CN216747541U - Ion-molecule reaction selection control measuring device based on ion mobility spectrometry - Google Patents
Ion-molecule reaction selection control measuring device based on ion mobility spectrometry Download PDFInfo
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Abstract
The utility model provides an ion-molecule reaction selection control measuring device based on ion mobility spectrometry. Initial reaction reagent ions generated by the ion source are enriched in the first ionization region and injected into the first migration region through the first ion gate to carry out ultrahigh-resolution ion mobility separation; the first migration region cooperates with the first and second ion gates to have a mobility ofKThe reaction reagent ions selectively pass through the second ion gate and enter the second ionization region to perform ion-molecule reaction with target sample molecules; injecting product ions of the ion-molecule reaction in the second ionization region into the second migration region through a third ion gate for separation and detection to obtain an ion mobility spectrum of the product ions;the ion-molecule reaction between the selected reaction reagent ions and the target sample molecules in the second ionization region can be measured and researched by utilizing the obtained ion mobility spectrum of the product ions.
Description
Technical Field
The utility model relates to a measuring device for an ion-molecule reaction rate constant in the field of physical chemistry, in particular to an ion-molecule reaction selective control measuring device based on a cascade ion mobility spectrometry technology.
Background
The atmospheric pressure ion source working under atmospheric pressure and sub-atmospheric pressure is a hot spot of recent research in the fields of mass spectrum and ion mobility spectrometry, and hundreds of novel ionization source technologies are developed, including electrospray ionization source ESI, analytic electrospray ionization source DESI, secondary electrospray ionization source SESI, low-temperature plasma ionization source LTP, direct online analysis ionization source DART and the like.
The same ionization source can vary greatly from instrument to instrument, and different types of ionization sources sometimes measure ionization products and have similar efficiencies. Such as: how gas phase protein ions are released from charged droplets in ESI ionization sources still does not gain a unified understanding, while ESI ionization efficiencies of different research teams differ by 6 orders of magnitude (j.am.soc.mass spectra.2019, 30: 1069); secondary electrospray ionization sources (SESI) and electrospray extraction ionization sources (EESI) developed by chenghu, professor Renato, etc. have been widely used in field analyses such as exhaled breath, medicine, and living body analysis, but there is still a big debate as to whether gas phase ion-molecule reactions occur in EESI and whether there is interaction between droplets in liquid phase (anal. chem.2010,82: 4494). In addition, Blanco et al found that the air pressure in the SESI ionization source had a great influence on the ionization efficiency, and the ionization efficiency of the TNT reducing air pressure reached 1/700(anal. chem.2012,84: 8475); we have recently found that the intensity of ions in Vacuum Ultraviolet (VUV) photoionization and photochemical ionization sources does not vary linearly with ionization region pressure, but increases exponentially (anal. chem.2018,90: 5398). Introducing high-concentration CH into high-pressure VUV photoionization source by professor fascicularis2Cl2And H2After O reagent molecules, an abnormally high-efficiency ionization phenomenon is also found, namely paranitrateThe ionization efficiency of the base compound is as high as 28% (chem. Commun.2006,19:2042), but the mechanism of enhancement is still unclear. This is mainly because the atmospheric pressure ion source generally generates complex reagent ions under atmospheric pressure and sub-atmospheric pressure conditions, and the clustering level of the reagent ions is greatly influenced by factors such as ambient humidity and background of gas atmosphere. The practical problem causes serious troubles for accurately analyzing an ion-molecule reaction mechanism in the ion source and designing a special high-efficiency ionization source.
At present, selective ion flow tube mass spectrometry (SIFT-MS) is an important technology for researching the ion-molecule reaction process in the atmospheric pressure ion source. SIFT-MS utilizes a quadrupole rod to carry out mass-to-charge ratio m/z screening on reaction reagent ions generated in an atmospheric pressure ionization source, and the reaction reagent ions are sent into an ion-molecule reaction tube to carry out reaction characteristic research. However, the working air pressure of the quadrupole mass filter and the ion-molecule reaction tube in the SIFT-MS is usually in the range of hectopascal, the difference between the selected reactive reagent ions and the original clustering state of the selected reactive reagent ions in the normal pressure ion source is large, and the experimental result is difficult to reflect the real process of the ion-molecule reaction in the normal pressure ion source.
The ionization mechanism of ions in the atmospheric pressure source is not only related to the species of the core ions, but also the size of the reactant ions and the reaction time (t)rL/KE) and the ion mobility K characterizes these physical parameters and can be measured experimentally with precision. The method has the advantages that the change trend of the mobility of the reaction ions along with the change of air pressure, temperature, humidity and the like is accurately measured, particularly, the reaction ions are screened based on the accurate mobility to develop the research rate constant and the reaction molecular ratio of the ion-molecule reaction, the reaction mechanism and the influence factors thereof are deeply known, and the comprehensive optimization of the ionization source is realized.
Disclosure of Invention
The utility model provides an ion-molecule reaction selection control measuring device based on ion mobility spectrometry. The ion migration tube is divided into four sequentially adjacent areas, namely a first ionization area, a first migration area, a second ionization area and a second migration area, by arranging three first ion gates, three second ion gates and three third ion gates which are arranged in parallel at intervals in the same ion migration tube. Initial reaction reagent ions generated by the ion source are enriched in the first ionization region and injected into the first migration region through the first ion gate to carry out ultrahigh-resolution ion mobility separation; the first migration area, the first ion gate and the second ion gate work cooperatively, so that reaction reagent ions with the mobility K pass through the second ion gate in a high selectivity manner and enter the second ionization area to perform ion-molecule reaction with target sample molecules; injecting product ions of the ion-molecule reaction in the second ionization region into the second migration region through a third ion gate for separation and detection to obtain an ion mobility spectrum of the product ions; the ion-molecule reaction between the selected reaction reagent ions and the target sample molecules in the second ionization region can be measured and researched by utilizing the obtained ion mobility spectrum of the product ions.
In order to achieve the purpose, the utility model adopts the technical scheme that:
an ion-molecule reaction selection control measuring device based on ion mobility spectrometry comprises an ion mobility tube, wherein the ion mobility tube is a hollow cylindrical cavity formed by sequentially, alternately and coaxially overlapping an annular electrode and an annular insulator, and an ion source and an ion receiving electrode are respectively arranged at two ends of the cavity;
the ion source and the ion receiving electrode are positioned in the columnar cavity, a first ion gate, a second ion gate and a third ion gate are sequentially arranged along the direction from the ion source to the ion receiving electrode, the interior of the columnar cavity is divided into four regions, a first ionization region is formed between the ion source and the first ion gate, a first migration region is formed between the first ion gate and the second ion gate, a second ionization region is formed between the second ion gate and the third ion gate, a second migration region is formed between the third ion gate and the ion receiving electrode, and the diameters of inner cavities of the first ionization region, the first migration region, the second ionization region and the second migration region are sequentially reduced in a step-by-step manner;
a first air outlet is arranged on the side wall of the cavity body close to one end of the ion source in the first ionization region, a first sample gas inlet is arranged on the side wall of the cavity body close to one end of the first ion gate, the first air outlet and the first sample gas inlet are positioned on the same axial cross section of the first ionization region and distributed on two sides of the axis, a first floating gas inlet is arranged on the side wall of the cavity body close to one end of the second ion gate in the first migration region, a second air outlet is arranged on the side wall of the cavity body close to one end of the second ion gate in the second ionization region and distributed on two sides of the axis, a second sample gas inlet is positioned on the same axial cross section of the second ionization region and distributed on two sides of the axis, and a second floating gas inlet is arranged on the circumferential side wall of one end of the second migration region close to the ion receiving electrode;
the first drift gas enters a first migration area through a first drift gas inlet, flows out of the first migration area from a first ion gate, is mixed with the first sample gas entering a first ionization area through a first sample gas inlet, and then flows out of the first ionization area through a first gas outlet, and the sum of the flow rate of the first drift gas in the first drift gas inlet and the flow rate of the sample gas in the first sample gas inlet is equal to the flow rate of gas in the first gas outlet;
the second path of floating gas enters a second migration area through a second floating gas inlet, flows out of the second migration area from a third ion gate, is mixed with the second path of sample gas entering a second ionization area through a second sample gas inlet, and then flows out of the second ionization area through a second gas outlet, and the sum of the flow rate of the floating gas in the second floating gas inlet and the flow rate of the sample gas in the second sample gas inlet is equal to the flow rate of gas in the second gas outlet;
the ion source is any ionization source capable of generating ions under atmospheric pressure, and comprises any one or the combination of more than two of a photoionization source, a discharge ionization source, an electrospray ionization source, a thermal surface ionization source and a radioactive ionization source;
the first ion gate, the second ion gate, and the third ion gate) is any one or a combination of two including a Bradbury-Nielsen type ion gate and a Tyndall-Powell type ion gate;
the ion migration electric fields in the first ionization region, the first migration region, the second ionization region and the second migration region are mutually independent and can be respectively adjusted;
an axial non-uniform direct current electric field with an ion enrichment function is arranged in the first ionization region along the direction from the ion source to the ion receiving electrode, and axial uniform direct current electric fields are respectively arranged in the first migration region, the second ionization region and the second migration region;
the axial direction is the axial direction of the ion transfer tube;
when the device works, sample molecules entering a first ionization region are converted into reaction reagent ions by an ionization source and are enriched in a region of the first ionization region, which is close to a first ion gate, under the drive of an axial non-uniform direct current electric field;
when the timing time T is equal to 0, the first ion gate is opened briefly, and the reaction reagent ions in the first ionization region are injected into the first ionization region in the form of pulse ion clusters with the axial length of Ld1In the first migration zone, the reagent ions with different mobilities are axially uniform in the first migration zoned1Are separated from each other and migrate towards the second ion gate;
timing time T ═ TdelayThen the second ion gate is opened briefly, and the mobility K in the first migration region is Ld1/(Ed1×tdelay) Is selected and injected into the thin disk-shaped reactant ion clusters with an axial length Lr2And the axial uniform DC electric field is Er2In the second ionization region, to perform an ion-molecule reaction with the sample molecules therein;
timing time T is more than or equal to TdelayThen the third ion gate is periodically and repeatedly opened for a short time, and the reaction product ions in the second ionization region are injected into the second ionization region in the form of pulse ion cluster with the axial length of Ld2In the second migration region, the product ions with different mobilities are in the axial uniform DC electric field Ed2Are mutually separated under the driving of the ion current sensor, and migrate towards the ion receiving electrode, and finally a product ion migration spectrogram of ion current intensity corresponding to migration time is formed;
the mobility K ═ Ld1/(Ed1×tdelay) The time required for the thin disk-shaped reactant ion cluster to migrate from the end adjacent to the second ion gate to the end adjacent to the third ion gate in the second ionization region is defined as the total time t of ion-molecule reactions between the reactant ions and the sample molecules in the second ionization regionrI.e. tr＝Lr2/(Er2×K)；
Changing the axial uniform DC electric field E in the second ionization regionr2Of variable ion intensityTotal time of molecular reaction trAnd obtaining corresponding product ion mobility spectra at the ion receiver using different trObtaining a product ion mobility spectrogram by calculation, namely obtaining a rate constant k of the ion-molecule reaction between the reaction reagent ions and the sample molecules in the second ionization region;
when the device works, the air pressure in the ion migration tube can be adjusted within 2-800 Torr, so that the rate constant k of the ion-molecule reaction between the reactive reagent ions and the sample molecules in the second ionization region under different air pressure conditions is obtained.
The ion migration tube is divided into four sequentially adjacent areas, namely a first ionization area, a first migration area, a second ionization area and a second migration area, by arranging three first ion gates, three second ion gates and three third ion gates which are arranged in parallel at intervals in the same ion migration tube. Initial reaction reagent ions generated by the ion source are enriched in the first ionization region and injected into the first migration region through the first ion gate to carry out ultrahigh-resolution ion mobility separation; the first migration area, the first ion gate and the second ion gate work cooperatively, so that reaction reagent ions with the mobility K pass through the second ion gate in a high selectivity manner and enter the second ionization area to perform ion-molecule reaction with target sample molecules; injecting product ions of the ion-molecule reaction in the second ionization region into the second migration region through a third ion gate for separation and detection to obtain an ion mobility spectrum of the product ions; the ion-molecule reaction between the selected reaction reagent ions and the target sample molecules in the second ionization region can be measured and researched by utilizing the obtained ion mobility spectrum of the product ions. The device can select the reactant ions with target mobility at high precision, and keeps the original clustering state of the reactant ions, thereby providing important data and technical support for analyzing an ion-molecule reaction mechanism in an atmospheric pressure and sub-atmospheric pressure ionization source.
The utility model has the advantages that:
the ion-molecule reaction selection control measuring device based on the ion mobility spectrometry can perform high-precision selection on the reaction reagent ions with the target mobility and keep the original clustering state of the reaction reagent ions, thereby providing important technical and data support for analyzing the ion-molecule reaction mechanism in the atmospheric pressure and sub-atmospheric pressure ionization source.
Drawings
The utility model is described in further detail below with reference to the accompanying drawings:
FIG. 1 is a schematic structural diagram of an ion-molecule reaction selective control measurement device based on ion mobility spectrometry. Wherein: 1. an ultraviolet light ion source; 2. an ion receiving electrode; 3. a first ion gate; 4. a second ion gate; 5. a third ion gate; 6. a first ionization region; 7. a first migration area; 8. a second ionization region; 9. a second migration area; 10. a first drift gas inlet; 11. a first sample gas inlet; 12. a first air outlet; 13. a second drift gas inlet; 14. a second sample gas inlet; 15. a second air outlet.
Fig. 2 shows that when the first path of sample gas is zero air containing 100ppm of acetone and 100% of RH, and the first path of drift gas, the second path of drift gas and the second path of sample gas are all zero air, the second ion gate 4 and the third ion gate 5 are set to be in a normally open state, and the first ion gate 3 is controlled to be opened for a short time to obtain a reaction reagent ion mobility spectrogram.
Fig. 3 shows that when the first path of sample gas is zero air containing 100ppm acetone and 100% RH, and the first path of drift gas, the second path of drift gas and the second path of sample gas are all zero air, the third ion gate 5 is set to be normally open, and the second ion gate 4 is controlled to be opened after the first ion gate 3 is opened for 2ms, so that the obtained reaction reagent ion migration spectrogram is obtained.
Detailed Description
Example 1
The ion-molecule reaction selective control measuring device based on the ion mobility spectrometry is shown in figure 1.
An ion source 1 of the ion migration tube is a VUV photoionization source of 10.6eV, an ion receiving electrode 2 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 first ion gate 3, the second ion gate 4 and the third ion gate 5 are all Bradbury-Nielsen type ion gates, and are all woven by metal wires with the diameter of 0.05mm on a PTFE PCB polar plate, the distance between the metal wires is 0.3mm, and the metal wires on the ion gates are divided into two groups which are insulated from each other and are respectively connected with two pulse high-voltage power supplies.
The first ionization region 6, the first migration region 7, the second ionization region 8 and the second migration region 9 are all formed by coaxially and alternately superposing annular conductive pole pieces with the axial length of 5mm and the outer diameter of 30mm and annular insulating pole pieces with the axial length of 5mm and the outer diameter of 30mm, the first ionization region 6 is 30mm, the first migration region 7 is 90mm, the second ionization region 8 is 50mm, and the second migration region 9 is 60 mm; the diameter of an inner cavity of the first ionization region is 22mm, the diameter of an inner cavity of the first migration region is 20mm, the diameter of an inner cavity of the second ionization region is 18mm, and the diameter of an inner cavity of the second migration region is 16 mm; the non-uniform direct current electric field in the first ionization region 6 is reduced to 200V/cm from 1200V/cm along the direction from the ion source to the ion receiving electrode, the uniform direct current electric field in the first migration region 7 is 800V/cm, the uniform direct current electric field in the second ionization region 8 is adjustable between 100V/cm and 1500V/cm, and the uniform direct current electric field in the second migration region 9 is 800V/cm.
Introducing a first path of floating gas with the flow rate of 500mL/min through a first floating gas inlet 10, introducing a first path of sample gas with the flow rate of 100mL/min through a first sample gas inlet 11, arranging an air extracting pump at a first air outlet 12, extracting the first path of floating gas and the first path of sample gas with the air extracting flow rate of 600mL/min, and extracting the first path of sample gas; introducing a second path of floating gas with the flow rate of 500mL/min through a second floating gas inlet 13, introducing a second path of sample gas with the flow rate of 100mL/min through a second sample gas inlet 14, arranging an air pump at a second air outlet 15, and extracting the second path of floating gas and the second path of sample gas with the air extraction flow rate of 600 mL/min; the temperature of the ion transfer tube was 100 ℃.
When the first path of sample gas is zero air containing 100ppm of acetone and 100% of RH, and the first path of drift gas, the second path of drift gas and the second path of sample gas are all zero air, the second ion gate 4 and the third ion gate 5 are set to be in a normally open state, and the first ion gate 3 is controlled to be opened for a short time to obtain a reaction reagent ion migration spectrogram shown in figure 2. In FIG. 2, it can be observed that the mobilities are respectively K0、K1And K2The three ion peaks of (A) are respectively (H)2O)6H+、(H2O)4H+And (H)2O)2H+Three reactant ions. The three reactant ions are generated by acetone sample gas with high humidity under the action of the VUV photoionization source 1. Since the second ion gate 4 and the third ion gate 5 are normally opened, all three kinds of reactant ions enter the second ionization region 8, and at this time, if a second sample gas containing a target compound is introduced into the second ionization region 8, the reactivity of a single reactant ion cannot be measured and studied.
When the first path of sample gas is zero air containing 100ppm acetone and 100% RH humidity, and the first path of drift gas, the second path of drift gas and the second path of sample gas are all zero air, the third ion gate 5 is set to be normally open, and the second ion gate 4 is controlled to be opened after the first ion gate 3 is opened for 2ms, so that the reaction reagent ion migration spectrogram shown in the figure 3 can be obtained. Obviously, since the first and second ion gates 3 and 4 keep the fixed delay time cooperating, only the mobility K is1Ion peak of (i), (H)2O)4H+Can be observed. This means that only the mobility is K1The reactive agent ion (H) of (2)2O)4H+Can enter the second ionization region 8 and both other reactant ions are shielded. At this time, if a second sample gas containing a target compound is introduced into the second ionization region 8 while controlling the third ion gate 5 to be periodically opened, the reagent ions (H) can be reacted2O)4H+The measurement study was carried out on the ion-molecule reaction with the target compound.
Claims (4)
1. The utility model provides an ion-molecule reaction selects accuse measuring device based on ion mobility spectrometry, the device includes the ion mobility pipe, and the ion mobility pipe is the hollow circular cylinder form cavity that constitutes by cyclic annular electrode and cyclic annular insulator coaxial coincide in proper order, sets up ion source (1) and ion receiving electrode (2) respectively in cavity both ends, its characterized in that:
a first ion gate (3), a second ion gate (4) and a third ion gate (5) are sequentially arranged between the ion source (1) and the ion receiving electrode (2) in the columnar cavity body along the direction from the ion source (1) to the ion receiving electrode (2) to divide the interior of the columnar cavity body into four areas, a first ionization region (6) is formed between the ion source (1) and the first ion gate (3), a first migration region (7) is formed between the first ion gate (3) and the second ion gate (4), a second ionization region (8) is formed between the second ion gate (4) and the third ion gate (5), a second migration region (9) is formed between the third ion gate (5) and the ion receiving electrode (2), and the diameters of inner cavities of the first ionization region (6), the first migration region (7), the second ionization region (8) and the second migration region (9) are sequentially reduced in a stepped manner;
a first air outlet (12) is arranged on the side wall of the cavity body close to one end of the ion source (1) of the first ionization region (6), a first sample gas inlet (11) is arranged on the side wall of the cavity body close to one end of the first ion gate (3), the first air outlet (12) and the first sample gas inlet (11) are positioned on the same axial section of the first ionization region (6) and are distributed on two sides of the axis, a first floating gas inlet (10) is arranged on the side wall of the cavity body close to one end of the second ion gate (4) of the first migration region (7), a second air outlet (15) is arranged on the side wall of the cavity body close to one end of the second ion gate (4) of the second ionization region (8), a second sample gas inlet (14) is arranged on the side wall of the cavity body close to one end of the third ion gate (5), the second air outlet (15) and the second sample gas inlet (14) are positioned on the same axial section of the second ionization region (8) and are distributed on two sides of the axis, a second floating gas inlet (13) is arranged on the circumferential side wall of one end of the second migration area (9) close to the ion receiving electrode (2).
2. The ion-molecule reaction selective control measuring device according to claim 1, characterized in that:
the ion source (1) is any ionization source capable of generating ions under atmospheric pressure, and comprises any one or the combination of more than two of a photoionization source, a discharge ionization source, an electrospray ionization source, a hot surface ionization source and a radioactive ionization source.
3. The ion-molecule reaction selective control measuring device according to claim 1, characterized in that:
the first ion gate (3), the second ion gate (4) and the third ion gate (5) are any one or a combination of two including Bradbury-Nielsen type ion gates and Tyndall-Powell type ion gates.
4. The ion-molecule reaction selective control measuring device according to claim 1, characterized in that:
the ion migration electric fields in the first ionization region (6), the first migration region (7), the second ionization region (8) and the second migration region (9) are mutually independent and can be respectively adjusted;
an axial non-uniform direct current electric field with an ion enrichment function is arranged in a first ionization region (6) along the direction from an ion source (1) to an ion receiving electrode (2), and axial uniform direct current electric fields are respectively arranged in a first migration region (7), a second ionization region (8) and a second migration region (9);
the axial direction is the axial direction of the ion transfer tube.
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