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Method for online-analyzing organic monomer chlorine or bromine isotope and based on chemical ionization

A chemical ionization and bromine isotope technology, applied in the fields of food, geology, environmental protection, and medicine, can solve the problems of complex practices, never been applied, and difficult transformation process, and achieve the effect of simplifying the process

Inactive Publication Date: 2012-07-18
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Using isotope ratio mass spectrometry (IRMS), chlorine isotope analysis in chlorinated organic compounds can be carried out, but the classical method is very complicated and requires the conversion of chlorinated organic compounds into chloromethane (CH 3 Cl), which is then ionized into CH 3 Cl + , and then sent to the isotope ratio mass spectrometry detection, because this conversion process itself is very difficult, so it can only be done offline, the same is true for brominated organic compounds
[0005] Theoretically speaking, chlorinated or brominated organic compounds are easy to lose a chlorine atom or bromine atom to form M-Cl or M-Br when they are bombarded by energy, that is to say, they can be easily detected when negative ion detection is performed. Chloride anion or bromide anion, but this rule has only been used to determine the content of organic matter for many years, but has never been applied to the field of isotope analysis

Method used

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  • Method for online-analyzing organic monomer chlorine or bromine isotope and based on chemical ionization
  • Method for online-analyzing organic monomer chlorine or bromine isotope and based on chemical ionization
  • Method for online-analyzing organic monomer chlorine or bromine isotope and based on chemical ionization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1. Determination of Chlorine Monomer Isotope Ratio in Soil Organochlorine Pesticide Four Isomers HCH and Four Isomers DDT

[0043] The extraction instrument is an accelerated solvent extraction instrument, the ASE200 type produced by Diane Corporation of the United States, and the detection instruments are gas chromatography, chemical ionization source and isotope ratio mass spectrometer, all purchased from Thermal Fisher Corporation of the United States, model MAT 253, equipped with 35, 37 Faraday receivers Cup, the specific method is as follows:

[0044] 1. Extraction process - accelerated solvent extraction

[0045] Crush the soil sample to about 100 mesh, put it into the extraction pool, and extract it with dichloromethane / acetone (1+1). The detailed extraction conditions are as follows:

[0046] Furnace temperature: 100°C, pressure: 10.3Mpa, static time: 5min (after 5min preheating and equilibrium), flushing volume: 60% of the volume of the extraction pool...

Embodiment 2

[0059] Embodiment 2: Determination of chlorine isotope ratio in volatile organic pollutant monomer in waste water

[0060] Taking the determination of the chlorine isotope ratio of vinyl chloride, dichloroethylene, trichloroethylene, and tetrachloroethylene monomers in volatile organic pollutants (VOCs) in water as an example,

[0061] The concentration instrument used is a purge-and-trap instrument. The American OI company produces a 4660-type purge-and-trap concentrator. The detection instruments are gas chromatography, a chemical ionization source, and an isotope ratio mass spectrometer, all of which are purchased from the Thermal Fisher Company of the United States, model MAT 253 , with 35, 37 Faraday receiving cups, the specific method is as follows:

[0062] 1. Concentration method - purge and trap method

[0063] 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...

Embodiment 3

[0077] Embodiment 3: the isotope ratio determination of bromine in the bromoform in the water volatile organic pollutant (VOCs)

[0078] The concentration instrument used is a purge-and-trap instrument. The American OI company produces a 4660-type purge-and-trap concentrator. The detection instruments are gas chromatography, a chemical ionization source, and an isotope ratio mass spectrometer, all of which are purchased from the Thermal Fisher Company of the United States, model MAT 253 , with 79,81 Faraday receiving cups, the specific method is as follows:

[0079] 1. Concentration method - purge and trap method

[0080] Put the water sample into the purge and trap instrument to carry out the purge and trap instrument. The purge and trap instrument used is the Model 4660 purge and trap concentrator produced by OI Company in the United States. The specific conditions are as follows: the trap is No. 10 trap, The purge gas is nitrogen, the purge flow rate is 40mL / min, and the p...

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Abstract

The invention aims at providing a method for online-analyzing organic monomer chlorine or bromine isotope, which adopts a direct negative chemical ionization to replace an original complex organic monomer conversion process. The method is characterized by including the steps: A. gathering chlorine or bromine substitute; B. separating gas chromatography: placing the gathered chlorine or bromine substitute into the gas chromatography to be separated; C. conducting negative chemical ionization: components analyzed through chromatography directly flow into a negative chemical ion source through acapillary column, the negative chemical ion source replaces an original electron bombardment source configured on an isotope ratio mass spectrum to conduct the negative chemical ionization; D. mass spectrometric detecting: on a gas isotope ratio mass spectrum, selecting a faraday receiving cup corresponding to mass number of chlorine or bromine substitute directly, and receiving electronegative isotope fragment ions generated by the negative chemical ionization. The process is conducted under high vacuum state, and degree of vacuum is higher than 1.0*10<-3> Pa. The method greatly simplifies aprocess of online-analyzing organic monomer chlorine or bromine isotope and can form various special devices for detecting organic monomer isotope ratio.

Description

Technical field: [0001] The invention relates to a novel analysis method for chlorine or brominated organic monomer chlorine isotope (CSIA-Cl) or bromine isotope (CSIA-Br), which belongs to the category of organic monomer isotope analysis technology (CSIA) and can be applied to environmental protection, Geology, food, medicine and other fields. 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 res...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 桂建业赵国兴陈宗宇刘福亮
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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