Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (8): 763-771.DOI: 10.3724/SP.J.1123.2022.02011
• Technical Notes • Previous Articles
HONG Haixiang1, ZANG Kunpeng1,2, CHEN Yuanyuan1,2, LIN Yi1,2, LI Jiaxin1, QING Xuemei1, QIU Shanshan1, XIONG Haoyu1, JIANG Kai1, FANG Shuangxi1,2,*()
Received:
2022-02-21
Online:
2022-08-08
Published:
2022-07-29
Contact:
FANG Shuangxi
Supported by:
CLC Number:
HONG Haixiang, ZANG Kunpeng, CHEN Yuanyuan, LIN Yi, LI Jiaxin, QING Xuemei, QIU Shanshan, XIONG Haoyu, JIANG Kai, FANG Shuangxi. Monitoring of atmospheric CH4, CO, CO2, N2O and SF6 using three-channel gas chromatography[J]. Chinese Journal of Chromatography, 2022, 40(8): 763-771.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.02011
Fig. 1 Diagram of three-channel gas chromatography (GC) system AUX: auxiliary; PCM: pressure control module; CAT: catalysis transition; FID: flame ionization detector; μ-ECD: micro-electrical capture detector.
Standard gas | Numbered | CH4/10-9 | CO/10-9 | CO2/10-6 | N2O/10-9 | SF6/10-12 |
---|---|---|---|---|---|---|
Tested gas | C1 | 1922.6 | 146.8 | 374.94 | 304.59 | 8.45 |
C2 | 2047.6 | 229.4 | 408.88 | 313.27 | 9.21 | |
C3 | 2236.8 | 255.8 | 453.38 | 332.69 | 10.86 | |
C4 | 2431.3 | 355.3 | 497.89 | 345.84 | 12.61 | |
C5 | 2622.3 | 428.9 | 595.47 | 349.06 | 14.16 | |
C* | 2005.9 | 191.6 | 422.25 | 334.37 | 10.76 | |
Working gas | W | 2005.9 | 191.6 | 422.25 | 334.37 | 10.76 |
Target gas | T | 2075.4 | 185.6 | 414.33 | 322.27 | 10.12 |
Table 1 Mole fractions of standard gases for the system testing
Standard gas | Numbered | CH4/10-9 | CO/10-9 | CO2/10-6 | N2O/10-9 | SF6/10-12 |
---|---|---|---|---|---|---|
Tested gas | C1 | 1922.6 | 146.8 | 374.94 | 304.59 | 8.45 |
C2 | 2047.6 | 229.4 | 408.88 | 313.27 | 9.21 | |
C3 | 2236.8 | 255.8 | 453.38 | 332.69 | 10.86 | |
C4 | 2431.3 | 355.3 | 497.89 | 345.84 | 12.61 | |
C5 | 2622.3 | 428.9 | 595.47 | 349.06 | 14.16 | |
C* | 2005.9 | 191.6 | 422.25 | 334.37 | 10.76 | |
Working gas | W | 2005.9 | 191.6 | 422.25 | 334.37 | 10.76 |
Target gas | T | 2075.4 | 185.6 | 414.33 | 322.27 | 10.12 |
Channel | Detected gas | Quantitative loop/mL | Precolumn | Analytical column | Carrier gas | |||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Specification | Packing | Specification | Packing | Species | Pressure/kPa | |||||||
1 | CH4/CO | 10 | 1.2 m, stainless steel | 60-80 meshes molecular sieves | 1.2 m, stainless steel | 60-80 meshes Unibeads 1 S | high purity N2 (99.999%) | 103.43 (backflush gas: 137.9) | ||||
2 | CO2 | 5 | 1.2 m, stainless steel | 60-80 meshes molecular sieves | 4.5 m, stainless steel | 80-100 meshes HayeSep Q | high purity N2 (99.999%) | 137.9 | ||||
3 | N2O/SF6 | 15 | 2 m, stainless steel | 80-100 meshes HayeSep Q | 2 m, stainless steel | 80-100 meshes HayeSep Q | high purity N2 (99.999%) and argon-methane (99.9999%) | 68.95 (backflush gas: 68.95) |
Table 2 Chromatographic working conditions for the GC system
Channel | Detected gas | Quantitative loop/mL | Precolumn | Analytical column | Carrier gas | |||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Specification | Packing | Specification | Packing | Species | Pressure/kPa | |||||||
1 | CH4/CO | 10 | 1.2 m, stainless steel | 60-80 meshes molecular sieves | 1.2 m, stainless steel | 60-80 meshes Unibeads 1 S | high purity N2 (99.999%) | 103.43 (backflush gas: 137.9) | ||||
2 | CO2 | 5 | 1.2 m, stainless steel | 60-80 meshes molecular sieves | 4.5 m, stainless steel | 80-100 meshes HayeSep Q | high purity N2 (99.999%) | 137.9 | ||||
3 | N2O/SF6 | 15 | 2 m, stainless steel | 80-100 meshes HayeSep Q | 2 m, stainless steel | 80-100 meshes HayeSep Q | high purity N2 (99.999%) and argon-methane (99.9999%) | 68.95 (backflush gas: 68.95) |
Analyte | Average mole fraction | SD(1σ) | RSD/% |
---|---|---|---|
CH4 | 2005.0×10-9 | 1.70×10-9 | 0.08 |
CO | 191.6×10-9 | 3.63×10-9 | 1.90 |
CO2 | 422.24×10-6 | 0.20×10-6 | 0.05 |
N2O | 334.39×10-9 | 0.26×10-9 | 0.08 |
SF6 | 10.76×10-12 | 0.07×10-12 | 0.66 |
Table 3 Mole fractions and their deviations, RSDs of the targets calculated from areas and heights (n=95)
Analyte | Average mole fraction | SD(1σ) | RSD/% |
---|---|---|---|
CH4 | 2005.0×10-9 | 1.70×10-9 | 0.08 |
CO | 191.6×10-9 | 3.63×10-9 | 1.90 |
CO2 | 422.24×10-6 | 0.20×10-6 | 0.05 |
N2O | 334.39×10-9 | 0.26×10-9 | 0.08 |
SF6 | 10.76×10-12 | 0.07×10-12 | 0.66 |
Analyte | SDs | RSDs/% | |||||||
---|---|---|---|---|---|---|---|---|---|
Ref. [ | Ref. [ | This work | Ref. [ | Ref. [ | Ref. [ | This work | |||
CH4 | 32× | 10-9 | 0.63×10-9 | 1.70×10-9 | 0.5-3.5 | - | 0.04 | 0.08 | |
CO | - | 0.55×10-9 | 3.63×10-9 | 0.5-3.5 | - | 0.50 | 1.90 | ||
CO2 | 1.29× | 10-6 | - | 0.20×10-6 | 0.5-3.5 | 0.4-6.6 | - | 0.05 | |
N2O | 5× | 10-9 | 0.25×10-9 | 0.26×10-9 | - | 1.0-5.1 | 0.08 | 0.08 | |
SF6 | - | 0.10×10-12 | 0.07×10-12 | - | - | 1.80 | 0.66 |
Table 4 Comparison of different GC system precision
Analyte | SDs | RSDs/% | |||||||
---|---|---|---|---|---|---|---|---|---|
Ref. [ | Ref. [ | This work | Ref. [ | Ref. [ | Ref. [ | This work | |||
CH4 | 32× | 10-9 | 0.63×10-9 | 1.70×10-9 | 0.5-3.5 | - | 0.04 | 0.08 | |
CO | - | 0.55×10-9 | 3.63×10-9 | 0.5-3.5 | - | 0.50 | 1.90 | ||
CO2 | 1.29× | 10-6 | - | 0.20×10-6 | 0.5-3.5 | 0.4-6.6 | - | 0.05 | |
N2O | 5× | 10-9 | 0.25×10-9 | 0.26×10-9 | - | 1.0-5.1 | 0.08 | 0.08 | |
SF6 | - | 0.10×10-12 | 0.07×10-12 | - | - | 1.80 | 0.66 |
Analyte | Regression equation | R2 | Mole fraction range |
---|---|---|---|
CH4 | y=0.023x-0.082 | 0.9999 | 1922.6×10-9-2622.3×10-9 |
CO | y=0.007x-0.148 | 0.9999 | 146.8×10-9-428.9×10-9 |
CO2 | y=-0.002x2+41.295x-343.036 | 0.9999 | 374.94×10-6-595.47×10-6 |
N2O | y=0.006x2+22.861x-1816.137 | 0.9999 | 304.59×10-9-349.06×10-9 |
SF6 | y=1.992x+1.083 | 0.9999 | 8.45×10-12-14.16×10-12 |
Table 5 Linear response results of GC system
Analyte | Regression equation | R2 | Mole fraction range |
---|---|---|---|
CH4 | y=0.023x-0.082 | 0.9999 | 1922.6×10-9-2622.3×10-9 |
CO | y=0.007x-0.148 | 0.9999 | 146.8×10-9-428.9×10-9 |
CO2 | y=-0.002x2+41.295x-343.036 | 0.9999 | 374.94×10-6-595.47×10-6 |
N2O | y=0.006x2+22.861x-1816.137 | 0.9999 | 304.59×10-9-349.06×10-9 |
SF6 | y=1.992x+1.083 | 0.9999 | 8.45×10-12-14.16×10-12 |
Fig. 3 Standard gas fitting residual distribution The gray areas represent World Meteorological Organization (WMO)/Global Atmospheric Watch (GAW) expanded quality control target.
Analyte | Regression equation | R2 | Calculated value | Calibrated value | Difference |
---|---|---|---|---|---|
CH4 | y=0.023x-0.077 | 0.9999 | 2232.65×10-9 | 2236.8×10-9 | 0.15×10-9 |
CO | y=0.007x-0.152 | 0.9998 | 256.0×10-9 | 255.8×10-9 | 0.20×10-9 |
CO2 | y=-0.002x2+41.202x-321.621 | 0.9999 | 453.75×10-6 | 453.38×10-6 | 0.37×10-6 |
N2O | y=0.023x2+11.798x+3622.442 | 0.9999 | 332.34×10-9 | 332.69×10-9 | 0.35×10-9 |
SF6 | y=1.992x+1.066 | 0.9999 | 10.88×10-12 | 10.86×10-12 | 0.02×10-12 |
Table 6 Accuracy test results of GC system
Analyte | Regression equation | R2 | Calculated value | Calibrated value | Difference |
---|---|---|---|---|---|
CH4 | y=0.023x-0.077 | 0.9999 | 2232.65×10-9 | 2236.8×10-9 | 0.15×10-9 |
CO | y=0.007x-0.152 | 0.9998 | 256.0×10-9 | 255.8×10-9 | 0.20×10-9 |
CO2 | y=-0.002x2+41.202x-321.621 | 0.9999 | 453.75×10-6 | 453.38×10-6 | 0.37×10-6 |
N2O | y=0.023x2+11.798x+3622.442 | 0.9999 | 332.34×10-9 | 332.69×10-9 | 0.35×10-9 |
SF6 | y=1.992x+1.066 | 0.9999 | 10.88×10-12 | 10.86×10-12 | 0.02×10-12 |
Fig. 4 Diurnal variations of atmospheric CH4, CO, CO2, N2O and SF6 mole fractions in Hangzhou from May to July in 2021 (n=60) The time series is consistent with Fig. 5 below.
Fig. 5 Variations of mole fractions of CH4, CO, CO2, N2O and SF6 in the atmosphere of the urban area of Hangzhou during the trial operation of the system The hollow boxes in the figure represent the mole fractions of the ambient atmosphere of Hangzhou, and the solid dots represent the mole fractions of the target gas measured by the GC system, the above data have not been filtered by background and non-background data. The system is used for both laboratory calibration and off-line sample analysis, thus the partial data missed.
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