CN112485321A - Ion mobility spectrometry determination method for content of ammonia gas in ammonia-containing gas - Google Patents
Ion mobility spectrometry determination method for content of ammonia gas in ammonia-containing gas Download PDFInfo
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Abstract
The invention provides an ion mobility spectrometry determination method for the content of ammonia in ammonia-containing gas. Pentanone is introduced as a dopant into the whole ion migration tube including a migration region, an ionization region and an ion source through the drift gas of the ion migration tube. Pentanone produces M under the action of photoionization source2H+Ions as reagent ions that react with NH in a high humidity, complex chemical background3High selectivity molecule substitution reaction is carried out to generate NH3Corresponding product ion M (NH)3)H+. The high-concentration pentanone doping agent in the ionization region and the migration region keeps the product ions highly stable in the migration process and is not interfered by high-humidity water vapor and complex chemical matrixes in the background. M (NH) present in the ionization region3)H+The ions pass through the ion gate which is opened periodically, enter the ion migration zone to form ion clusters, and arrive at the ion under the drive of the electric field in the migration zoneAnd the sub-receiving electrode forms a spectrogram of ion current intensity corresponding to ion migration time, so that the ammonia gas is identified and quantified.
Description
Technical Field
The invention relates to NH in the atmosphere3The method for detecting ion mobility spectrometry. In particular to a method for realizing NH in a high-humidity complex chemical background based on a photoionization source technology and a pentanone chemical doping technology3An ion mobility spectrometry method for accurate identification and sensitive quantification.
Background
NH3And organic amine is used as the most important alkaline gas in the atmospheric environment, participates in atmospheric chemical reaction, aggravates the nucleation rate of aerosol and seriously influences the air quality in China. In particular organic amines, having a basicity ratio NH3Stronger, not only easily react with acidic substances and O in the atmosphere3OH radicals and NO3Free radicals and the like are easy to react with granular ammonium salt to generate more stable organic amine salt, so that the nucleation energy barrier is obviously reduced, and the nucleation and growth of new particles are accelerated. Recent external field observations and quantum chemical calculations have further demonstrated NH3And organic amines contribute greatly to the development of haze weather. In addition, NH3And organic amine is gas with foul smell, stimulates olfactory organ, and harms human health and living environment7. The national standard GB14554-93 specifies 8 kinds of malodorous gas NH for limiting emission in plain text3And trimethylamine are 2 of these. Therefore, the real-time monitoring source discharges NH from the aspects of national environmental regulation and treatment and human health3And the concentration level of the organic amine is imperative.
At present, NH3And measurement techniques for organic amines can be divided into two broad categories: an off-line analysis method and an on-line analysis method. NH (NH)3The off-line analysis techniques mainly comprise a nano reagent photometry (GB/T14668 + 1993), a diffusion tube method, an ion chromatography and the like; the off-line analysis technology of the organic amine also comprises a gas chromatography, a gas chromatography-mass spectrometry combination method, a liquid chromatography-mass spectrometry combination method and the like. These analytical methods generally involve complex sample pretreatment processes: first collecting NH in a sample by a solid or liquid medium3And an organic amine, and then analyzed,Extracting or derivatizing, and injecting into an instrument for analysis. These off-line analytical methods are complex to operate, require large amounts of reagents, and do not allow for on-line continuous measurements with a lag in response time.
NH3And the on-line measurement technology of the organic amine mainly comprises a sensor method, a spectrum method, a mass spectrometry method, an ion mobility spectrometry method and the like. The ion mobility spectrometry is a technology for separating and detecting sample ions by a uniform weak electric field according to the difference of ion mobility under atmospheric pressure. The method has the advantages of high detection speed (single detection period is less than 20ms), high sensitivity, easiness in realizing miniaturization, low cost and the like, and is particularly suitable for developing online continuous measurement equipment for ammonia in the atmosphere. In recent years, the emergence of high-selectivity chemical doping photoionization sources, ultrahigh resolution and ultrahigh sensitivity ion mobility region technology enables the ion mobility spectrometry technology to have greater application potential in the field.
Huangwei et al (CN201510890326.0) also used radioactivity63Ni is used as an ionization source of ion mobility spectrometry, and NH is reacted by generating hydrated protons as reaction reagent molecules3On-line monitoring of (2). Dumei et al (201911288763.X) produced hydrated ions as reactive reagent ions in photoionization ion mobility spectrometry by using acetone and water vapor as doping reagents to realize NH pair3Sensitive detection of (3). However, hydrated protons vs. NH3The ionization efficiency of (a) is greatly affected by humidity, and in addition, the resistance to interference of complex chemical backgrounds is poor. Chemical doping of ion sources is an important means to improve ion mobility spectrometry selectivity. Environmental Technologies Group used DMMP as radioactivity in 1991 (US5234838)63Ni ionization source dopant to realize NH3Selective detection of (2); myles et al (Atmospheric. environ.,2006,40,5745) also utilize DMMP as a light source63Doping agent of Ni ionization source for ppb in atmosphere environment by using ion mobility spectrometervMagnitude NH3Long-term monitoring was performed. However, it is possible to use a single-layer,63the radioactivity of the Ni ionization source is an important limiting factor that limits the widespread use of this technology. In addition, whether the doping technique is resistant to humidity versus NH3Detected interference, not reported.
The invention provides a method for detecting NH in atmosphere with high selectivity and high sensitivity based on a photoionization source technology and a chemical doping technology3The ion mobility spectrometry method of (1). Pentanone is introduced as a dopant through a drift gas of the ion transfer tube to the inside of the whole ion transfer tube including a transfer region, an ionization region and an ion source. Pentanone produces M under the action of photoionization source2H+Ions (M stands for pentanone molecules) as reagent ions which can interact with NH in a high humidity, complex chemical background3High selectivity and high efficiency molecular substitution reaction to generate NH3Corresponding product ion M (NH)3)H+. High concentrations of pentanone dopant in the ionization and transport regions can keep the product ions highly stable. And forming a spectrogram of ion current intensity corresponding to ion migration time through the periodically opened ion gate, thereby realizing the identification and quantification of the ammonia gas.
Disclosure of Invention
The invention provides a method for detecting NH in atmosphere with high selectivity and high sensitivity based on a photoionization source technology and a chemical doping technology3The ion mobility spectrometry method realizes NH in high-humidity and complex chemical background3Accurate identification and sensitive quantification.
In order to achieve the purpose, the invention adopts the technical scheme that:
an ion mobility spectrometry determination method for the content of ammonia in ammonia-containing gas comprises an ion mobility tube, wherein the ion mobility tube is a hollow cylindrical cavity formed by alternately overlapping an annular electrode and an annular insulator, a light ion source and an ion receiving electrode are respectively arranged at two ends of the cavity, an ion gate is arranged in the cavity between the light ion source and the ion receiving electrode, the cavity is divided into two areas, a reaction area is formed between the light ion source and the ion gate, and a mobility area is formed between the ion gate and the ion receiving electrode;
a tail gas outlet is arranged on the outer wall surface of the reaction area close to one end of the light ion source, a sample gas inlet is arranged on the outer wall surface of the reaction area close to one end of the ion gate, and a floating gas inlet is arranged on the outer wall surface of the migration area close to one end of the ion receiving electrode;
passing the ammonia-containing gas to be detected through the reaction area at the sample gas inlet;
the floating gas inlet is connected with a floating gas source through a doping reagent generating device, the doping reagent generating device is a closed container with a gas inlet and a gas outlet, the floating gas source is communicated with the gas inlet, the gas outlet is connected with the floating gas inlet through a pipeline, a container filled with pentanone and provided with an opening at the upper end is arranged in the closed container, and volatilized molecules of the pentanone doping reagent are carried to the migration region, the reaction region and the light ion source through the floating gas;
the floating gas is one or more than two of air, nitrogen, helium and argon; adding 30-100ppm pentanone molecules, preferably 40-60ppm pentanone molecules in final volume concentration into the bleaching gas;
the doped reagent pentanone molecule generates high-concentration reaction reagent ions M under the action of a light ion source2H+(M represents a pentanone molecule) and migrates towards the ion gate driven by an electric field in the ionization region; carrying ammonia molecules (NH)3) The sample gas enters the reaction zone through the sample gas inlet, and the reagent ions M react2H+With ammonia molecules (NH)3) High selectivity molecule substitution reaction is carried out to generate ammonia molecule (NH)3) Corresponding product ion M (NH)3)H+Meanwhile, the molecular-ion reaction of high humidity and other complex chemical components in the sample gas is prevented, and the interference of the molecular-ion reaction on the ammonia molecule ionization process is eliminated;
m (NH) in the reaction zone3)H+Ions enter the migration region through the periodically opened ion gate to form ion clusters, the ion clusters are kept stable in the atmosphere of high-concentration pentanone molecules in the migration region and reach the ion receiving electrode under the drive of an electric field in the migration region to form a spectrogram of ion current intensity corresponding to ion migration time, and ammonia molecules (NH) are subjected to ion bombardment3) Qualitative and quantitative identification.
The light ion source is any light source with the energy of emitted photons higher than 9.5 eV; the ion gate is a Tyndall-Powell type ion gate.
The sample gas inlet amount of the sample gas at the sample gas inlet is 50-100ml/min, and the sample gas inlet amount of the floating gas inlet is 100-300 ml/min.
The invention has the advantages that:
the invention combines the photoionization power technology and the pentanone chemical doping technology, and solves NH in high humidity and complex chemical background by using the pentanone as the chemical dopant in the whole ion migration tube3Accurate identification and sensitive quantification.
The invention is described in further detail below with reference to the accompanying drawings:
drawings
FIG. 1 is a schematic diagram of the structure of ion mobility spectrometry disclosed in the present invention. Wherein: 1. a source of photo-ions; 2. an ionization region; 3. an ion gate; 4. a migration zone; 5. an ion receiving electrode; 6. a float gas inlet; 7. a sample gas inlet; 8. an air outlet; 9. doping agent generating device.
FIG. 2 is a response spectrum of 50ppb ammonia gas in sample gas with different humidities.
FIG. 3 shows the response characteristics of 50ppb ammonia in sample gases containing different chemical interferences.
FIG. 4 is a linear response range of the disclosed method to ammonia gas.
FIG. 5 shows the results of on-line monitoring of the volatility of ammonia in a toilet from 12.00 am to 04:00 am.
Detailed Description
Example 1
An ion mobility tube used with the present invention is shown in fig. 1. The light ion source 1 of the ion transfer tube is a VUV Kr lamp of 10.6 eV; the ion gate 3 is a Tyndall-Powell type ion gate; the ion receiving electrode 5 is a Faraday disc with the diameter of 6mm and is fixed on a metal shielding cylinder with the outer diameter of 30 mm. The ionization region 2 and the migration region 4 are respectively formed by alternately overlapping annular conductive pole pieces with the thickness of 1mm, the inner diameter of 20mm and the outer diameter of 30mm and annular insulating pole pieces with the thickness of 4mm, the inner diameter of 20mm and the outer diameter of 30mm, the length of the ionization region 2 is 40mm, and the length of the migration region 4 is 60 mm; the shielding cylinders of the light ion source 1, the annular conductive pole piece and the ion receiving electrode 5 are electrically connected with a high-voltage output terminal of a high-voltage power supply and the ground through a voltage dividing resistor chain formed by connecting end to end 2M omega resistors; the output value of the high-voltage power supply is 10500V, and a migration electric field of 1000V/cm is formed in the ion migration tube; the temperature of the ion transfer tube was set to 150 ℃.
A tail gas outlet 8 is arranged on the outer wall surface of one end of the reaction zone 2 close to the light ion source 1, a sample gas inlet 7 is arranged on the outer wall surface of one end of the reaction zone 2 close to the ion gate 3, and a floating gas inlet 6 is arranged on the outer wall surface of one end of the migration zone 4 close to the ion receiving electrode 5;
the ammonia-containing gas to be detected passes through the reaction area 2 at the sample gas inlet 7;
the floating gas inlet 6 is connected with a floating gas source through a doping reagent generating device 9, the doping reagent generating device 9 is a closed container with a gas inlet and a gas outlet, the floating gas source is communicated with the gas inlet, the gas outlet is connected with the floating gas inlet 6 through a pipeline, a container filled with pentanone and provided with an opening at the upper end is arranged in the closed container, and volatilized doping reagent pentanone molecules are carried to the migration zone 4, the reaction zone 2 and the light ion source 1 through the floating gas;
the floating gas is 200mL/min to purify air, the concentration of pentanone molecules in the floating gas is 50ppm after the floating gas passes through the doping reagent generating device 9, the flow rate of the sample gas is 50mL/min, the floating gas and the sample gas enter the reaction zone 2 of the ion migration tube through the sample gas inlet 7, and the floating gas and the sample gas finally flow out of the ion migration tube through the tail gas outlet 8;
the doped reagent pentanone molecule generates high-concentration reaction reagent ions M under the action of the photoionization source 12H+(M represents a pentanone molecule) and migrates towards the ion gate 3 driven by an electric field in the ionization region; carrying ammonia molecules (NH)3) The sample gas enters the reaction area 2 through the sample gas inlet 7, and the reagent ions M2H+With ammonia molecules (NH)3) High selectivity molecule substitution reaction is carried out to generate ammonia molecule (NH)3) Corresponding product ion M (NH)3)H+Meanwhile, the ionization of high humidity and complex chemical components in the sample gas is inhibited;
m (NH) in reaction zone 23)H+Ions enter the migration region 4 through the periodically opened ion gate 3 to form ion clusters, the ion clusters are kept stable in the atmosphere of high-concentration pentanone molecules in the migration region 4 and reach the ion receiving electrode 5 under the drive of the electric field in the migration region 4, and the ion current intensity corresponding to the ion migration time is formedSpectrum, realization of ammonia molecule (NH)3) Qualitative and quantitative identification of (a);
example 2
FIG. 2 shows the 50ppb of sample gas at different humiditiesvResponse spectrum of ammonia. It can be seen that the ion peak intensity of ammonia remains substantially unchanged as humidity increases from RH 11% to RH 99%, demonstrating that this method can eliminate the effect of humidity on ammonia detection.
Example 3
FIG. 3 shows that 50ppb of methanol, ethanol, propionaldehyde and dichloromethane are added as chemical interference agents to a sample gasvVariation of the ammonia ion peak intensity. Notably, 50ppbvThe ion peak intensity of ammonia gas is basically kept unchanged, which shows that the method disclosed by the invention can overcome the influence of the chemical interference agents on ammonia gas detection.
Example 4
Figure 4 shows the linear response range of the disclosed method to ammonia. The method can be used for the concentration of 20ppbv～800ppbvAmmonia in the range responds linearly. The linear range meets the requirement of quantitative detection of trace ammonia in the atmosphere.
Example 5
FIG. 5 shows the results of the disclosed method for on-line monitoring of ammonia gas concentration in a toilet from 12:00 a.m. to 04:00 a.m., from which a clear change in ammonia gas concentration is observed.
Comparative example 1
In order to show that pentanone is used as a chemical doping reagent in the method, the influence of humidity, chemical matrix and the like on the ammonia gas response in the sample gas when acetone, 2-butanone, toluene, anisole and the like are used as the chemical doping reagent is simultaneously tested in an experiment. As a result, when acetone, 2-butanone, toluene or anisole was used as a chemical doping agent, 50ppb was not observed when the humidity of the sample gas was increased to RH 50% or morevProduct ion peak of ammonia gas. Similarly, when acetone, 2-butanone, toluene or anisole is used as chemical doping agent, it is unable to completely overcome the chemical interference pairs such as alcohols, chlorinated hydrocarbons, aromatic hydrocarbons, etcInfluence of ammonia detection.
Claims (3)
1. An ion mobility spectrometry determination method for the content of ammonia in ammonia-containing gas is characterized in that:
the ion mobility spectrometry comprises an ion mobility tube, the ion mobility tube is a hollow cylindrical cavity formed by alternately overlapping annular electrodes and annular insulators, a light ion source (1) and an ion receiving electrode (5) are respectively arranged at two ends of the cavity, an ion gate (3) is arranged in the cavity between the light ion source (1) and the ion receiving electrode (5), the cavity is divided into two regions, a reaction region (2) is formed between the light ion source (1) and the ion gate (3), and a mobility region (4) is formed between the ion gate (3) and the ion receiving electrode (5);
a tail gas outlet (8) is arranged on the outer wall surface of one end of the reaction area (2) close to the light ion source (1), a sample gas inlet (7) is arranged on the outer wall surface of one end of the reaction area (2) close to the ion gate (3), and a floating gas inlet (6) is arranged on the outer wall surface of one end of the migration area (4) close to the ion receiving electrode (5);
the ammonia-containing gas to be detected passes through the reaction area (2) at the sample gas inlet (7);
the floating gas inlet (6) is connected with a floating gas source through a doping reagent generating device (9), the doping reagent generating device (9) is a closed container with a gas inlet and a gas outlet, the floating gas source is communicated with the gas inlet, the gas outlet is connected with the floating gas inlet (6) through a pipeline, a container filled with pentanone and provided with an opening at the upper end is placed in the closed container, and volatilized doping reagent pentanone molecules are carried to the migration zone (4), the reaction zone (2) and the light ion source (1) through the floating gas;
the floating gas is one or more than two of air, nitrogen, helium and argon; adding 30-100ppm pentanone molecules, preferably 40-60ppm pentanone molecules in final volume concentration into the bleaching gas;
the doped reagent pentanone molecule generates high-concentration reaction reagent ions M under the action of the light ion source (1)2H+(M represents a pentanone molecule) and migrates towards the ion gate (3) driven by an electric field in the ionization region; carrying ammonia molecules (NH)3) The sample gas enters the reaction area (2) through the sample gas inlet (7) and reacts with reagent ions M2H+With ammonia molecules (NH)3) High selectivity molecule substitution reaction is carried out to generate ammonia molecule (NH)3) Corresponding product ion M (NH)3)H+Meanwhile, the molecular-ion reaction of high humidity and other complex chemical components in the sample gas is prevented, and the interference of the molecular-ion reaction on the ammonia molecule ionization process is eliminated;
m (NH) in the reaction zone (2)3)H+Ions enter the migration region (4) through the periodically opened ion gate (3) to form ion clusters, the ion clusters are kept stable in the atmosphere of high-concentration pentanone molecules in the migration region (4) and reach the ion receiving electrode (5) under the drive of an electric field in the migration region (4), a spectrogram of ion current intensity corresponding to ion migration time is formed, and ammonia molecules (NH) are subjected to ion transfer3) Qualitative and quantitative identification.
2. The ion mobility spectrometry method according to claim 1, wherein: the light ion source (1) is any light source with the energy of emitted photons higher than 9.5 eV; the ion gate (3) is a Tyndall-Powell type ion gate.
3. The ion mobility spectrometry method according to claim 1 or 2, characterized in that: the sample gas inlet amount of the sample gas inlet (7) is 50-100ml/min, and the floating gas inlet amount of the floating gas inlet (6) is 100-300 ml/min.
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