CN220455273U - CO for ambient air 2 And CH (CH) 4 Gas marking value setting device - Google Patents
CO for ambient air 2 And CH (CH) 4 Gas marking value setting device Download PDFInfo
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- CN220455273U CN220455273U CN202321819106.5U CN202321819106U CN220455273U CN 220455273 U CN220455273 U CN 220455273U CN 202321819106 U CN202321819106 U CN 202321819106U CN 220455273 U CN220455273 U CN 220455273U
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- 239000012080 ambient air Substances 0.000 title claims description 15
- 238000002347 injection Methods 0.000 claims abstract description 21
- 239000007924 injection Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003908 quality control method Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007789 gas Substances 0.000 abstract description 143
- 230000000694 effects Effects 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 70
- 229910002092 carbon dioxide Inorganic materials 0.000 description 35
- 239000001569 carbon dioxide Substances 0.000 description 35
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000003570 air Substances 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 4
- 238000012937 correction Methods 0.000 description 4
- 238000010812 external standard method Methods 0.000 description 4
- 239000005431 greenhouse gas Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000012417 linear regression Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000007430 reference method Methods 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The utility model discloses a method for using environmental air CO 2 And CH (CH) 4 The device comprises a first gas storage component, a second gas storage component, a third gas storage component and a fourth gas storage component which are respectively used for introducing each level of standard gas, standard gas to be fixed, quality control standard gas and reference gas; the first gas storage assembly, the second gas storage assembly and the third gas storage assembly are connected with sample injection selection valves for switching and selecting different standard gas samples; fourth gas storage component and sample injection selector valve are connectedThe four-way two-position valve for switching the sequential alternate entry of the reference gas and the standard gas is arranged, and the outlet end of the four-way two-position valve is connected with CO 2 /CH 4 High-precision spectrometer and CO 2 Isotope spectrometer. The device can reduce the use amount of the high-level standard gas, and can realize that the upper-level standard gas, the reference gas, the standard gas to be fixed value and the like are automatically switched into the analyzer according to the program. The method is suitable for correcting the isotope discrimination effect when the isotope content of different standard gases is different, and ensures the accuracy of the standard gas calibration value.
Description
Technical Field
The utility model relates to the technical field of standard gas constant value, in particular to a standard gas constant value device for CO in ambient air 2 And CH (CH) 4 And a device for calibrating the standard gas.
Background
Climate change crisis is one of the major problems facing today's human society, atmospheric carbon dioxide (CO 2 ) Methane (CH) 4 ) The increased concentration of iso-greenhouse gases is a major cause of global warming. The concentration of greenhouse gases in the atmosphere is monitored from the beginning around the sixties of the last century abroad, and monitoring networks of different scales such as global-regional-national-urban and the like are gradually formed. Currently, the World Meteorological Organization (WMO) has built the world-wide maximum, most functional international atmospheric greenhouse gas monitoring network (GAW), in which the background greenhouse gas monitoring sites of the meteorological department of our country are also in. To ensure the comparability of the data of each monitoring site of GAW, WMO sets up a data quality target, CO 2 The comparative target in the northern hemisphere was 0.1. Mu. Mol/mol (comparative target in the southern hemisphere was 0.05 ppm), CH 4 The comparability target was 2nmol/mol.
At present, china also provides requirements for data quality of urban atmospheric temperature chamber gas monitoring, and CO 2 And CH (CH) 4 Drift data between two calibrations of the instrument of (a) is not more than 0.2ppm and 5ppb. In order to meet the strict data quality target, a high-precision magnitude traceability system and accurate value determination of standard gas are particularly important. In the prior art, when the magnitude is transmitted, the direct external standard method is generally adopted to scale the value standard gas step by step, but the direct external standard method has larger consumption of the high-level standard gas. Stable isotope content of different standard gasesThe difference also affects the result of the high-precision calibration of the standard gas.
Disclosure of Invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present utility model to provide a method for ambient air CO 2 And CH (CH) 4 The gas calibration device can reduce the use amount of high-level gas calibration and ensure the accuracy of gas calibration.
In order to achieve the aim of the utility model, the utility model adopts the following technical scheme:
providing a method for ambient air CO 2 And CH (CH) 4 The gas calibration device comprises a first gas storage component, a second gas storage component, a third gas storage component and a fourth gas storage component which are respectively used for introducing each level of gas, gas to be calibrated, quality control gas and reference gas; the first gas storage assembly, the second gas storage assembly and the third gas storage assembly are connected with sample injection selection valves for switching and selecting different standard gas samples; the fourth gas storage component and the sample injection selection valve are connected with a four-way two-position valve for switching the sequential alternate entry of the reference gas and the standard gas, and the outlet end of the four-way two-position valve is connected with CO 2 /CH 4 High-precision spectrometer and CO 2 Isotope spectrometer.
Further, the first gas storage assembly, the second gas storage assembly and the third gas storage assembly are respectively connected with a first multi-channel switching valve, a second multi-channel switching valve and a third multi-channel switching valve, and the first multi-channel switching valve, the second multi-channel switching valve and the third multi-channel switching valve are connected with the sampling selection valve.
Further, a first control module is arranged between the sample injection selection valve and the four-way two-position valve, a second control module is arranged between the fourth gas storage assembly and the four-way two-position valve, and the first control module and the second control module both comprise an electronic pressure controller and a mass flowmeter.
Further, a four-way two-position valve and CO 2 /CH 4 High-precision spectrometer, four-way two-position valve and CO 2 A water removal unit is arranged between the isotope spectrometers.
Further, the water removal unit is a cold trap.
Further, the constant value device also comprises a first three-way valve, a second three-way valve, a third three-way valve, an idle gas storage component, a third three-way valve, a first three-way valve and CO 2 /CH 4 The high-precision spectrometer is communicated, and a third three-way valve, a second three-way valve and CO 2 The isotope spectrometer is communicated.
The beneficial effects of the utility model are as follows:
1. the device can reduce the use amount of the high-level standard gas, and can realize that the upper-level standard gas, the reference gas, the standard gas to be fixed value and the like are automatically switched into the analyzer according to the program.
2. The method is suitable for correcting the isotope discrimination effect when the isotope content of different standard gases is different, and ensures the accuracy of the standard gas calibration value.
Drawings
FIG. 1 is a schematic diagram of the structure of the device of the present utility model;
FIG. 2 is a schematic diagram of CO provided by an embodiment of the present utility model 2 A regression curve schematic diagram;
wherein: 1. a first gas storage assembly; 2. a second gas storage assembly; 3. a third gas storage assembly; 4. a fourth gas storage assembly; 5. a first multi-channel switching valve; 6. a second multi-channel switching valve; 7. a third multi-channel switching valve; 8. a sample injection selection valve; 9. a first control module; 10. a second control module; 11. a four-way two-position valve; 12. a first cold trap; 13. a second cold trap; 14. a first three-way valve; 15. a second three-way valve; 16. a third three-way valve; 17. CO 2 /CH 4 A high-precision spectrometer; 18. CO 2 An isotope spectrometer; 19. a drying tube; 20. and (5) idling the gas storage assembly.
Detailed Description
The following description of the embodiments of the present utility model is provided to facilitate understanding of the present utility model by those skilled in the art, but it should be understood that the present utility model is not limited to the scope of the embodiments, and all the utility models which make use of the inventive concept are protected by the spirit and scope of the present utility model as defined and defined in the appended claims to those skilled in the art.
Examples
Referring to FIG. 1, a system for ambient air CO 2 And CH (CH) 4 The gas calibration device comprises a first gas storage component 1, a second gas storage component 2, a third gas storage component 3 and a fourth gas storage component 4 which are respectively used for introducing each level of gas calibration, gas calibration to be calibrated, quality control gas calibration and reference gas. The quality control standard gas is used as a gas to be measured with known concentration to be measured for periodic and repeated measurement and is used for evaluating the running state of the detection system. The standard gas of each level is the standard gas of each level such as a first level and a second level, the standard gas of the first level and the second level is a series of standard gases with different concentrations of the last level of the standard gas to be fixed value in the magnitude tracing system, the reference gas is the standard gas with stable magnitude, the quality control standard gas is the standard gas with accurate fixed value, and the standard gas to be fixed value is the standard gas without utilizing the fixed value of the last level of standard gas.
The first gas storage assembly 1, the second gas storage assembly 2 and the third gas storage assembly 3 are respectively connected with a first multi-channel switching valve 5, a second multi-channel switching valve 6 and a third multi-channel switching valve 7, and the first multi-channel switching valve 5, the second multi-channel switching valve 6 and the third multi-channel switching valve 7 are connected with a sample injection selection valve 8. Wherein, the multi-channel switching valve 5/6/7 is a multi-position convolution electromagnetic valve for switching and selecting different standard gas channels for sample injection; the sample injection selector valve 8 is used for switching different multi-channel switching valves, typically four-channel multi-position selector valves or solenoid valves.
The fourth gas storage component 4 and the sample injection selection valve 8 are connected with a four-way two-position valve 11 for switching the sequential alternate entry of the reference gas and the standard gas, and the outlet end of the four-way two-position valve 11 is connected with CO 2 /CH 4 High-precision spectrometer 17, CO 2 Isotope spectrometer 18.
As a preferable mode, a first control module 9 is arranged between the sample injection selection valve 8 and the four-way two-position valve 11, a second control module 10 is arranged between the fourth gas storage assembly 4 and the four-way two-position valve 11, and the first control module 9 and the second control module 10 both comprise an electronic pressure controller and a mass flowmeter. The electronic pressure controller is used for maintaining pressure stability, and the mass flowmeter is used for controlling the flow of gas entering the analyzer to be stable.
Four-way two-position valve 11 and CO 2 /CH 4 A first cold trap 12, a four-way two-position valve 11 and CO are arranged between the high-precision spectrometers 17 2 A second cold trap 13 is arranged between the isotope spectrometers 18. The method is used for removing moisture in the standard gas, the dew point of the standard gas is not higher than-70 ℃, and when the dew point temperature of the standard gas is lower than-70 ℃, a water removal system can be omitted; CO 2 /CH 4 High-precision analyzer 17 performance index CO 2 Nominal interval is 350-600 mu mol/mol, CO 2 Measuring the average concentration precision (within 2 hours) of less than or equal to 0.025 mu mol/mol and CH within 5 minutes 4 Nominal interval is 1300-4000 nmol/mol, CH 4 The average concentration precision (within 2 hours) of 5 minutes is less than or equal to 0.25nmol/mol. CO 2 High-precision co-located spectrum analyzer 18 performance index delta 13 The average precision of C measurement for 10 seconds is less than or equal to 0.025 per mill, delta 18 The average precision of O measurement for 10 seconds is less than or equal to 0.025 per mill.
As a preferable mode, the constant value device also comprises a first three-way valve 14, a second three-way valve 15, a third three-way valve 16, an idle gas storage component 20, a third three-way valve 16, a first three-way valve 14 and CO 2 /CH 4 The high-precision spectrometer 17 is communicated with a third three-way valve 16, a second three-way valve 15 and CO 2 The isotope spectrometer 18 is in communication. When the instrument is idle for a short time, dry synthetic air can be introduced as idle air, and when the instrument is idle for a long time, indoor air dehydrated through the nafion drying pipe 19 can be introduced as idle air to maintain the state of the instrument.
The method for carrying out the value setting by using the device comprises the following steps:
step 1, preparing upper-level standard gas and standard gas to be fixed value, wherein the upper-level standard gas comprises five concentration points and is marked as CS 1 、CS 2 、CS 3 、CS 4 、CS 5 The method comprises the steps of carrying out a first treatment on the surface of the Preparing a reference gas;
step 2, according to CS 1 Reference gas, CS 1 Reference gas, CS 1 Sequentially setting a sample injection sequence of the reference gas, setting the sample injection time of each bottle of gas to be 6min, and circulating for 8 times;
step 3, sequentially completing CS according to the sequence of the step 2 2 、CS 3 、CS 4 、CS 5 Is introduced into the sample;
step 4, analyzing the spectrum after sample injection;
step 5, taking instrument indication values of 4min30s-5min30s of each sample injection to calculate an average value, and taking an average value of 8 times of circulation;
step 6, calculating the magnitude of the standard gas to be fixed value through reference method curve regression;
specifically, the upper level standard gas CS 1 、CS 2 、CS 3 、CS 4 、CS 5 The concentration certificate value is taken as an ordinate, and the upper standard gas CS calculated in the step 5 is extracted 1 、CS 2 、CS 3 、CS 4 、CS 5 The average value of the indication value of 8 cycles/the average value of the reference indication value of 8 cycles is taken as the abscissa, linear regression is carried out to obtain the slope k and the intercept b, the average value of the indication value of the standard indication value to be fixed (the average value is calculated by taking the instrument indication value of 4min30s-5min30s of each sample injection, the average value of 8 cycles is taken, and the average value of the standard indication value and CS are combined 1 -CS 5 And substituting the average value of the reference gas indication value into the regression curve to calculate the magnitude of the standard gas to be fixed value, wherein the calculation formula is as follows: c=k×r+b
Wherein: c=standard concentration of target in target gas to be calibrated;
r=average value of the ratio of the standard gas spectrum indication value to be fixed value or the upper standard gas spectrum indication value to the adjacent reference gas spectrum indication value;
k = slope of linear regression equation;
b = intercept of linear regression equation.
And 7, performing an isotope discrimination effect correction algorithm on the constant value result obtained by the regression calculation to obtain a final constant value result.
Specifically, δ 13 CVPDB and delta 18 The OVPDB can be measured by an isotope mass spectrometer or an isotope spectrometer, an isotope discrimination effect correction algorithm is provided, and calculation is performed 16 O 12 C 16 O occupies total CO 2 Ratio P (626);
wherein:
δ 17 O＝0.528·δ 18 O
standard concentration C and upper level standard gas measured based on high-precision spectrum comparison method according to standard gas to be fixed value 16 O 12 C 16 O proportion P 1 (626) And CO of standard gas to be fixed 2 (626) Proportion P 2 (626) Calculating CO after correction of standard gas isotope with to-be-fixed value 2 Concentration C revise ；
C revise ＝C×P1(626)/P2(626)
C-calculating the concentration of the standard gas to be fixed value based on a reference external standard method;
P 1 (626) -upper level standard gas C 1-5 A kind of electronic device 16 O 12 C 16 O ratio;
P 2 (626) -gas calibration to be fixed W 1-3 A kind of electronic device 16 O 12 C 16 O ratio;
CH in standard gas 4 And CH in ambient air 4 Stable isotope ratio is relatively close to CH 4 The isotopic effect of (c) is less and negligible.
The standard bottom gas used in the embodiment of the utility model is ambient air, and the target compounds are carbon dioxide and methane. The regression curve is shown in FIG. 2, the slope k of the curve is 387.216, the intercept b is 0.9031, the standard gas concentration to be determined is 425.33 mu mol/mol by substituting the standard gas indicating value to be determined/reference gas indicating value into calculation, the result is shown in Table 1, the isotope discrimination effect correction is carried out on the regression result, and the final fixed value result is 425.44 mu mol/mol.
Table 1 reference method for calculating fixed values
| Mean value of indication value | Average value of reference gas indication value | Standard gas indication value/reference gas indication value | Certificate value/fixed value | |
| CS1 | 495.1156667 | 385.4297016 | 1.284580987 | 498.28 |
| CS2 | 434.0708841 | 385.4252417 | 1.126212913 | 436.93 |
| CS3 | 369.6188907 | 385.4213029 | 0.95899964 | 372.33 |
| CS4 | 594.7965354 | 385.4736827 | 1.54302761 | 598.43 |
| CS5 | 399.3670609 | 385.4301765 | 1.036159297 | 402.09 |
| Preparation of gas | 422.4253502 | 385.3859919 | 1.096109768 | 425.33 |
The utility model provides a method for preparing carbon dioxide (CO) suitable for environmental air 2 ) Methane (CH) 4 ) A high-precision standard gas value setting device and a method. The utility model can reduce the consumption of high-level standard gas, and can realize that the upper-level standard gas, the reference gas, the standard gas to be fixed value and the like are automatically switched into the analyzer according to the program. The method is suitable for correcting the isotope discrimination effect when the isotope content of different standard gases is different, and ensures the accuracy of the standard gas calibration value. The utility model uses the reference external standard method to carry out the calibration, the precision of the calibration result is good, the accuracy is high, the operation is convenient, the utility model can be used for the calibration of standard gas, the long-term stability is good, the use of superior standard gas can be greatly saved, and the utility model can be used for CO in the ambient air 2 And CH (CH) 4 Is significant for magnitude tracing and transmission of the number.
It will be evident to those skilled in the art that the utility model is not limited to the details of the foregoing illustrative embodiments, and that the present utility model may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the utility model being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (6)
1. CO for ambient air 2 And CH (CH) 4 The gas calibration device is characterized by comprising a first gas storage component (1), a second gas storage component (2), a third gas storage component (3) and a fourth gas storage component (4) which are respectively used for introducing each level of gas, gas to be calibrated, quality control gas and reference gas; the first gas storage assembly (1), the second gas storage assembly (2) and the third gas storage assembly (3) are connected with sample injection selection valves (8) for switching and selecting different standard gas sample injections; the fourth gas storage component (4) and the sample injection selection valve (8) are connected with a four-way two-position valve (11) for switching the sequential alternate entry of the reference gas and the standard gas, and the outlet end of the four-way two-position valve (11) is connected with CO 2 /CH 4 High-precision spectrometer (17) and CO 2 Isotope spectrometer (18).
2. For ambient air CO according to claim 1 2 And CH (CH) 4 The gas marking and setting device is characterized in that a first gas storage component (1), a second gas storage component (2) and a third gas storage component (3) are respectively connected with a first multichannel switching valve (5), a second multichannel switching valve (6) and a third multichannel switching valve (7), and the first multichannel switching valve (5), the second multichannel switching valve (6) and the third multichannel switching valve (7) are connected with a sample injection selection valve (8).
3. For ambient air CO according to claim 1 2 And CH (CH) 4 The gas marking and setting device is characterized in that a first control module (9) is arranged between the sample injection selection valve (8) and the four-way two-position valve (11), a second control module (10) is arranged between the fourth gas storage component (4) and the four-way two-position valve (11), and the first control module (9) and the second control module (10) both comprise an electronic pressure controller and a mass flowmeter.
4. For ambient air CO according to claim 1 2 And CH (CH) 4 The gas marking and setting device is characterized in that a four-way two-position valve (11) and CO 2 /CH 4 High-precision spectrometer (17), four-way two-position valve (11) and CO 2 A water removal unit is arranged between the isotope spectrometers (18).
5. The method for ambient air CO of claim 4 2 And CH (CH) 4 The device for calibrating the standard gas is characterized in that the water removal unit is a cold trap.
6. The method for ambient air CO of claim 5 2 And CH (CH) 4 The gas standard value device is characterized by further comprising a first three-way valve (14), a second three-way valve (15), a third three-way valve (16), an idle gas storage component (20), a third three-way valve (16), a first three-way valve (14) and CO 2 /CH 4 The high-precision spectrometer (17) is communicated, a third three-way valve (16), a second three-way valve (15) and CO 2 The isotope spectrometer (18) is communicated.
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| CN202321819106.5U CN220455273U (en) | 2023-07-11 | 2023-07-11 | CO for ambient air 2 And CH (CH) 4 Gas marking value setting device |
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