement mechanism, and as shown in Figure 2, described measuring method may further comprise the steps:
(A1) the first gas, the second gas are passed into respectively in the mass spectrometer, obtain respectively the ion signal intensity I corresponding to the second gas
0, I
1Preferably, the concentration of the water vapor in described the first gas and/or the second gas is lower than 0.01%.As, the first gas is that concentration is 99.998% nitrogen, the second gas is that concentration is 99.998% argon gas.
(A2) described the second gas is carrying water vapor and is entering in the described mass spectrometer, obtains the ion signal intensity I corresponding to the second gas
2, corresponding to the ion signal intensity of water vapor
And corresponding to the fragment coefficient of the fragmention signal intensity of water vapor;
The concentration of the water vapor that carries in the first gas and the second gas in the described step (A1) all is not more than described concentration
0.01 times;
Preferably, in described step (A1) and/or the step (A2), calculate the relative standard deviation RSD value of all ion signal intensity I that within the some time, record, also preserve I if described RSD value less than threshold value, records.
According to above-mentioned measuring method, preferably, the described some time is in the final stage of ventilation, and the described some time is not less than 1 minute, and described threshold value is not more than 3%.Above-mentioned some time and threshold value are thought setting according to the needs, the mass spectrometric detectability that detect.
(A3) utilize described
Coefficient is set up the water vapor concentration measurement model; The concrete mode that model is set up is the state of the art, does not repeat them here;
(A4) utilize described measurement model to process the ion signal intensity corresponding to water vapor to be measured that described mass spectrometer records, thereby know the concentration of water vapor to be measured.
Preferably, in described step (A2), described the second gas is passed in the water, thereby so that the second gas carries water vapor.
Alternatively, in described step (A2), carry the second gas of water vapor and accompanied heat.
Embodiment 2:
Fig. 3 has schematically provided the process flow diagram that is applied in the standard water vapour measurement method in the mass spectrometer of the embodiment of the invention, has specifically used above-mentioned measurement mechanism, and as shown in Figure 3, described measuring method may further comprise the steps:
(A1) the first gas, the second gas are passed into respectively in the mass spectrometer, obtain respectively the ion signal intensity I corresponding to the second gas
0, I
1, also obtain in the second gas the ion signal intensity corresponding to water vapor
The concentration of the water vapor in described the first gas and/or the second gas is lower than 0.01%.As, the first gas is that concentration is 99.991% nitrogen, the second gas is that concentration is 99.991% argon gas;
(A2) described the second gas is passed in the tank, discharges afterwards, is carrying second of water vapor and is being accompanied heat to enter in the described mass spectrometer, obtains the ion signal intensity I corresponding to the second gas
2, corresponding to the ion signal intensity of water vapor
And corresponding to the fragment coefficient of the fragmention signal intensity of water vapor;
The concentration of the water vapor that carries in the first gas and the second gas in the described step (A1) all is not more than described concentration
0.01 times;
Preferably, in described step (A1) and/or the step (A2), calculate the relative standard deviation RSD value of all ion signal intensity I that within the some time, record, also preserve I if described RSD value less than threshold value, records.
According to above-mentioned measuring method, preferably, the described some time is in the final stage of ventilation, and the described some time is not less than 1 minute, and described threshold value is not more than 3%.
(A3) utilize described
The fragment coefficient is set up the water vapor concentration measurement model; The concrete mode that model is set up is the state of the art, does not repeat them here;
(A4) utilize described measurement model to process the ion signal intensity corresponding to water vapor to be measured that described mass spectrometer records, thereby know the concentration of water vapor to be measured.
Embodiment 3:
Measurement mechanism and the application examples of method in the ethene preparing ethylene glycol according to the embodiment of the invention 1.Concrete preparation process is: utilize ethene to make oxirane, oxirane reacts with water again, thereby makes ethylene glycol.In order to improve preparation efficiency, to reduce production costs, need the content of water in the monitoring preparation process.
In this application examples, the first gas adopts high pure nitrogen, and concentration is 99.999%.The second gas adopts high-purity argon gas, and concentration is that water vapour content is starkly lower than 0.01% in 99.999%, the first gas and the second gas.When the first gas and the second gas are passed into mass spectrometer, corresponding to the ion signal intensity (ground unrest) of water vapor
Very little, and mass spectrometric ground unrest is less than 1 * 10
-13, therefore described
Can ignore.Therefore, when setting up measurement model, no longer consider described
Impact.Some time is 2 minutes, and threshold value is 1%.The second gas is passed in the airtight tank, thereby so that the second gas carries water vapor; Simultaneously, companion's heat carries the second gas of water vapor.
Embodiment 4:
Measurement mechanism and the application examples of method in the ethene preparing ethylene glycol according to the embodiment of the invention 2.Concrete preparation process is: utilize ethene to make oxirane, oxirane reacts with water again, thereby makes ethylene glycol.In order to improve preparation efficiency, to reduce production costs, need the content of water in the monitoring preparation process.
In this application examples, the first gas adopts high pure nitrogen, and concentration is 99.991%.The second gas adopts high-purity argon gas, and concentration is that water vapour content is lower than 0.01% in 99.991%, the first gas and the second gas.When the first gas and the second gas are passed into mass spectrometer, corresponding to the ion signal intensity (ground unrest) of water vapor
No longer ignore, when setting up measurement model, need consider described
Impact.
Above-described embodiment only is that exemplarily to have provided the first gas be nitrogen, and the second gas is argon gas, can also be other gases certainly, and as being respectively argon gas, helium etc. when the first gas, the second gas is nitrogen etc.This it will be apparent to one skilled in the art that, is lower than in 0.01% the situation satisfying the first gas and the second gas water vapor concentration, and the selection of the first gas and the second gas is predictable.
Claims (10)
1. the measurement mechanism of a water vapor comprises mass spectrometer, and described measurement mechanism also comprises:
The first gas source of the gas, described the first gas source of the gas is communicated with mass spectrometer;
The second gas source of the gas, described the second gas source of the gas are communicated with the inner and described mass spectrometer of tank;
Tank, described tank has import and outlet, and described import is communicated with described the second gas source of the gas, and described outlet is communicated with described mass spectrometer;
The first computing module, the ion signal intensity corresponding to the second gas that described the first computing module is used for sending according to described mass spectrometer draws water vapor concentration;
What water vapor concentration, the mass spectrometer that model building module, described model building module are used for drawing according to the first computing module sent draws the measurement model of water vapor concentration corresponding to the ion signal intensity of water vapor;
The second computing module, described the second computing module is used for the ion signal intensity corresponding to water vapor to be measured that sends according to mass spectrometer, the concentration that described measurement model draws water vapor to be measured.
2. measurement mechanism according to claim 1, it is characterized in that: described measurement mechanism further comprises:
Companion's thermal modules, described companion's thermal modules is arranged on the pipeline between described tank and the mass spectrometer.
3. measurement mechanism according to claim 1, it is characterized in that: the concentration of the water vapor in described the first gas and/or the second gas is lower than 0.01%.
4. water vapor measuring method, described measuring method may further comprise the steps:
(A1) the first gas, the second gas are passed into respectively in the mass spectrometer, obtain respectively the ion signal intensity I corresponding to the second gas
0, I
1
(A2) described the second gas is carrying water vapor and is entering in the described mass spectrometer, obtains the ion signal intensity I corresponding to described the second gas
2, corresponding to the ion signal intensity of water vapor
And corresponding to the fragment coefficient of the fragmention signal intensity of water vapor;
(A3) utilize described
The fragment coefficient is set up the water vapor concentration measurement model;
(A4) utilize described measurement model to process the ion signal intensity corresponding to water vapor to be measured that described mass spectrometer records, thereby know the concentration of water vapor to be measured.
6. according to claim 4 or 5 described measuring methods, it is characterized in that: in described step (A1) and/or step (A2), the relative standard deviation RSD value of all ion signal intensity I that calculating recorded within the some time is also preserved I if described RSD value less than threshold value, records.
7. measuring method according to claim 6, it is characterized in that: the described some time is in the final stage of ventilation.
8. measuring method according to claim 6, it is characterized in that: the described some time is not less than 1 minute, and described threshold value is not more than 3%.
9. measuring method according to claim 4, it is characterized in that: in described step (A2), described the second gas is passed in the water, thereby so that the second gas carries water vapor.
10. measuring method according to claim 4, it is characterized in that: in described step (A1), the concentration of the water vapor in described the first gas and/or the second gas is lower than 0.01%.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109856298A (en) * | 2019-02-25 | 2019-06-07 | 上海交通大学 | The mass spectrograph caliberating device and method of the measurement of mixed gas containing high-temperature vapor |
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EP0469437A1 (en) * | 1990-07-25 | 1992-02-05 | Hitachi, Ltd. | Method of and apparatus for preparing calibration gas |
JPH04249056A (en) * | 1991-02-04 | 1992-09-04 | Seiko Instr Inc | Mass-spectrometric device using induction coupling plasma with heating and gasification |
JP2000275217A (en) * | 1999-03-24 | 2000-10-06 | Hitachi Ltd | Forming method and device for calibration curve with mass spectrometer |
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2012
- 2012-11-05 CN CN201210434516.8A patent/CN102980936B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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EP0469437A1 (en) * | 1990-07-25 | 1992-02-05 | Hitachi, Ltd. | Method of and apparatus for preparing calibration gas |
JPH04249056A (en) * | 1991-02-04 | 1992-09-04 | Seiko Instr Inc | Mass-spectrometric device using induction coupling plasma with heating and gasification |
JP2000275217A (en) * | 1999-03-24 | 2000-10-06 | Hitachi Ltd | Forming method and device for calibration curve with mass spectrometer |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109856298A (en) * | 2019-02-25 | 2019-06-07 | 上海交通大学 | The mass spectrograph caliberating device and method of the measurement of mixed gas containing high-temperature vapor |
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