CN116242906A - Online rapid monitoring and early warning method for fluorodichloroethane in air - Google Patents

Online rapid monitoring and early warning method for fluorodichloroethane in air Download PDF

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CN116242906A
CN116242906A CN202111492788.9A CN202111492788A CN116242906A CN 116242906 A CN116242906 A CN 116242906A CN 202111492788 A CN202111492788 A CN 202111492788A CN 116242906 A CN116242906 A CN 116242906A
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蒋丹丹
李海洋
李东明
陈创
王卫国
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention discloses an online rapid monitoring and early warning method for fluorodichloroethane in air, and belongs to the technical field of chemical analysis and detection. The system comprises an online sampling system, an online dehumidification system, an ion mobility spectrometry real-time online detection system, a software real-time online tracking system and the like. Sampling an environmental sample into an ion mobility spectrometry instrument by pumping and sampling in real time, and generating a large amount of reactant ions CO by photoionization in a negative ion mode 3 ‑ (K 0 ＝2.44cm 2 V ‑1 s ‑1 ) The monofluorodichloroethane reacts with the ions of the reactant to generate ionic molecules, and the ionic molecules react with CO in a negative ion mode 3 ‑ Generating electron transfer reaction to generate product ion M specific to monofluoro dichloroethane ‑ Acting in a high voltage electric fieldThe specific product ion M of the monofluorodichloroethane ‑ (K 0 ＝2.84cm 2 V ‑1 s ‑1 ) The ion detector is used for effectively separating the ion from the reactant ions, detecting the ion after the ion reaches the receiving electrode of the ion detector, generating a peak in front of the reactant ion peak, and carrying out real-time online monitoring on the product ion peak.

Description

Online rapid monitoring and early warning method for fluorodichloroethane in air
Technical Field
The invention belongs to the field of analytical chemistry instrument detection, and particularly relates to an online rapid monitoring and early warning method for monofluorodichloroethane in air.
Background
Monofluorodichloroethane (HCFC-141 b, an organic compound of the formula CCl 2 FCH 3 Is colorless transparent volatile liquid, has pungent aromatic smell, is toxic when inhaled, and has an explosion limit of 5.6-17.0% (by volume) with vapor and air to form an explosive mixture. The aqueous emulsion is mainly used as a solvent and a refrigerant and is widely used in the fields of cleaning and solvents. Since its destruction to the ozone layer is 1/10 of that of freon CFC-113, it is designated as an ideal substitute for perhalofluorocarbons and is widely used in industry, where effective monitoring of its on-site concentration is of great importance for public safety. The existing methods for detecting the monofluorodichloroethane comprise gas chromatography, gas-mass spectrometry and the like, but the gas chromatography method requires sample pre-separation, the detection time is required to be a few minutes, and the on-line rapid and effective early warning and monitoring of the monofluorodichloroethane of the environmental gas of a factory cannot be realized.
Aiming at the problems that the sample pre-separation time is long, the detection time needs a few minutes, the off-line detection is only possible, and the like in the analysis and detection method, the monitoring method for the pre-alarm of the leakage of the monofluorodichloroethane does not need any sample pretreatment, chemical reagent preparation and analysis response time can reach the ms order, is very suitable for on-site rapid and accurate quantitative detection of the explosion limit pre-alarm of the monofluorodichloroethane in the environmental air of a factory, has a very sensitive and rapid specific response mechanism for the on-line monitoring and pre-alarm of the concentration of the monofluorodichloroethane, and has the detection limit reaching the pptv order.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the rapid on-line analysis and detection method for the on-site concentration ultrahigh early warning of the monofluoro-dichloroethane solves the problem of high sensitivity response of the monofluoro-dichloroethane, eliminates the interference of other components in the complex environment, shortens the analysis time and the response time to ms magnitude, and completely eliminates any complicated sample preparation and preparation processes such as sample pretreatment and the like.
The specific contents include:
an online rapid monitoring and early warning method for fluorodichloroethane in air comprises a photoionization ion mobility spectrometry, an online gas sampler, a particle filtering device, a gas dehumidifier and a computer;
the online sampler comprises a sampling pump and a gas mass flowmeter for controlling the sampling amount, an ambient air sample is continuously collected through the sampling pump, the sample firstly passes through an ambient air particle filtering device, and then is subjected to online dehumidification through a gas dehumidifier to eliminate the influence of ambient air humidity on the detection of the next-stage photoionization ion mobility spectrometry, and the dehumidified sample directly enters the ion mobility spectrometry for detection; in the ion mobility spectrometry, the monofluorodichloroethane and a Reactant Ion (RIP) are subjected to electron transfer reaction under the action of vacuum ultraviolet light ionization to form a specific product ion peak (M-) with the migration time of 2.31ms, signals acquired by the ion mobility spectrometry are transmitted to a computer in real time, the product ion peak of the monofluorodichloroethane is tracked in real time by adopting computer software, the migration time of the reagent ion peak is RIPt (2.69 ms), the ratio of the tracked peak position is 0.86, the deviation of the tracked peak position is 0.20, the peak position interval of the tracked monofluorodichloroethane is RIPt 0.86-0.20ms to RIPt 0.86+0.20ms, the computer automatically identifies the peak position with the highest intensity in the peak position interval, the peak position is automatically read, the quantitative curve equation y=a+c is brought into, the automatic alarm function is set, and when the detected monofluorodichloroethane is more than 1%, the computer alarms.
The online gas sampler samples ambient gas through a sampling pump, the ambient gas passes through a particle filtering device, one end of the ambient gas is connected with an air inlet of the sampling pump, the other end of the ambient gas is connected with an air outlet of the sampling pump, the air outlet of the sampling pump is connected with an air inlet end of the mass flowmeter, the air outlet end of the mass flowmeter is connected with the air inlet end of the online dehumidifier, and the flow velocity range of the mass flowmeter is set to be 10-1000ml/min.
The particle filter device adopts a large porous structure filtering membrane to remove large particle matters in the ambient gas, and the pore diameter is in the range of 0.1-10 mu m.
The air inlet end of the air dehumidifier is connected with the air outlet end of the mass flowmeter, the air dehumidifier is a membrane dehumidifier, the dehumidifier adopts a hydrophobic polydimethylsiloxane membrane (PDMS) or a perfluorinated sulfonic acid membrane (nafion) to dehumidify, and the air outlet end of the air dehumidifier is connected with the sample inlet port of the ion mobility spectrometry.
The gas dehumidifier uses clean compressed air to sweep the outside of the membrane of the gas dehumidifier (the side of the membrane contacted with the air sample is called as the inside of the membrane, and the other side is called as the outside of the membrane) to remove redundant moisture, and the humidity of the collected sample is kept below 1 ppm.
The computer automatically identifies the RIPt of the product ion peak of the reagent ion peak, sets the peak position multiple 0.86 and the peak position deviation 0.20, tracks the peak position interval of the monofluoro dichloroethane to be RIPt 0.86-0.20ms to RIPt 0.86+0.20ms, the computer software finds the highest peak in the peak position interval of the monofluoro dichloroethane, automatically reads the peak high intensity, obtains the intensity ratio of the peak high intensity to the reagent ion peak, substitutes the ratio into a quantitative curve y=a+c, wherein a and b are dimensionless parameters, obtains the concentration C of the monofluoro dichloroethane, sets an alarm threshold value of 1%, and automatically alarms when the C is more than 1%, namely the concentration is exceeded.
In the detection mode, one or more than two of ketone such as acetone and aromatic hydrocarbon reagent molecules such as toluene are adopted to realize high-sensitivity online monitoring of monofluoro-dichloroethane, the temperature of a migration tube of an ion mobility spectrometry is set to be 40-150 ℃, the opening time of an ion gate is 40-100 mu s, the carrier gas flow rate of the acetone reagent molecules is 20-200ml/min, and a computer with automatic monitoring software is adopted to automatically alarm after the concentration exceeds a threshold value, so that unattended continuous monitoring can be realized, and the method has important safety pre-warning significance for on-site monitoring.
And detecting air samples containing monofluorodichloroethane with different concentrations to obtain the intensity ratio of peak high intensity of 1ppm, 5ppm, 10ppm and 100ppm of monofluorodichloroethane to reagent ion peak, and drawing standard curves by taking the concentration (C) and the intensity ratio (y) as abscissa to obtain a quantitative curve y=a+c+b of the monofluorodichloroethane concentration corresponding to the intensity ratio, so as to obtain the parameter values of a and b.
The specific method is also suitable for on-line monitoring and leakage early warning of halogenated hydrocarbons such as chloromethane, fluorotrichloromethane, chloroethane, chloroethylene or 1, 2-dichloroethane and the like in gas, and different compounds have different specific signal responses.
The invention comprises an on-line sampling system, an on-line dehumidification system, an ion mobility spectrometry real-time on-line detection system, a software real-time on-line tracking system and the like. Sampling an environmental sample into an ion mobility spectrometry instrument by pumping and sampling in real time, and generating a large amount of reactant ions CO by photoionization in a negative ion mode 3 - (K 0 ＝2.44cm 2 V -1 s -1 ) The monofluorodichloroethane reacts with reactant ions in an ionic molecular manner and reacts with CO in a negative ion mode 3 - Adding to generate specific product ion of the monofluorodichloroethane, and under the action of high-voltage electric field, generating specific product ion M of the monofluorodichloroethane - (K 0 ＝2.84 cm 2 V -1 s -1 ) The ion detector is used for effectively separating the ion from the reactant ions, detecting the ion after the ion reaches the receiving electrode of the ion detector, generating a peak in front of the reactant ion peak, and carrying out real-time online monitoring on the product ion peak. The analysis detection method has the advantages of simplicity, rapidness, no need of any sample pretreatment, sample preparation and other processes, can realize rapid high-selectivity early warning and monitoring of the monofluorodichloroethane on site, has the detection time of only 80ms and the response time of up to the ms order, can be applied to rapid specific leakage early warning and monitoring of monofluorodichloroethane in the environmental air of a factory, can automatically track and monitor through software, does not need on-site personnel supervision and duty, and can realize the function of network data acquisitionThe remote monitoring data is automatically returned to the main control platform, so that the method is very suitable for on-site rapid early warning and monitoring of dangerous chemicals, emergency response processing and the like.
Drawings
Fig. 1 is a schematic diagram of an ion mobility spectrometry structure for rapidly monitoring and early warning of the fluorodichloroethane in the air on line, wherein 1 is a vacuum ultraviolet lamp, 2 is a total air outlet, 3 is a reagent molecule generating bottle, 4 is a reagent molecule carrier gas, 5 is a membrane dehumidifier, 6 is outside the membrane dehumidifier, 7 is a mass flowmeter, 8 is a gas sampling pump, 9 is a gas sampling pipeline, 10 is a gas particle primary filtration membrane, 11 is a gas drift inlet of a mobility tube, 12 is an amplifier, 13 is a computer, 14 is a grid, 15 is an electrode ring, 16 is an ion gate of TP, 17 is a first grid of the ion gate, 18 is a second grid of the ion gate, and 19 is a negative high-voltage module.
FIG. 2 is a graph 2 of ion mobility spectrum of monofluorodichloroethane in air monitored by on-line rapid pre-warning
FIG. 3 is a graph 3 showing the ion mobility of monofluorodichloroethane of different concentrations in air for on-line rapid early warning
FIG. 4 is a graph 4 of a monitoring and early warning of the leakage of concentration of monofluorodichloroethane in continuous on-line tracking air
Detailed Description
Example 1
An online rapid monitoring and early warning method for fluorodichloroethane in air comprises a photoionization ion mobility spectrometry, an online gas sampler, a gas dehumidifier and a computer; the ion mobility spectrometry structure diagram of the on-line monitoring monofluorodichloroethane in real time is shown in fig. 1, the specific structure is that the on-line gas sampler comprises a sampling pump and a gas mass flowmeter for controlling sampling amount, an ambient air sample is continuously collected through the sampling pump, the sample passes through an ambient air particle filtering device, then passes through an air inlet at one end and an air outlet at the other end of the sampling pump and is connected with an air inlet end of the mass flowmeter, an air outlet end of the mass flowmeter is connected with an air inlet end of an on-line dehumidification system, the flow velocity range of the flowmeter is set to be 10-1000ml/min, on-line dehumidification is carried out through a gas dehumidifier to eliminate the influence of ambient air humidity on the detection of the next stage of photoionization mobility spectrometry, the air inlet end of the gas dehumidifier is connected with an air outlet end of the mass flowmeter, the gas dehumidifier is a membrane dehumidifier, the dehumidifier is dehumidified by adopting a hydrophobic polydimethylsiloxane membrane (PDMS), a perfluorinated sulfonic acid membrane (nafion) or a polytetrafluoroethylene membrane (teflon), and the air outlet end of the gas dehumidifier is connected with an inlet port of the ion mobility spectrometry. The gas dehumidifier uses clean compressed air to sweep the outside of the membrane of the gas dehumidifier (the side of the membrane contacted with the air sample is called as the inside of the membrane, and the other side is called as the outside of the membrane) to remove redundant moisture, and the humidity of the collected sample is kept below 1 ppm. The sample exceeds the gas dehumidifier to perform on-line dehumidification to eliminate the influence of the ambient air humidity on the detection of the next-stage photoionization ion mobility spectrometry, and the dehumidified sample directly enters the ion mobility spectrometry to be detected.
Example 2
The apparatus and procedure used was the same as in example 1, except that: the carrier gas flow rate of the acetone reagent molecules is 100ml/min, the temperature of a migration tube is 110 ℃, the opening time of an ion gate is 50 mu s in a negative ion unidirectional airflow mode, a fluorodichloroethane sample in an environment sample is sampled and dehumidified at a sampling flow rate of 15ml/min and enters an ion migration spectrum for detection, the ion migration spectrum of the detected fluorodichloroethane is shown as figure 2, in the ion migration spectrum, the fluorodichloroethane and a reaction Reagent Ion (RIP) undergo electron transfer reaction under the action of vacuum ultraviolet ionization, the migration time of the reagent ion in the negative ion mode is 2.69ms, the migration time of a product ion peak specific to the fluorodichloroethane is 2.31ms, and the single analysis time is 0.8s.
Example 3
The apparatus and procedure used was the same as in example 1, except that: the flow rate of the acetone reagent molecular carrier gas is 100ml/min, the temperature of a migration tube is 110 ℃, the method for detecting the monofluorodichloroethane with different concentrations by adopting a photoionization online ion migration spectrum detection method, and a computer automatically identifies the product ion peak position RIP of the reagent ion peak t Setting peak position multiple 0.86 and peak position deviation 0.20, and tracking the peak position interval of the monofluorodichloroethane as RIP t *0.86-0.20ms～RIP t *0.86+0.20msThe computer software finds the highest peak in the peak position interval of the monofluorodichloroethane, automatically reads the peak high intensity and obtains the intensity ratio of the peak high intensity to the reagent ion peak. Samples of monofluorodichloroethane of different concentrations were prepared, samples of concentrations C of 1ppm, 5ppm, 10ppm and 100ppm respectively, the maximum intensity ratio y at each concentration was detected and fitted to obtain a quantitative curve y=a×c+b of monofluorodichloroethane concentration versus intensity ratio, where a and b are parameters.
Example 4
The apparatus and procedure used was the same as in example 1, except that: simulating a leakage early warning monitoring process of the monofluorodichloroethane in a fume hood, setting the flow rate of acetone reagent molecular carrier gas to 100ml/min, and the temperature of a migration tube to 110 ℃, continuously tracking and monitoring the leaked monofluorodichloroethane by adopting a photoionization online ion migration spectrum detection method, and automatically identifying the product ion peak position RIP of a reagent ion peak by a computer t Setting peak position multiple 0.86 and peak position deviation 0.20, and tracking the peak position interval of the monofluorodichloroethane as RIP t *0.86-0.20ms～RIP t * The computer software finds the highest peak in the peak position interval of the monofluorodichloroethane, automatically reads the peak high intensity and obtains the intensity ratio of the peak high intensity to the reagent ion peak. The signal intensity ratio y of the monofluorodichloroethane is tracked in real time according to the quantitative equation, and the concentration C is calculated, as shown in fig. 4, the concentration of the monofluorodichloroethane continuously monitored before the simulated leakage is very low, after the leakage, the instrument rapidly monitors the leakage concentration of the monofluorodichloroethane, and when the concentration exceeds the software set threshold C > 5%, monitoring and early warning are carried out, and the software carries out the alarm in real time.

Claims (9)

1. An online rapid monitoring and early warning method for fluorodichloroethane in air comprises a photoionization ion mobility spectrometry, an online gas sampler, a particle filtering device, a gas dehumidifier and a computer;
the on-line sampler comprises a sampling pump and a gas mass flowmeter for controlling the sampling amount, and continuously collects an ambient air sample through the sampling pump, wherein the sample firstly passes through an ambient air particle filtering device and then passes through the ambient air particle filtering deviceOn-line dehumidification is carried out through a gas dehumidifier to eliminate the influence of ambient air humidity on the detection of the next-stage photoionization ion mobility spectrometry, and a dehumidified sample directly enters the ion mobility spectrometry for detection; in the ion mobility spectrometry, the monofluorodichloroethane and a Reactant Ion (RIP) are subjected to electron transfer reaction under the action of vacuum ultraviolet ionization to form a specific product ion peak (M) with the migration time of 2.31ms - ) Transmitting the signal acquired by the ion mobility spectrometry to a computer in real time, tracking the product ion peak of the monofluorodichloroethane in real time by adopting computer software, wherein the migration time of the reagent ion peak is RIP t (2.69 ms), the peak position ratio of the tracking is 0.86, the peak position deviation of the tracking is 0.20, and the peak position interval of the tracking of the monofluorodichloroethane is RIP t *0.86-0.20ms～RIP t * And 0.86+0.20ms, automatically identifying the highest intensity peak position in the peak position interval by a computer, automatically reading the peak position, bringing a quantitative curve equation y=a×c+b to obtain the concentration C of the fluorodichloroethane, setting an automatic alarm function by the instrument, wherein y is the ratio of the high intensity of the fluorodichloroethane peak to the intensity of the reagent ion peak, and immediately alarming by the computer when the monitored concentration C of the fluorodichloroethane is more than 1%.
2. The monitoring and early warning method according to claim 1, characterized in that: the online gas sampler samples ambient gas through a sampling pump, the ambient gas passes through a particle filtering device, one end of the ambient gas is connected with an air inlet of the sampling pump, the other end of the ambient gas is connected with an air outlet of the sampling pump, the air outlet of the sampling pump is connected with an air inlet end of the mass flowmeter, the air outlet end of the mass flowmeter is connected with the air inlet end of the online dehumidifier, and the flow velocity range of the mass flowmeter is set to be 10-1000ml/min.
3. The monitoring and early warning method according to claim 1 or 2, wherein the particle filtering device adopts a large porous structure filtering membrane to remove large particle matters in the ambient gas, and the pore diameter is in the range of 0.1-10 μm.
4. The monitoring and early warning method according to claim 1, characterized in that: the air inlet end of the air dehumidifier is connected with the air outlet end of the mass flowmeter, the air dehumidifier is a membrane dehumidifier, the dehumidifier adopts a hydrophobic polydimethylsiloxane membrane (PDMS), a perfluorinated sulfonic acid membrane (nafion) or a polytetrafluoroethylene membrane (teflon) for dehumidification, and the air outlet end of the air dehumidifier is connected with the sample inlet port of the ion mobility spectrometry.
5. The monitoring and early warning method according to claim 1 or 4, characterized in that: the gas dehumidifier uses clean compressed air to sweep the outside of the membrane of the gas dehumidifier (the side of the membrane contacted with the air sample is called as the inside of the membrane, and the other side is called as the outside of the membrane) to remove redundant moisture, and the humidity of the collected sample is kept below 1 ppm.
6. The monitoring and early warning method according to claim 1, characterized in that: computer automatically recognizes RIP (RIP) at peak position of product ion peak of reagent ion peak t Setting peak position multiple 0.86 and peak position deviation 0.20, and tracking the peak position interval of the monofluorodichloroethane as RIP t *0.86-0.20ms～RIP t * And (3) finding the highest peak in the peak position interval of the fluorodichloroethane by 0.86+0.20ms, automatically reading the peak high intensity by computer software, obtaining the intensity ratio of the peak high intensity to the reagent ion peak, substituting the ratio into a quantitative curve y=a+c+b, wherein a and b are dimensionless parameters, obtaining the concentration C of the fluorodichloroethane, setting an alarm threshold value of 1%, and automatically alarming by the computer after the concentration C is more than 1%.
7. The monitoring and early warning method according to claim 1, characterized in that: in the detection mode, one or more than two of ketone such as acetone and aromatic hydrocarbon reagent molecules such as toluene are adopted to realize high-sensitivity online monitoring of monofluoro-dichloroethane, the temperature of a migration tube of an ion mobility spectrometry is set to be 40-150 ℃, the opening time of an ion gate is 40-100 mu s, the carrier gas flow rate of the acetone reagent molecules is 20-200ml/min, and a computer with automatic monitoring software is adopted to automatically alarm after the concentration exceeds a threshold value, so that unattended continuous monitoring can be realized, and the method has important safety pre-warning significance for on-site monitoring.
8. The monitoring and early warning method according to claim 1 or 7, characterized in that: and detecting air samples containing monofluorodichloroethane with different concentrations to obtain the intensity ratio of peak high intensity of 1ppm, 5ppm, 10ppm and 100ppm of monofluorodichloroethane to reagent ion peak, and drawing standard curves by taking the concentration (C) and the intensity ratio (y) as abscissa to obtain a quantitative curve y=a+c+b of the monofluorodichloroethane concentration corresponding to the intensity ratio, so as to obtain the parameter values of a and b.
9. The monitoring and early warning method according to claim 1, characterized in that: the specific method is also suitable for on-line monitoring and leakage early warning of halogenated hydrocarbons such as chloromethane, fluorotrichloromethane, chloroethane, chloroethylene or 1, 2-dichloroethane and the like in gas, and different compounds have different specific signal responses.
CN202111492788.9A 2021-12-08 2021-12-08 Online rapid monitoring and early warning method for fluorodichloroethane in air Pending CN116242906A (en)

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