CN118209619A - Device and method for measuring hydrogen chloride with high sensitivity by using ion mobility spectrometry of non-radioactive ionization source - Google Patents
Device and method for measuring hydrogen chloride with high sensitivity by using ion mobility spectrometry of non-radioactive ionization source Download PDFInfo
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- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 62
- 238000001871 ion mobility spectroscopy Methods 0.000 title claims abstract description 48
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- GBZANUMDJPCQHY-UHFFFAOYSA-L mercury(ii) thiocyanate Chemical compound [Hg+2].[S-]C#N.[S-]C#N GBZANUMDJPCQHY-UHFFFAOYSA-L 0.000 description 3
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Abstract
The invention discloses a device and a method for measuring hydrogen chloride in an atmospheric environment with high sensitivity by using a VUV lamp-ion mobility spectrometry. The invention is based on anion mode ion mobility spectrometry, a novel Vacuum Ultraviolet (VUV) lamp ionization source is adopted, reagent ions are generated by auxiliary reagent molecules such as acetone and the like in organic compounds with ionization energy smaller than 10.04ev in carrier gas of IMS, then the reagent ions react with hydrogen chloride in a sample to generate chloride ions, finally the ions enter an ion mobility tube, are separated in a uniform electric field, and sequentially reach a Faraday disc in the mobility tube to be detected. The method realizes on-line monitoring of HCl based on a VUV-ion migration method, has the remarkable advantages of high resolution, high sensitivity and real-time monitoring, can detect the content of hydrogen chloride in different environments, has high response speed, and has wide application prospect for detecting the content of hydrogen chloride in the air on line in real time.
Description
Technical Field
The invention relates to a device and a method for measuring hydrogen chloride with high sensitivity by using a non-radioactive ionization source ion mobility spectrometry, and belongs to the technical field of ion mobility spectrometer analysis.
Background
Chlor-alkali is widely used in many industrial processes such as chemical synthesis, oil refining, bleaching, pharmaceutical and water and wastewater disinfection. About 7000 ten thousand tons of chlorine were produced in 2015, and 2024 would be expected to exceed 10000 ten thousand tons. Hydrogen chloride is a common chemical raw material and a product of a chemical production process, such as metal cleaning, polyvinyl chloride, synthetic rubber and the like. And can be used for batteries, medicines, dyes, fertilizers, glass processing, metal cleaning, organic synthesis, corrosion imaging, ceramic manufacturing, food processing, inorganic chloride manufacturing, rubber, catalysts, electron gases, standard gases, epitaxy, diffusion, oxidation, etching, chemical vapor deposition, light emitting diodes, and the like.
The maximum allowable emission concentration of hydrogen chloride is 150mg/m 3, as specified by the integrated emission Standard for atmospheric pollutants (GB 16297-1996). The gas is colorless non-flammable gas, has a pungent smell, is white smoke in the air, is very easy to dissolve in water to form hydrochloric acid, has strong corrosiveness, and can react with various metals to generate hydrogen. And can form explosive mixture with air to produce highly toxic hydrogen cyanide when meeting cyanide. Most of the hydrogen chloride is retained by the upper respiratory tract mucosa after being inhaled and is neutralized, so that the hydrogen chloride has stimulation and cauterization effects on local mucosa, and causes inflammatory edema, congestion and necrosis to damage human health. HC1 has become the preferred industrial toxic and harmful exhaust gas monitoring object for the environmental protection organizations around the world. Therefore, the method has important practical significance in detecting the hydrogen chloride in real time.
At present, a plurality of standard methods for measuring the content of the hydrogen chloride gas at home and abroad are available, such as a mercury thiocyanate colorimetric method, an ion selective electrode method and the like. The mercury thiocyanate colorimetric method and the selective electrode method have the characteristics of accuracy, sensitivity, simplicity, convenience and the like, but cannot realize online real-time monitoring, a sample is required to be sent to a laboratory after being collected, the process is extremely tedious, and other interferences can be generated in the transportation process. Other detection methods are spectroscopy, electrochemical sensors and wet chemistry. Spectroscopic methods such as high resolution infrared emission spectroscopy, tuned Diode Laser Absorption Spectroscopy (TDLAS), spectrophotometry, and the like. The method has the advantages of high accuracy, high response speed, high sensitivity and the like, but the signal acquisition system is complex due to huge volume, and the on-site rapid detection is difficult to realize. The electrochemical sensor method instrument has the advantages of miniaturization and portability, but has poor gas selectivity and higher detection limit (more than 1 ppm), and is difficult to detect low-concentration hydrogen chloride. However, the wet chemical method requires manual experiments to complete detection, and has the advantage of high precision, but also has the limitation that real-time monitoring cannot be realized.
The invention develops a novel method for measuring hydrogen chloride with high sensitivity by using a non-radioactive ionization source ion mobility spectrometry based on an ion mobility spectrometry technology (Ion Mobility Spectrometry, IMS) with high sensitivity and quick response time. The sensitivity can reach 8.23mv/ppb, the response time is less than 1s, the detection limit is better than 1ppb, and compared with the traditional method, the method has obvious advantages and wide application prospect.
Disclosure of Invention
The invention relates to a device and a method for measuring hydrogen chloride with high sensitivity by ion mobility spectrometry of a non-radioactive ionization source.
The technical scheme adopted by the invention is as follows:
the invention provides a high-sensitivity hydrogen chloride measuring and detecting device for ion mobility spectrometry of a non-radioactive ionization source, which comprises an ionization region narrowing anion mode photoionization ion mobility spectrometry, a flowmeter, a doping agent, a tail gas pump, a gas source and a three-way joint, wherein the negative ion mode photoionization ion mobility spectrometry comprises a gas source, a gas source and a gas-liquid separator;
the ion mobility spectrometry is a hollow cavity formed by coaxially and alternately placing, extruding and sealing an insulating ring and an electrode ring; an ionization source is arranged at one end of the ion mobility spectrometry, and a tail gas interface 9, a carrier gas inlet 5 and a sample inlet 8 are sequentially arranged on one side, close to the ionization source, of the outer wall of the ion mobility spectrometry; the carrier gas inlet 5 is sequentially connected with the doping agent 4 and the flowmeter II 3; the sample inlet 8 is connected with one end of the three-way joint 7, and the other end of the three-way joint 7 is connected with the sample gas 6; and a drift gas inlet 2 is arranged on the outer wall of the other end of the ion mobility spectrometry. The reason for using the three-way joint is that the ion mobility spectrometry adopts atmospheric pressure for sampling, and the three-way joint is not connected with a gas path end so as to ensure that the sample is sampled under the atmospheric pressure condition.
Further, in the above technical solution, the exhaust port 9 is sequentially connected with a flow meter iii 10 and an air pump 11; the floating gas inlet 2 is connected with a flowmeter I1.
The invention also provides a method for measuring hydrogen chloride with high sensitivity by adopting the device, and a gas sample enters an ion mobility spectrometer through the tee joint 7 and the sample port 8; the drift gas is controlled to enter the ion mobility spectrometry through a drift gas inlet 2 by a flowmeter I1; the doping agent 4 is purged by air and is controlled to enter the ion mobility spectrometry through a carrier gas port 5 by a flowmeter II 3; the tail gas from the tail gas port 9 is discharged from the air pump 11 through the flowmeter III 10. Dopant molecules in the dopant 4 enter the ion mobility spectrometry from a carrier gas port 5. The reagent molecules first generate sufficient reagent ions by direct photoionization, followed by ionization of the sample molecules by molecular-ion reaction of the reagent ions with the sample molecules. Sample ions reach the Faraday disc through the migration area to be detected, and the ion migration spectrogram of the hydrogen chloride is obtained through the signal amplifier and the signal acquisition and display device.
Further, in the above technical solution, the ion mobility spectrometry ionization source is a vacuum ultraviolet lamp; the working mode is an anion mode; the flow rate of the floating gas is 300-400 ml/min, the sample injection flow rate is 300-400 ml/min, and the flow rate of the carrier gas is 100-150 ml/min.
Further, in the above technical solution, the bleaching gas is purified dry air, and the carrier gas is purified dry air gas for blowing the dopant; the purified dry air is the dry air treated by the molecular sieve; the dopant molecule is acetone.
Further, in the above technical scheme, when sample is introduced, hydrogen chloride sample gas is sampled by inhalation under atmospheric pressure to enter an ion mobility spectrometry, reagent molecules are firstly ionized by direct photoionization to generate enough reagent ions, and then the ionization of the sample molecules is realized by the molecular-ion reaction of the reagent ions and the sample molecules. Sample ions pass through the migration zone to reach the Faraday plate to be detected. Further, in the above technical scheme, the standard gas of hydrogen chloride is measured with high sensitivity by using the ion mobility spectrometry of a non-radioactive ionization source, and the obtained ion mobility spectrometry of hydrogen chloride is then used for qualitatively detecting the hydrogen chloride according to the time position of Cl - in the spectrometry. The intensities of the peaks of the series Cl - at the time positions in the spectrogram were obtained by measuring the standard gas of the series concentration of hydrogen chloride, and a standard curve of the measurement of hydrogen chloride was made from a simulated curve of peak intensity-concentration. When an unknown sample is measured, the content level of hydrogen chloride in the sample can be obtained through the intensity of the peak at the position.
The method adopts a non-radioactive novel radio frequency Vacuum Ultraviolet (VUV) lamp ionization source and is based on ion mobility spectrometry of negative ion mode. First, the ultraviolet rays emitted from the VUV lamp irradiate reagent molecules having ionization energy lower than photon energy, and the reagent molecules are photoionization-generated a large amount of low-energy electrons. Oxygen molecules and ozone molecules in the air can capture low-energy electrons generated by photoionization of reagent molecules to form O 2 - and O 3 -, the formed O 2 - and O 3 - can be combined with trace water molecules in the air to form corresponding hydrated ions O 2 -(H2O)n and O 3 -(H2O)m, as the electron affinity of ozone is higher than that of the oxygen molecules, O 2 -(H2O)n can generate charge transfer reaction with ozone to form partial O 3 -(H2O)n, since the air contains about 300ppm of CO 2, the formed O 3 -(H2O)n can be rapidly converted into CO 3 -(H2O)n.O2 -(H2O)n (hereinafter referred to as O 2 -) and CO 3 -(H2O)n (hereinafter referred to as CO 3 -) at 0.4 mu s, namely two reagent ions. Wherein the ionization effect of CO 3 - on HCl is not obvious, the drift gas flow rate is improved by reducing the inner diameter of the ionization region, the generated O 3 molecules are taken away rapidly, the product concentration of CO 3 - is reduced, the output of O 2 - is improved, and the ionization efficiency on HCl is improved. Ionization of HCl is mainly dependent on O 2 - and its ionization formula is shown as follows:
HCl+O2 -(H2O)n→Cl-+O2+n H2O
Under the action of a radio frequency vacuum ultraviolet lamp, organic compounds with ionization energy smaller than 10.04ev such as acetone are ionized to give electrons, oxygen in the bleaching gas is used for ionization to generate reagent ions O 2 -, then the reagent ions O 2 - react with a sample to enable hydrogen chloride therein to generate Cl -, then the Cl - reacts with hydrogen chloride in the sample to generate chloride ions, finally the ions enter an ion migration tube to be separated in a uniform electric field, and finally the ions reach a Faraday disc in the migration tube successively to be detected.
The invention has the beneficial effects that
1. The method greatly improves the sensitivity of hydrogen chloride gas detection, can reach 3.73mv/ppb, has the detection limit of 0.048ppb, can completely realize on-site real-time monitoring, eliminates a part of possible interference of the added dopant molecules, is more accurate and reliable in detection, and has the problems that the on-line monitoring of hydrogen chloride cannot be realized, the sensitivity is lower and the like compared with the traditional detection methods such as an ion selective electrode method, a mercury thiocyanate colorimetric method, an ion chromatographic method and the like.
2. The method has extremely high analysis speed and response time of <1s, and can meet the requirements of monitoring the hydrogen chloride content in industrial parks and production workshops and early warning of leakage.
3. The method has the advantages of simple operation, simple and quick instrument, small volume and easy carrying, and is suitable for on-site on-line monitoring of hydrogen chloride in various environments.
Drawings
FIG. 1 is a block diagram of a method for detecting hydrogen chloride gas in a high sensitivity hydrogen chloride measurement method by ion mobility spectrometry of a non-radioactive ionization source;
the device comprises a 1-flowmeter I, a 2-bleaching gas inlet, a 3-flowmeter II, a 4-doping agent, a 5-carrier gas inlet, a 6-sample gas, a 7-three-way joint, an 8-sample inlet, a 9-tail gas interface, a 10-flowmeter III and an 11-air pump.
Fig. 2 is a background spectrum of ion mobility spectrometry when acetone is used as a dopant.
FIG. 3 is a standard spectrum of ion mobility spectrometry for hydrogen chloride.
Fig. 4 is a standard curve of the rf lamp vacuum uv lamp ionization source ion mobility spectrometry for hydrogen chloride.
Detailed Description
The following examples illustrate the use of the invention, but do not limit the scope of application.
Example 1
As shown in figure 1, the device for measuring the hydrogen chloride with high sensitivity by using the ion mobility spectrometry of the non-radioactive ionization source comprises an anion mode ion mobility spectrometry with a narrowed ionization region, a flowmeter, a doping agent, a tail gas pump, a gas source and a three-way joint;
The ion mobility spectrometry comprises a hollow cavity formed by coaxially and alternately placing, extruding and sealing an insulating ring and an electrode ring; an ionization source is arranged at one end of the photoionization migration spectrum, and a tail gas interface 9, a carrier gas inlet 5 and a sample inlet 8 are sequentially arranged on one side, close to the ionization source, of the outer wall of the photoionization migration spectrum; the carrier gas inlet 5 is sequentially connected with the doping agent 4 and the flowmeter II 3; the sample inlet 8 is connected with one end of the three-way joint 7, and the other end of the three-way joint 7 is connected with the sample gas 6; and a drift gas inlet 2 is arranged on the outer wall of the other end of the ion mobility spectrometry.
The tail gas interface 9 is sequentially connected with a flowmeter III 10 and an air pump 11; the floating gas inlet 2 is connected with a flowmeter I1.
Example 2
Comprises a newly designed ionization region narrowing anion mode ion mobility spectrometry, a flowmeter, a molecular sieve, a tail gas pump, a gas source and a three-way joint; the ion mobility spectrometry comprises four air ports, wherein a tail gas interface 9, a carrier gas inlet 5, a sample inlet 8 and a drift gas inlet 2 are sequentially arranged from left to right, clean air is taken as drift gas and enters from the drift gas inlet 2 of the ion mobility spectrometry through a flowmeter I1, and carrier gas is taken from the carrier gas inlet 5 of the ion mobility spectrometry through a flowmeter II 3 with a doping agent 4; the sample gas 6 is communicated with a sample inlet 8 of the anion mode photoionization mobility spectrometry through a three-way joint 7; the air pump 11 is connected with the tail gas interface 9 of the ion transition spectrum through the flowmeter III (10).
Example 3
A novel method for measuring hydrogen chloride with high sensitivity by adopting a non-radioactive ionization source ion mobility spectrometry adopts a radio-frequency non-radioactive ionization source VUV lamp as an ionization source, the voltage of a migration area is set to 600V/cm, the drift gas flow is set to 400ml/min, the tail gas flow is set to 850m/min, the sampling amount is 300ml/min, and the background spectrogram of the instrument is shown in figure 2 when the carrier gas flow is 150 ml/min. By dynamically diluting the gas distribution system, and taking dry clean air as diluent gas to prepare 50ppb concentration HCl standard gas, a new peak appears at 2.325ms when the sample contains hydrogen chloride component, the peak is a spectrum peak of Cl -, and the intensity of the peak can be used for representing the content of hydrogen chloride as shown in figure 3.
Example 4
The dynamic dilution gas distribution system is adopted, dry clean air is used as dilution gas, and standard gas of chlorine with a series of concentrations is prepared: 10ppb, 20ppb, 30ppb, 40ppb, 50ppb. The method is used for detection, and an ion mobility spectrum of the hydrogen chloride standard gas with the concentration is obtained. The intensity of 2.325ms ion spectrum peak is extracted, the intensity of the peak is plotted with the corresponding concentration, and a calibration curve for detecting hydrogen chloride by an ion mobility spectrometry is obtained, as shown in fig. 4, the detection limit of hydrogen chloride gas reaches 0.048ppb, and the sensitivity can reach 3.73mv/ppb as can be seen from fig. 4.
The description is made for the purpose of illustrating the general principles of the invention and should not be taken in any way as limiting the scope of the invention. Other embodiments of the invention will occur to those skilled in the art from consideration of this specification without the exercise of inventive faculty, and such equivalent modifications and alternatives are intended to be included within the scope of the invention as defined in the claims appended hereto.
Claims (8)
1. The device for measuring hydrogen chloride with high sensitivity by using the ion mobility spectrometry of the non-radioactive ionization source is characterized by comprising a hollow cavity formed by coaxially and alternately placing, extruding and sealing an insulating ring and an electrode ring; one end of the ion mobility spectrometry is provided with an ionization source, and one side, close to the ionization source, of the outer wall of the ion mobility spectrometry is sequentially provided with a tail gas interface (9), a carrier gas inlet (5) and a sample inlet (8); the carrier gas inlet (5) is sequentially connected with the doping agent (4) and the flowmeter II (3); the sample inlet (8) is connected with an interface at one end of the three-way joint (7), and the other end of the three-way joint (7) is connected with the sample gas (6); a drift gas inlet (2) connected with a flowmeter I (1) is arranged on the outer wall of the other end of the ion mobility spectrometry.
2. The device according to claim 1, characterized in that the exhaust gas interface (9) is connected in sequence to a flow meter iii (10) and an extraction pump (11); the floating gas inlet (2) is connected with the flowmeter I (1).
3. A method for highly sensitively measuring hydrogen chloride using the apparatus according to any one of claims 1 to 2, characterized in that: sample gas (6) enters an ion mobility spectrometry through a three-way joint (7) and a sample port (8); the drift gas is controlled to enter the ion mobility spectrometry through a drift gas inlet (2) by a flowmeter I (1); the doping agent (4) is purged by air, and is controlled to enter the ion mobility spectrometry through a carrier gas port (5) by a flowmeter II (3); the tail gas of the tail gas port (9) is discharged by a suction pump (11) through a flowmeter III (10). Dopant molecules in the dopant (4) enter an ion mobility spectrum from a carrier gas port (5); the reagent molecules first generate sufficient reagent ions by direct photoionization, followed by ionization of the sample molecules by molecular-ion reaction of the reagent ions with the sample molecules. Sample ions reach the Faraday disc through the migration area to be detected, and the ion migration spectrogram of the hydrogen chloride is obtained through the signal amplifier and the signal acquisition and display device.
4. A method of measuring hydrogen chloride according to claim 3, wherein the ion mobility spectrum is a photoionization ion mobility spectrum; the ion mobility spectrometry ionization source is a vacuum ultraviolet lamp; the working mode is an anion mode; the flow rate of the floating gas is 300-400 ml/min, the sample injection flow rate is 300-400 ml/min, and the flow rate of the carrier gas is 100-150 ml/min.
5.A method of measuring hydrogen chloride according to claim 3, wherein the bleaching gas is purified dry air; the carrier gas is purified dry air for sweeping the doping agent; the purified dry air is the dry air treated by the molecular sieve.
6. A method of measuring hydrogen chloride according to claim 3, wherein the dopant molecule is an ionizable organic solvent which is acetone.
7. A method for measuring hydrogen chloride according to claim 3, characterized in that, in the sample injection, the sample gas (6) is sampled by inhalation at atmospheric pressure into the ionization ion mobility spectrum, the reagent molecules are first subjected to direct photoionization to generate sufficient reagent ions, then the ionization of the sample molecules is realized by the molecular-ionic reaction of the reagent ions with the sample molecules, and the sample ions reach the faraday plate through the mobility area to be detected.
8. A method of measuring hydrogen chloride according to claim 3, wherein the standard gas of hydrogen chloride is measured by ionization ion mobility spectrometry using a non-radioactive ionization source, an ion mobility spectrum of hydrogen chloride is obtained, then hydrogen chloride is qualitatively detected according to a mobility time position of Cl - in the spectrum, an intensity of a peak at a time position in the spectrum of the series Cl - is obtained, and a standard curve of hydrogen chloride measurement is made according to a simulated curve of peak intensity-concentration; when measuring an unknown sample, the content level of hydrogen chloride in the sample is obtained by the intensity of the peak at the Cl - response time of the unknown sample.
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