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Novel chlorine/bromine isotope mass spectrometer based on normal pressure plasma ionization and analysis method thereof

A new type of atmospheric pressure plasma technology, applied in the direction of ion source/gun, material analysis and material analysis through electromagnetic means, can solve the problems of difficult equipment maintenance, low efficiency of ionization source, stripping of halogen atoms, etc., and achieve the goal of instrument Convenient maintenance and debugging, overcoming isobaric interference, and high analysis accuracy

Inactive Publication Date: 2018-09-18
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the negative chemical ionization method is a soft ionization technology, the efficiency of the ionization source is still not high, and some substances with strong molecular structure symmetry (such as hexachlorobenzene, etc.) still cannot achieve the stripping of halogen atoms while ionizing
To solve this problem, our research group has developed an isotope mass spectrometer based on radio frequency discharge ionization, but this ionization source needs to work in a vacuum, which has caused certain difficulties for equipment maintenance.

Method used

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  • Novel chlorine/bromine isotope mass spectrometer based on normal pressure plasma ionization and analysis method thereof
  • Novel chlorine/bromine isotope mass spectrometer based on normal pressure plasma ionization and analysis method thereof
  • Novel chlorine/bromine isotope mass spectrometer based on normal pressure plasma ionization and analysis method thereof

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Effect test

Embodiment 1

[0032] Such as Figure 4As shown, the isotope mass spectrometer is composed of an atmospheric pressure plasma ion source 200, a gas chromatography system 100, and a magnetic mass spectrometry system 300. The magnetic mass spectrometry system 300 is composed of an ion transmission system 310, a mass analyzer 320, and an ion detection system 330. The capillary column of the gas chromatography system 100 is connected to the reaction ionization tube of the ion source, and the reaction ionization tube, ion transmission system, mass analyzer, and ion detection system are connected in sequence;

[0033] The gas chromatographic system adopts a capillary gas chromatographic system, and a capillary chromatographic column with a length of 30-60 meters and a theoretical plate number of 3000-4000 per meter is selected to ensure that the total plate number reaches 10 5 Above, ensure that the peak time of different components is between 10-50s.

[0034] Such as figure 1 As shown, the norma...

Embodiment 2

[0040] The chlorine isotope ratio analysis method of chlorinated hydrocarbon pollutants in groundwater pollution site, instrument used is gas chromatography-atmospheric pressure plasma-isotope mass spectrometer (GC-APP-IRMS) of the present invention, and supporting equipment is purging and trapping Device (U.S. OI company, model 4660), monitoring object is trichlorethylene, comprises the following steps:

[0041] A. Put the water sample into the purge-and-trap instrument for purge-and-trap instrument. The trap is No. 10 trap, the purge gas is nitrogen, the purge flow rate is 40mL / min, and the purge time is 11min; analytical preheating is 180°C , the analysis temperature is 190°C, the analysis time is 0.5min; the baking temperature is 220°C, and the baking time is 6min; the enrichment of chlorinated organic compounds is realized;

[0042] B. Gas chromatographic separation: put the enriched chlorinated organic samples into a gas chromatographic system for separation. Gas chromat...

Embodiment 3

[0050] The bromine isotope analysis of deltamethrin in the soil sample, instrument used is gas chromatography-atmospheric pressure plasma-isotope mass spectrometer (GC-APP-IRMS) of the present invention, and supporting equipment is accelerated solvent extraction instrument (U.S. Diana company, model ASE200), including the following test steps:

[0051] A. Extraction process—accelerated solvent extraction

[0052] Crush the soil sample to about 100 mesh, put it into the extraction tank, and extract it with dichloromethane / acetone (5:1). The detailed extraction conditions are: furnace temperature: 100°C, pressure: 10.3Mpa, static time: 5min (5min After preheating and equilibrium), flushing volume: 60% of the volume of the extraction pool, nitrogen cleaning: 80s under 1.03Mpa pressure, static cycle: 2 times. Concentrate the extracted sample to less than 0.5ml on a nitrogen blower, and then dilute to 1ml with n-hexane;

[0053] B. Gas chromatographic separation: Put the above-me...

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Abstract

The invention provides a normal pressure plasma ion source; an inertia reaction gas tube is connected with the inlet end of a reaction ionization tube; the reaction ionization tube is wrapped by an electrode slice; an insulation sleeve sleeves on the reaction ionization tube and the electrode slice; the electrode slice is connected with an electrode wire; the electrode wire leads out from a hole of the insulation sleeve and is connected with a high pressure medium block discharge source phase; the invention also discloses a new chlorine / bromine isotope mass spectrometer comprising the ion source, and provides a chlorine / bromine isotope ratio analysis method. The method can use a plasma ionization source stably working under a normal pressure to combine a sample conversion process with an ionization process, thus greatly reducing the analysis flow; a magnetic mass analyzer and a Faraday detector satisfying ionization fragment requirements are matched and coupled to form the novel chlorine / bromine isotope mass spectrometer with a high analysis precision; the ionization source can work under a normal pressure and atmospheric pressure conditions, and can be applied to the chemical, environmental protection, geosciences and medical science fields.

Description

technical field [0001] The invention relates to an atmospheric pressure plasma ion source, a novel chlorine / bromine isotope mass spectrometer based on atmospheric pressure plasma ionization and a chlorine or bromine isotope analysis method, belonging to the field of isotope mass spectrometry analysis. Background technique [0002] With the continuous deepening of earth science, environmental science, food science and medical research, the traditional whole sample isotope ratio analysis (BSIA) can no longer meet the research needs, and the new organic monomer isotope technology (CSIA) has become a frontier research hotspot. The CSIA method can be used to identify and track groundwater, surface water and soil organic pollution sources, monitor the degradation process of organic pollutants and test the effect of prevention and control measures, identify manufacturers of chlorinated organic substances, and investigate the relevant responsibilities of organic pollution incidents. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01J49/00H01J49/10G01N27/62
CPCG01N27/62H01J49/0031H01J49/004H01J49/10
Inventor 桂建业张晶张辰凌赵国兴
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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