AU2019101689A4 - A new chlorine / bromine isotope mass spectrometer and its analytical method - Google Patents

A new chlorine / bromine isotope mass spectrometer and its analytical method Download PDF

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AU2019101689A4
AU2019101689A4 AU2019101689A AU2019101689A AU2019101689A4 AU 2019101689 A4 AU2019101689 A4 AU 2019101689A4 AU 2019101689 A AU2019101689 A AU 2019101689A AU 2019101689 A AU2019101689 A AU 2019101689A AU 2019101689 A4 AU2019101689 A4 AU 2019101689A4
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chlorine
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Jianye GUI
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • G01N30/7206—Mass spectrometers interfaced to gas chromatograph
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0027—Methods for using particle spectrometers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • G01N30/7206—Mass spectrometers interfaced to gas chromatograph
    • G01N2030/7226—OWTC, short capillaries or transfer line used as column

Abstract

Abstract The present invention provides an ion source comprising two reaction gas inlet devices, which are respectively arranged at the inlet and outlet of the reaction ionization tube. A new chlorine / bromine isotope mass spectrometer is also disclosed, comprising the ion source described above coupled to a capillary gas chromatography system and a magnetic mass spectrometry system. In addition, a chlorine or bromine isotope ratio analysis method is also disclosed. The sample is ionized by a radio frequency discharge reaction with the help of a reaction gas, and the chlorine or bromine in the sample forms pure chlorine anion or bromine anion under the action of a supplementary reaction gas for quality analysis. In the invention, pure chlorine anion or bromine anion is obtained under the action of radio frequency discharge through introduction and control of reaction gas. A new chlorine / bromine isotope mass spectrometer is formed through the design and adjustment of partial magnetic field of magnetic mass spectrum and Faraday detector, with high accuracy in analysis. It completely solves the interference of isobars in previous isotope tests, which can be applied in many fields such as chemical industry, environmental protection, geology, medicine and so on. Drawings o o230 220 Figure 1 Figure 2

Description

A New Chlorine / Bromine Isotope Mass Spectrometer and Its Analytical Method
Technical field
The invention relates to an ion source, a new chlorine / bromine isotope mass spectrometer and a chlorine or bromine isotope ratio analysis method, belonging to the field of isotope mass spectrometry.
Background Technology
With the continuous development of earth science, environmental science, food science and medical research, the traditional bulk sample isotope ratio analysis (BSIA) has been unable to meet the research needs, while the new compound-specific isotope analysis technology (CSIA) has become a hot research field. The CSIA method can be used to identify and track organic pollution sources in groundwater, surface water and soil, monitor the degradation of organic pollutants, test the effectiveness of control measures, identify manufacturers of chlorinated organic compounds, investigate the responsibility of makers of organic pollution events, and identify the source of major diseases, etc.
With the increasing of halogenated organic pollutants, in addition to the traditional stable isotopes of carbon (13C/12C), hydrogen (2H/1H) and oxygen (180/160) in CSIA technology, ratio analysis of chlorine (37C1/35C1) and bromine (79Br/81Br) has become a hot topic.
At present, the commonly used instrument for testing chlorine/bromine isotopes is isotope ratio mass spectrometry (IRMS), which uses electron impact (El) as the ion source. The ionized fragments are in the form of chloromethane ion or bromomethane ion, and the magnetic field deflection and mass number received by Faraday cup are 50, 52, 94, 96, etc. Although such instrument can be used for analysis of chlorine/bromine isotope in halogenated organics, the process is very complicated. Chlorinated organics need to be converted to CH3C1, which is then ionized into CH3C1+ by a mass spectrometer for mass analysis and detection. Because the process itself is very difficult, applications are very limited, as are brominated organics.
Thermal ionization mass spectrometry (TIMS) can also be used to analyze chlorine and bromine isotopes. The ionization source is a thermal ionization ion source, referred to as thermal ionization source. The basic principle is that the prepared sample is coated on the heated metal surface and the sample components are ionized by losing or gaining electrons in the thermal evaporation process. Although the thermal ionization source has the advantages of
2019101689 24 Dec 2019 good ionization efficiency and low memory effect, when testing chlorine or bromine isotopes, organic chlorine shall be converted into inorganic chlorine and then synthesized into cesium chloride before being coated on the sample zone, a process that is difficult to complete online. Another type of mass spectrometer is used for chlorine and bromine isotope analysis by adding a high-temperature combustion device between gas chromatography and mass spectrometry. Halogenated organics are separated by gas chromatography and then transferred to a high temperature combustion facility (HTC). At temperature above 1300 degrees, the organics are converted to hydrogen chloride (HC1) or hydrogen bromide (HBr) form, which is then ionized, deflected, and detected. The ionization source is still the classical electron impact (El), and the mass number detected by Faraday cup is (36, 38) or (80, 82).
Document CN 102590379 B discloses a chlorine / bromine isotope analysis instrument and method based on negative chemical ionization source. By adjusting the ion source and transforming the collection mode, the method can separate the chlorine or bromine from the carbon skeleton when the chlorinated or brominated organics are ionized, so the analysis can be achieved by direct collection (35, 37) or (79, 81). This method can simplify the analysis process and improve the analysis speed while ensuring the analysis accuracy. However, as negative chemical ionization is a kind of soft ionization technique, the efficiency of ionization source is still low, and some substances with strong molecular symmetry (such as hexachlorobenzene, etc.) still cannot dissociate halogen atoms at the same time of ionization. The invention discloses an ion source based on the principle of radio frequency discharge. Through the introduction and control of reaction gas, pure chlorine anion or bromine anion can be obtained under the action of RF discharge. Through the design and adjustment of partial magnetic field of magnetic mass spectrometry and Faraday detector, a new type of chlorine / bromine isotope mass spectrometer has been formed, and corresponding analysis method has been developed. The name of the new instrument is Gas Chromatography-RF Discharge Reaction Ion Source- Isotope Ratio Mass Spectrometer (GC-RFRIS-IRMS).
Summary of the Invention
This invention intends to provide an ion source with high accuracy, high efficiency and good applicability.
To achieve that purpose, the present invention provides an ion source comprising a reaction ionization tube, an induction coil, a power amplifier and a radio frequency signal generator, wherein the middle section of the reaction ionization tube is wrapped by the induction coil and the radio frequency signal generator is coupled to the power amplifier. When the RF
2019101689 24 Dec 2019 signal of the RF signal generator passes the power amplifier, it is amplified and transmitted to the induction coil, forming a RF signal field inside the induction coil. The present invention is characterized in the fact that it also comprises two reaction gas inlet devices, which are separately set on the inlet and outlet of the reaction ionization tube. The reaction ionization tube is provided with carrier gas and auxiliary reaction gas distilled from the gas chromatography. The reaction gas inlet devices at the inlet and outlet of gas chromatography capillary column are connected to the reaction ionization tube through a reducer, respectively serving as a passageway to supply the carrier gas and the first path auxiliary reaction gas, while the carrier gas and the first path auxiliary reaction gas will generate a discharge under the action of radio frequency to ionize the gas; the other reaction gas inlet device is connected to the outlet of the ion source, serving as a passageway for the second reaction gas. Under the action of the second reaction gas, the ionized gas will be cooled to a certain extent by the collision reaction, through dissociation resonance electron capture reaction, pure negatively charged target ions (i.e. Cf , Cf or Br, Br) are formed. Both of the first and the second reaction gases are introduced by the mass flow controller.
Preferable, the reaction ionization tube is made of high temperature resistant quartz tube or ceramic material.
Preferable, the radio frequency range of the radio frequency signal generator is within 20-400 MHz.
The present invention also provides a new high-precision, high-efficiency and on-line measurement chlorine / bromine isotope mass spectrometer, which is composed of the above-mentioned ion source, the capillary gas chromatography system and the magnetic mass spectrometry system. The capillary column of the capillary gas chromatography is connected to the inlet of the reaction ionization tube of the ion source, and the outlet of the reaction ionization tube is connected to the magnetic mass spectrometer system, wherein the magnetic mass spectrometer system comprises ion transport channels, a magnetic mass analyzer, a Faraday cup ion detection and signal output system and the corresponding vacuum system. Preferable, the length of the capillary column of the capillary gas chromatography system is within 30-60 meters, the number of theoretical plates of the chromatographic column is more than 3000 per meter, the total number of plates is more than 105, and the peak of different components appears within 10- 50s.
Preferable, the ion detection and signal output system comprises a Faraday cup detector and an electron multiplier, wherein the mass number that is received by the Faraday cup can be
2019101689 24 Dec 2019 (35, 37) or (79, 81) and the Faraday cup detector has 3 Faraday cups, in which one channel is shared by switching.
The magnetic field of the magnetic mass analyzer system has a radius of 230 mm, with incidence and emergence angles of 26.5 degrees, theoretical dispersion coefficient of 920, source slit of 0.3 mm apart, receiving slit of 1.4 mm apart and mass resolution of more than 160.
The present invention also provides a chlorine or bromine isotope ratio analysis method based on the isotope mass spectrometer, which comprises the following steps:
A> A sample of chlorine or bromine organic compound is loaded into the gas chromatography system for separation;
B> After chromatographic analysis, the components flow directly from the capillary column into the reaction ionization tube of the ion source and simultaneously the reaction gas is introduced from the inlet of the reaction ionization tube, by the RF discharge reaction, the target is ionized; The supplement reaction gas is introduced from the outlet of the reaction ionization tube, under the action of supplementary reaction gas, the chlorine or bromine in the target ion forms pure negative charged ion chloride or bromine for mass analysis;
C> Chlorine or bromine anions pass through the ion transmission channel into the magnetic mass analyzer, and are received and detected by the Faraday Cup ion detection and signal output system after the deflection in the magnetic field.
Preferable, the reaction gas is helium or argon, of which the flow rate range is 1.0 - 50.0 mL / min.
Preferable, the supplementary reaction gas is nitrogen, of which the flow rate range is 1.0 100.0 mL / min.
The present invention adopts an ion source of innovative design and integrates the sample conversion and ionization into one process through reaction control radio frequency ionization, which has greatly reduced the analysis process. By coupling the magnetic mass analyzer and the Faraday detector that meet the requirements of fragment ions, a complete analytical instrument is formed. When coupling the instrument with the gas chromatography, the entire instrument is named gas chromatography radio frequency reaction ionization system isotope ratio mass spectrometer (GC-RFRIS-IRMS). Due to the fact that this ionization method can directly obtain pure chloride or bromine anions (i.e. Cl', CP or Br‘, 81Br‘), it completely overcomes the isobaric interference caused by the ionization debris containing carbon, hydrogen and other elements compared to traditional method; since the ionization has strong discharge energy and is capable of adjusting the reaction gas for
2019101689 24 Dec 2019 different targets, the adjustment of the first reaction gas can ensure the discharge process, and the adjustment of the second reaction gas makes the dissociation resonance electron capture reaction occur in the ionized organic matter, thus all contribute to the formation of negative ions. As the first path and second path of reaction gases can be adjusted, in theory, all the halogenated organic matter can be ionized and the chlorine or bromine atoms can be stripped for analysis of its isotope ratio; the flow rate of the reaction gas used in this instrument is small, usually less than lOOmL / min, so the vacuum load of the entire instrument is also small, which is conducive to saving instrument costs and maintaining instrument stability. This instrument, with a novel principle and a sophisticated design, not only has high analysis accuracy, but also completely solves the problem of isotopic interference of isotope testing. It is an innovative mass spectrometric technique that can be applied to chemical engineering, environmental protection, geosciences, medicine and other fields.
Description of the Drawings
Figure 1 Schematic diagram of ion source;
Figure 2 Schematic diagram of magnetic mass analyzer system;
Figure 3 Schematic diagram of ion detection and signal output system;
Figure 4 Schematic diagram of isotope mass spectrometer.
Detailed Description of the Presently Preferred Embodiments
The present invention may be embodied in specific forms. The described embodiments are to be considered in all respects only as illustrative and not restrictive.
Embodiment 1
As shown in Fig. 4, the new chlorine / bromine isotope mass spectrometer is composed of a capillary gas chromatography system 100 coupled to an ion source 200 and a magnetic mass spectrometry system 300. As shown in Fig. 1, the ion source 200 comprises a reaction ionization tube 210, an induction coil 220, a power amplifier 230 and a radio frequency signal generator 240. The middle section of the reaction-ionization tube 210 is wrapped by the induction coil 220, and the RF signal generator 240 is coupled to the power amplifier 230. The RF signal of the RF signal generator 240 is amplified and enhanced through the power amplifier 230 and transmitted to the induction coil 220, forming a RF signal field inside the induction coil. It also comprises two reaction gas inlet devices 250, which are respectively arranged at the inlet and outlet of the reaction ionization tube. The capillary column of the capillary gas chromatography system is connected to the inlet of the reaction ionization tube
2019101689 24 Dec 2019
210 of the ion source through a reducer. The magnetic mass spectrum system is composed of an ion transmission section 310, magnetic mass analyzer section 320 and the Faraday cup ion detection and signal output section 330. The outlet of the reaction ionization tube 210 is connected with the ion transmission part 310, the magnetic mass analysis part 320, the ion detection and signal output part 330 successively.
The capillary column length of the capillary gas chromatography system 100 is in the range of 30-60 meters. The number of theoretical plates of chromatographic column is more than 3000 per meter, the total number of plates is over 105, and the peak-out time of different components is in the range of 10-50 s. As shown in Fig. 2, the magnetic mass analysis section 320 includes a source slit 321, a magnetic field 322 and a receiving slit 323. The magnetic field has a radius of 230mm, the boundary of magnetic field incidence and emission is 26.5 degrees, the theoretical dispersion coefficient is 920, the source slit is 0.3mm apart, the receiving slit is 1.4mm apart, and the mass resolution is above 160;
As shown in Fig. 3, the ion detection and signal output section 330 includes a Faraday cup detector and an electron multiplier 332. The mass number received by the Faraday cup is (35, 37) or (79,81), and the Faraday cup detector has 3 Faraday cups, in which one channel is shared by switching.
The whole mass spectrometer system is in a high vacuum state, which is realized by multi-stage vacuum. The pressure ranges from a few pa to 10'3pa from the reducer to the ion source, and the vacuum of the analyzed pipeline is higher than 10’4pa.
Embodiment 2
The instrument for the analysis of chlorine isotope ratios of chlorinated hydrocarbon pollutants in groundwater contaminated sites is GC-RFRIS-IRMS in the present invention, and the auxiliary equipment is a purge and trap device (OI Company, Model 4660, USA), and the monitoring target is trichloroethylene. The following steps are included:
A> Load the water sample into the purge collector for purging and trapping: the trap: No. 10 trap, the purge gas: nitrogen, the purge flow: 40mL / min, the purge time: llmin; analysis preheating temperature: 180 °C, analysis temperature: 190 °C, analysis time: 0.5 min; baking temperature: 220 °C, baking time: 6 min; realizing the enrichment of chlorinated organic compounds;
B> Gas chromatography separation: The enriched samples of the enriched chlorinated organic compounds are loaded into the gas chromatographic system for separation. Gas chromatography separation conditions are as follows: the capillary chromatography column is Rtx-624 (column length: 30m, internal diameter: 0.25mm, film thickness: 0.25 gm), and the
2019101689 24 Dec 2019 initial column temperature is 40 °C and kept for 2 min; the temperature is raised to 210 °C at 20°C/min and kept for 5min. Temperature of inlet: 220 °C; split sampling at the split ratio of 20; column flow rate: 1 mL / min;
CL After chromatographic analysis, the components flow directly from the pipe column into the reaction ionization tube of the ion source and are ionized by the RF discharge field at the RF operating voltage of 12V and the operating frequency of 20MHz. The reaction helium flow rate is 1.0ml /min, and the postteaction nitrogen flow rate is 1.0ml /min. The chlorine in trichloroethylene is ionized to form chlorine anion, and 35Cf and 37Cf are produced efficiently for mass analysis.
D> 35Cf and 37Cf produced in ionization are deflected by the magnetic field and then received by the Faraday cup having a mass number of 35 and 37. Finally, they are amplified and output by the signal detector, which can detect the peak intensity I37 and I35 of 35Cf and 37CF respectively. The isotope ratio Ra is calculated by the following formula:
Figure AU2019101689A4_D0001
Figure AU2019101689A4_D0002
Figure AU2019101689A4_D0003
Finally, the Rq value above is compared with that of similar reference material with known isotopic standard. The calculation formula is as follows:
Figure AU2019101689A4_D0004
Where
Figure AU2019101689A4_D0005
is the value of reference material.
Embodiment 3
The instrument for bromine isotope analysis of deltamethrin in soil samples is RFRIS-IRMS in the invention, and the auxiliary equipment is the accelerated solvent extractor (DIONEX, model ASE200). The following test steps are included:
A> Extraction process - accelerated solvent extraction
The soil samples are crushed to about 100 mesh, then loaded into the extraction tank, and extracted with dichloromethane/acetone (5:1) under the following extraction conditions: furnace temperature: 100 °C, pressure: 10.3Mpa, static time: 5 min (after 5 min preheating and equilibration), flush volume: 60% of extraction tank volume, nitrogen cleaning time: 80 s
2019101689 24 Dec 2019 at 1.03 Mpa, static cycle: 2 times. The extracted sample is concentrated to less than 0.5 ml on a pressure blowing concentrator and then fixed to 1 ml with n-hexane;
B > Gas chromatography separation: the extracted sample is loaded into the gas chromatography system for separation. The chromatographic conditions are as follows: capillary chromatography column: DB-5MS (30m x 0.25mm x 0.25pm) column.
Chromatographic program heating conditions: the initial temperature: 50 °C, maintained for 0 min, then increased to 180 °C at 25 °C / min, then increased to 300 °C at 15 °C / min, kept for 3 min. Temperature of inlet: 210 °C; sampling method: no split sampling; injection volume: 1 μΐ;
C\ After chromatographic analysis, the components flow directly from the pipe column into the reaction ionization tube of the ion source and are ionized by the RF discharge field at the RF operating voltage of 12V and the operating frequency of 75MHz. The reaction argon flow rate is 50.0ml /min, and the postreaction nitrogen flow rate is 50.0ml /min. Under the above conditions, the bromine in deltamethrin is ionized, 79Br‘ and 81Br' are produced efficiently for mass analysis.
D> The ionized 79Br‘ and 81Br are compressed and transmitted to the source slit and deflected by the magnetic field, then received by the Faraday cup having a mass number of 79, 81. The isotope ratio RBr is calculated by the following formula with the ionic current intensity I79 and I8i of 79Br and 81Br:
Figure AU2019101689A4_D0006
Finally, the RBr value above is compared with that of similar reference material with known isotope standard value, and the final δ81 Br value is obtained:
Figure AU2019101689A4_D0007
l)xl000%0
Figure AU2019101689A4_D0008
Where
Br is the value of the reference material.
Embodiment 4
The instrument for fingerprint analysis of chlorine isotope in the reagent hexachlorobenzene is GC-RFRIS-IRMS in the present invention. The following test steps are included:
A > Gas chromatography separation: Hexachlorobenzene reagent is dissolved in n-hexane and then loaded into the gas chromatography system for separation. Chromatographic conditions are as follows: capillary chromatography column: DB-5MS (30m x 0.25mm x 0.25pm) column. Chromatographic program heating conditions: the initial temperature: 50 °C, maintained for 0 min, then increased to 180 °C at 25 °C / min, then increased to 300 °C at 15 °C / min, kept for 3 min. Temperature of inlet: 210 °C; sampling method: no split sampling; injection volume: 1 μΐ;
C. After chromatographic analysis, the components flow directly from the pipe column into the reaction ionization tube of the ion source and are ionized by the RF discharge field at the RF operating voltage of 12V and the operating frequency of 400MHz. The reaction helium flow rate is 20.0ml /min, and the postreaction nitrogen flow rate is 100.0ml /min. Under the above conditions, the hexachlorobenzene is ionized, 35C1‘ and 37C1‘ are produced efficiently.
D> 35Cf and 37Cf produced in ionization are deflected by the magnetic field and then received by the Faraday cup having a mass number of 35 and 37. Finally, they are amplified and output by the signal detector, which can detect the peak intensity I37 and I35 of 35Cf and 37Cf respectively. The isotope ratio Ra is calculated by the following formula:
Figure AU2019101689A4_D0009
Figure AU2019101689A4_D0010
Figure AU2019101689A4_D0011
Finally, the RCi value above is compared with that of similar reference material with known isotopic standard. The calculation formula is as follows:
j37 ci = (-— -1) x i ooo %o v T)Std '
Figure AU2019101689A4_D0012
Cl
Where is the value of the reference material.

Claims (10)

1. It is an ion source comprising a reaction ionization tube, an induction coil, a power amplifier and a radio-frequency signal generator. The middle section of the reaction-ionization tube is wrapped by the induction coil, and the RF signal generator is coupled to the power amplifier. The RF signal of the RF signal generator is amplified and enhanced through the power amplifier and transmitted to the induction coil, forming a RF signal field inside the induction coil. It is characterized by the fact that it also comprises two reaction gas inlet devices, which are respectively arranged at the inlet and outlet of the reaction ionization tube.
2. The ion source according to claim 1 is characterized in the fact that the reaction ionization tube is made of a high temperature resistant quartz tube or ceramic material.
3. The ion source according to claim 2 is characterized in the fact that the radio frequency of the radio frequency signal generator is in the range of 20-400 MHz.
4. A new chlorine / bromine isotope mass spectrometer consists of an ion source according to any one of claims 1-3 coupled to a capillary gas chromatography system and a magnetic mass spectrometry system. The capillary column of the capillary gas chromatography system is connected to the inlet of the reaction ionization tube of the ion source, and the outlet of the reaction ionization tube is connected to the magnetic mass spectrometry system. The magnetic mass spectrometry system comprises an ion transmission channel, a magnetic mass analyzer, Faraday cup ion detection and signal output system and corresponding vacuum system.
5. The new chlorine / bromine isotope mass spectrometer according to claim 4 is characterized in the fact that the capillary column length of the capillary gas chromatography system ranges from 30 to 60 meters, the number of theoretical plates of chromatographic column is more than 3000 per meter, the total number of plates is over 105, and the peak-width of different components is between 10-50 s.
6. The new chlorine / bromine isotope mass spectrometer according to claim 4 is characterized in the fact that the Faraday cup ion detection and signal output system
2019101689 24 Dec 2019 comprises a Faraday cup detector and an electron multiplier. The mass number received by the Faraday cup is (35, 37) or (79,81), and the Faraday cup detector has 3 Faraday cups, in which one channel is shared by switching.
7. The new chlorine / bromine isotope mass spectrometer according to any one of claims 4-6, characterized in the fact that the magnetic mass analyzer has a magnetic field with a radius of 230mm, and angles of incidence and emergence of 26.5 degrees. The theoretical dispersion coefficient is 920, the source slit is 0.3mm apart, the receiving slit is 1.4mm apart, and the mass resolution is over 160.
8. A chlorine or bromine isotope ratio analysis method comprising, in particular, the steps of:
A> Loading the sample of chlorinated or brominated organic compounds into a gas chromatography system for separation;
B> After chromatographic analysis, the components flow directly from the capillary column into the reactive ionization tube of the ion source, and the reaction gas is simultaneously imported from the inlet of the reaction ionization tube. With the aid of the reaction gas, the object is ionized by the RF discharge reaction, and the supplementary reaction gas is imported from the outlet of the reaction ionization tube. Under the action of the supplementary reaction gas, the chlorine or bromine in the object forms pure negative charged ion chlorine or bromine for quality analysis;
C> Chlorine or bromide anions pass through the ion transmission channel to the magnetic mass analyzer, which is deflected in the magnetic field and then received and detected by the Faraday cup ion detection and signal output system.
9. The chlorine or bromine isotope ratio analysis method according to claim 8 is characterized in the fact that the first reaction gas is helium or argon at a flow rate in the range of 1.0-50.0 mL / min.
10. The chlorine or bromine isotope ratio analysis method according to claim 9 is characterized in the fact that the second reaction gas is nitrogen at a flow rate ranging from 1.0 to 100.0 mL/min.
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