CN117233273A - Method for measuring and analyzing compound in fluorine-containing greenhouse gas - Google Patents
Method for measuring and analyzing compound in fluorine-containing greenhouse gas Download PDFInfo
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- CN117233273A CN117233273A CN202310978385.8A CN202310978385A CN117233273A CN 117233273 A CN117233273 A CN 117233273A CN 202310978385 A CN202310978385 A CN 202310978385A CN 117233273 A CN117233273 A CN 117233273A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 150000001875 compounds Chemical class 0.000 title claims abstract description 27
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 26
- 239000011737 fluorine Substances 0.000 title claims abstract description 26
- 239000005431 greenhouse gas Substances 0.000 title claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 59
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 238000001819 mass spectrum Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000010813 internal standard method Methods 0.000 claims abstract description 9
- 230000014759 maintenance of location Effects 0.000 claims abstract description 5
- 238000005070 sampling Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 238000011088 calibration curve Methods 0.000 claims description 24
- 238000004458 analytical method Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 230000003111 delayed effect Effects 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 238000004094 preconcentration Methods 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 230000003595 spectral effect Effects 0.000 claims description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N monofluoromethane Natural products FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 abstract description 12
- BCCOBQSFUDVTJQ-UHFFFAOYSA-N octafluorocyclobutane Chemical compound FC1(F)C(F)(F)C(F)(F)C1(F)F BCCOBQSFUDVTJQ-UHFFFAOYSA-N 0.000 abstract description 6
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 abstract description 6
- 239000004341 Octafluorocyclobutane Substances 0.000 abstract description 5
- 235000019407 octafluorocyclobutane Nutrition 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000004454 trace mineral analysis Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 229910018503 SF6 Inorganic materials 0.000 description 2
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 description 2
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 2
- 229960000909 sulfur hexafluoride Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
Classifications
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for measuring and analyzing compounds in fluorine-containing greenhouse gases, which adopts a vacuum sampling tank with an inert inner wall to collect air samples, the temperature and humidity of the air samples are recorded during collection, the collected air samples are concentrated and pyrolyzed and absorbed by a pre-concentrator three-stage, then the air samples sequentially enter a gas chromatograph for separation and a mass spectrum detector for detection, and the air samples are quantitatively compared with a standard substance retention time and a mass spectrogram for qualitative determination by an internal standard method, wherein standard use gas and internal standard use gas are respectively prepared by the standard substance and the internal standard method quantitatively. The method realizes trace analysis of the monofluoromethane, the tetrafluoromethane and the octafluorocyclobutane in the fluorine-containing greenhouse gas, is simple and convenient to operate and easy to execute, does not involve expensive materials, can obtain reagent consumables in situ, does not need special purchasing, and saves the measurement cost.
Description
Technical Field
The invention relates to the technical field of environmental detection, in particular to a method for measuring and analyzing compounds in fluorine-containing greenhouse gases.
Background
Fluorine-containing greenhouse gases generally include Hydrofluorocarbons (HFCs), perfluorocarbons (PFCs), sulfur hexafluoride (SF) 6 ) And nitrogen trifluoride (NF) 3 ) Among the compounds in the fluorine-containing greenhouse gas are monofluoromethane, tetrafluoromethane and octafluorocyclobutane. Although methods for detecting compounds in fluorine-containing greenhouse gases are widely studied at home and abroad, most of the analysis methods for compounds have no detection standard yet.
Disclosure of Invention
The invention aims to provide a method for measuring and analyzing compounds in fluorine-containing greenhouse gases, which is used for realizing trace analysis of monofluoromethane, tetrafluoromethane and octafluorocyclobutane in the fluorine-containing greenhouse gases, has the advantages of simple operation, easy execution, no expensive materials, available reagent consumables in situ, no special purchasing, and measurement cost saving.
In order to solve the technical problems, the method for measuring and analyzing the compounds in the fluorine-containing greenhouse gas adopts a vacuum sampling tank with the inner wall subjected to inerting treatment to collect an air sample, the temperature and the humidity of the air sample are recorded during collection, the collected air sample is concentrated and pyrolyzed and absorbed by a pre-concentrator three-stage device and then sequentially enters a gas chromatograph to be separated and a mass spectrum detector to be detected, and the standard gas and the internal standard gas are quantitatively prepared by comparing the standard gas with the retention time and the mass spectrum of the standard substance, wherein the standard substance and the internal standard gas are quantitatively prepared by an internal standard method respectively.
In the method, the standard use gas and the internal standard use gas are humidified according to saturated moisture or according to the temperature and humidity of an air sample, and then are prepared and kept stand for more than 12 hours.
Further, the standard gas is prepared according to two concentrations of 20nmol/mol and 100nmol/mol respectively, wherein one of the standard gas is used for drawing a low concentration point in the calibration curve, the other standard gas is used for drawing a high concentration point in the calibration curve, if the linearity of the calibration curve drawn by the two standard gas is good, the gas distribution introducing deviation can be judged to be small, and the collected air sample can be continuously analyzed.
Further, after the standard use gas balance is finished, respectively drawing calibration curves with the concentrations of 5.0nmol/mol, 10.0nmol/mol, 20.0nmol/mol, 30.0nmol/mol, 40.0nmol/mol, 50.0nmol/mol and 100nmol/mol by adopting the standard use gas with the two concentrations under the same instrument condition, wherein the relative response factor mean value RSD of the calibration curves is less than or equal to 30%, otherwise, drawing the calibration curves by re-distributing gas, and then analyzing the collected air samples according to the same instrument condition.
Further, after the air sample is concentrated, the pre-concentrator is baked for 20min, wherein the baking temperature of the primary cold trap is 150 ℃, and the baking temperature of the secondary cold trap is 220 ℃.
Further, the solvent delay was set before the peak of the first compound upon detection by the mass spectrometer.
Further, the preconcentrator performs three-stage concentration on the air sample according to the following operation parameters: the first-stage cold trap trapping temperature is-20 ℃, the analysis preheating temperature is 10 ℃, the analysis temperature is 10 ℃, the baking temperature is 150 ℃, and the first-stage cold trap is an empty trap; the trapping temperature of the secondary cold trap is-100 ℃, the analysis preheating temperature is-40 ℃, the analysis temperature is 230 ℃, the baking temperature is 220 ℃, and the secondary cold trap is a trapping trap filled with Tenax filler; the focusing temperature of the three-stage cold trap is-180 ℃ and the resolving temperature is 80 ℃; after the air sample is concentrated, the air sample enters a gas chromatograph, an Agilent 123-1063 chromatographic column is adopted, and the gas phase parameters are as follows: the temperature programming is maintained at 0 ℃ for 13min,5 ℃/min is increased to 40 ℃ for 0min, then 20 ℃/min is increased to 220 ℃ for 15min, and then the operation is carried out at 120 ℃ for 5min; the split ratio is 20:1, the temperature of the sample inlet is 150 ℃, and the column flow is 1.5ml/min; the mass spectral parameters were as follows: the temperature of the transmission line is 280 ℃, the temperature of the ion source is 230 ℃, the temperature of the four-stage rod is 150 ℃, the EI voltage is 70 ℃, and the solvent is delayed for 2min by adopting a full scanning mode.
The method adopts the technical scheme that the method adopts a vacuum sampling tank with the inner wall subjected to inerting treatment to collect an air sample, the temperature and the humidity of the air sample are recorded during collection, the collected air sample is subjected to three-stage concentration and pyrolysis absorption by a pre-concentration instrument, then sequentially enters a gas chromatograph for separation and a mass spectrum detector for detection, and is compared and qualitative with the retention time and a mass spectrum of a standard substance and quantitative by an internal standard method, wherein the standard substance and the internal standard method are respectively used for preparing standard use gas and internal standard use gas quantitatively. The method realizes trace analysis of the monofluoromethane, the tetrafluoromethane and the octafluorocyclobutane in the fluorine-containing greenhouse gas, is simple and convenient to operate and easy to execute, does not involve expensive materials, can obtain reagent consumables in situ, does not need special purchasing, and saves the measurement cost.
Drawings
The invention is described in further detail below with reference to the attached drawings and embodiments:
FIG. 1 is a graph of total ion chromatogram (abundance-retention time) of fluorine-containing greenhouse gases in the present method;
FIG. 2 is a schematic representation of a calibration curve for monofluoromethane (response factor-concentration) in a fluorine-containing greenhouse gas of the present method;
FIG. 3 is a schematic representation of a calibration curve for tetrafluoromethane (response factor-concentration) in a fluorine-containing greenhouse gas of the present method;
FIG. 4 is a graph showing the calibration curve of octafluorocyclobutane (response factor-concentration) in the fluorine-containing greenhouse gas of the present method.
Detailed Description
The method for measuring and analyzing the compound in the fluorine-containing greenhouse gas adopts a vacuum sampling tank with the inner wall subjected to inerting treatment to collect an air sample, the temperature and the humidity of the air sample are recorded during collection, the collected air sample is subjected to three-stage concentration and pyrolysis absorption by a pre-concentration instrument, then sequentially enters a gas chromatograph to be separated and a mass spectrum detector to be detected, and is quantitatively determined by comparing with the retention time and the mass spectrum of a standard substance and an internal standard method, wherein the standard substance and the internal standard method are respectively used for preparing standard use gas and internal standard use gas quantitatively.
Preferably, in the method, the standard use gas and the internal standard use gas are humidified according to saturated moisture or according to the temperature and humidity of an air sample, and then are prepared and kept stand for more than 12 hours. Thereby prolonging the preservation time of the standard use gas and the internal standard use gas, improving the linearity of the calibration curve, and ensuring the accuracy and reliability of the internal standard use gas and the standard use gas.
Preferably, the standard gas is prepared according to two concentrations of 20nmol/mol and 100nmol/mol respectively, wherein one of the standard gas is used for drawing a low concentration point in the calibration curve, the other standard gas is used for drawing a high concentration point in the calibration curve, if the linearity of the calibration curve drawn by the two standard gas is good, the gas distribution introducing deviation can be judged to be small, and the collected air sample can be continuously analyzed. Standard use gas of both concentrations is used to check deviations introduced by accidental factors in the process of standard gas preparation.
Preferably, after the standard use gas balance is finished, respectively drawing calibration curves with the concentrations of 5.0nmol/mol, 10.0nmol/mol, 20.0nmol/mol, 30.0nmol/mol, 40.0nmol/mol, 50.0nmol/mol and 100nmol/mol by adopting the standard use gas with two concentrations under the same instrument condition, wherein the relative response factor mean value RSD of the calibration curves is less than or equal to 30%, otherwise, re-distributing gas to draw the calibration curves, and then analyzing the collected air samples according to the same instrument condition.
Preferably, after the air sample is concentrated, the pre-concentrator is baked for 20min, wherein the baking temperature of the primary cold trap is 150 ℃, and the baking temperature of the secondary cold trap is 220 ℃. Avoiding the influence of moisture and sample residues on the subsequent sample analysis.
Preferably, the solvent delay is set before the peak of the first compound when detected by the mass spectrometer. Reducing interference of moisture on the detection of the mass spectrum detector.
Preferably, the preconcentrator performs a three-stage concentration of the air sample according to the following operating parameters: the first-stage cold trap trapping temperature is-20 ℃, the analysis preheating temperature is 10 ℃, the analysis temperature is 10 ℃, the baking temperature is 150 ℃, and the first-stage cold trap is an empty trap; the trapping temperature of the secondary cold trap is-100 ℃, the analysis preheating temperature is-40 ℃, the analysis temperature is 230 ℃, the baking temperature is 220 ℃, and the secondary cold trap is a trapping trap filled with Tenax filler; the focusing temperature of the three-stage cold trap is-180 ℃ and the resolving temperature is 80 ℃; after the air sample is concentrated, the air sample enters a gas chromatograph, an Agilent 123-1063 chromatographic column is adopted, and the gas phase parameters are as follows: the temperature programming is maintained at 0 ℃ for 13min,5 ℃/min is increased to 40 ℃ for 0min, then 20 ℃/min is increased to 220 ℃ for 15min, and then the operation is carried out at 120 ℃ for 5min; the split ratio is 20:1, the temperature of the sample inlet is 150 ℃, and the column flow is 1.5ml/min; the mass spectral parameters were as follows: the temperature of the transmission line is 280 ℃, the temperature of the ion source is 230 ℃, the temperature of the four-stage rod is 150 ℃, the EI voltage is 70 ℃, and the solvent is delayed for 2min by adopting a full scanning mode. Through the debugging of the instrument parameters, good analysis effect is ensured, and the measurement accuracy is improved.
Fig. 1 shows a total ion chromatogram of the method, and fig. 2, fig. 3 and fig. 4 show calibration curves of three compounds in fluorine-containing greenhouse gas drawn by the method, wherein the concentration ratio is the ratio of the concentration of the target compound to the concentration of the internal standard compound, and the response ratio is the ratio of the response of the target compound to the response of the internal standard compound. The calibration curve shows that the RSD is 6.449%, 8.778% and 11.253%, respectively, and the relative standard deviation of the relative response factor is less than or equal to 30%, which meets the linear requirement of the general method.
And (3) evaluating the detection limit, calculating the detection limit by adopting the method, wherein the detection limit of all three compounds is 0.2nmol/mol, the trace analysis requirement is met, and the analysis result is shown in table 1.
Table 1:
precision and accuracy are evaluated, the precision and accuracy are calculated by adopting the method, the precision RSD of the three compounds is 0.57-14.6%, the relative error is 0.79-12.8%, and the accuracy requirement of the method is met. The analysis results are shown in Table 2.
Table 2:
the method obtained by the evaluation is completely suitable for the determination and analysis of the monofluoromethane, the tetrafluoromethane and the octafluorocyclobutane compounds in the fluorine-containing greenhouse gas, and meets the determination and analysis precision.
Claims (7)
1. A method for measuring and analyzing compounds in fluorine-containing greenhouse gases is characterized in that: the method adopts a vacuum sampling tank with an inert inner wall for collecting an air sample, the temperature and the humidity of the air sample are recorded during collection, the collected air sample is subjected to three-stage concentration and pyrolysis absorption by a pre-concentration instrument, then sequentially enters a gas chromatograph for separation and a mass spectrum detector for detection, and is qualitatively compared with the retention time and the mass spectrum of a standard substance and quantitatively determined by an internal standard method, wherein the standard substance and the internal standard method quantitatively prepare standard use gas and internal standard use gas respectively.
2. The method for measuring and analyzing a compound in a fluorine-containing greenhouse gas according to claim 1, wherein: in the method, the standard use gas and the internal standard use gas are humidified according to saturated moisture or according to the temperature and humidity of an air sample, and then are prepared and kept stand for more than 12 hours.
3. The method for measuring and analyzing a compound in a fluorine-containing greenhouse gas according to claim 2, wherein: the standard gas is prepared according to two concentrations of 20nmol/mol and 100nmol/mol respectively, wherein one of the standard gas is used for drawing a low concentration point in a calibration curve, the other standard gas is used for drawing a high concentration point in the calibration curve, and if the linearity of the calibration curve drawn by the two standard gas is good, the gas distribution introducing deviation can be judged to be small, and the collected air sample can be continuously analyzed.
4. The method for measuring and analyzing a compound in a fluorine-containing greenhouse gas according to claim 3, wherein: after the standard use gas balance is finished, respectively drawing calibration curves with the concentrations of 5.0nmol/mol, 10.0nmol/mol, 20.0nmol/mol, 30.0nmol/mol, 40.0nmol/mol, 50.0nmol/mol and 100nmol/mol by adopting standard use gas with two concentrations under the same instrument condition, wherein the relative response factor mean value RSD of the calibration curves is less than or equal to 30%, otherwise, drawing the calibration curves by re-distributing gas, and then analyzing the collected air samples according to the same instrument condition.
5. The method for measuring and analyzing a compound in a fluorine-containing greenhouse gas according to claim 1, wherein: and after the air sample is concentrated, baking the pre-concentrator for 20min, wherein the primary cold trap baking temperature is 150 ℃, and the secondary cold trap baking temperature is 220 ℃.
6. The method for measuring and analyzing a compound in a fluorine-containing greenhouse gas according to claim 1, wherein: the solvent delay was set before the peak of the first compound when detected by the mass spectrometer.
7. The method for measuring and analyzing a compound in a fluorine-containing greenhouse gas according to claim 1, wherein: the preconcentrator performs three-stage concentration on the air sample according to the following operation parameters: the first-stage cold trap trapping temperature is-20 ℃, the analysis preheating temperature is 10 ℃, the analysis temperature is 10 ℃, the baking temperature is 150 ℃, and the first-stage cold trap is an empty trap; the trapping temperature of the secondary cold trap is-100 ℃, the analysis preheating temperature is-40 ℃, the analysis temperature is 230 ℃, the baking temperature is 220 ℃, and the secondary cold trap is a trapping trap filled with Tenax filler; the focusing temperature of the three-stage cold trap is-180 ℃ and the resolving temperature is 80 ℃; after the air sample is concentrated, the air sample enters a gas chromatograph, an Agilent 123-1063 chromatographic column is adopted, and the gas phase parameters are as follows: the temperature programming is maintained at 0 ℃ for 13min,5 ℃/min is increased to 40 ℃ for 0min, then 20 ℃/min is increased to 220 ℃ for 15min, and then the operation is carried out at 120 ℃ for 5min; the split ratio is 20:1, the temperature of the sample inlet is 150 ℃, and the column flow is 1.5ml/min; the mass spectral parameters were as follows: the temperature of the transmission line is 280 ℃, the temperature of the ion source is 230 ℃, the temperature of the four-stage rod is 150 ℃, the EI voltage is 70 ℃, and the solvent is delayed for 2min by adopting a full scanning mode.
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