Method for enriching and separating trace amount of polychlorinated biphenyls (PCBs)

A polychlorinated biphenyl and separation method technology, applied in the field of environmental detection, can solve problems such as changes and column efficiency reduction, harm to the environment and human health, and detection sensitivity reduction, etc., to achieve easy automation, reduce pollution, and reduce pre-rich Effect of collection sample size and assay time

Active Publication Date: 2012-06-20
NINGBO UNIV
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  • Abstract
  • Description
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Problems solved by technology

[0005] (1) A large amount of organic solvents are required, causing secondary pollution and endangering the environment and human health
[0006] (2) Some traditional extraction methods are time-consuming and labor-intensive, reducing analysis efficiency
[0007] (3) The problem of emulsification occurs, prolonging the extraction time
[0008] (4) Interference peaks are generated, resulting in changes in the peaks of the analyte and reduction in column efficiency
[0009] (5) The injected extract sometimes reduces the sensitivity of the detector and shortens the life of the column
At present, in this field of technology, the use of the present invention to detect organic monomers has not yet been reported.

Method used

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  • Method for enriching and separating trace amount of polychlorinated biphenyls (PCBs)
  • Method for enriching and separating trace amount of polychlorinated biphenyls (PCBs)
  • Method for enriching and separating trace amount of polychlorinated biphenyls (PCBs)

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Embodiment Construction

[0031] The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.

[0032] 1. Filling fiber modification in solid phase microextraction column

[0033]Step 1: Take a beaker, add 4 to 5 grams of 3-(trimethyloxysilane) propyl methacrylate, then take it into a fume hood, and add 50 mL of distilled water to it. Take a set of magnetic stirrer and magnetically stir at 2000 rpm for 1 hour to obtain a propyl methacrylate polymer macromonomer containing a silica gel structure. The second step: add tributyl tin chloride as a catalyst in the above solution, add 4 to 5 grams of butylamine methacrylate, mix according to the mass ratio of 1:1; the third step: add 5 ~10 grams of commercial solid-phase microextraction fiber, heated at 50° for 3 to 4 hours until the color turns reddish brown, centrifuged at 2000 rpm to obtain 4 to 5 grams of brown precipitate. Step 4: Spread the above-mentioned precipitate on a 10 square cen...

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Abstract

The invention relates to a method for enriching and separating a trace amount of polychlorinated biphenyls (PCBs). According to the method, a trace amount of the PCBs in an environmental sample are enriched by a modified solid-phase microextraction column by a combining a method that a trace amount of the PCBs are subjected to linkage separation by a double column gas chromatography-electron capture detector, and then are eluted and detected. Compared with the prior art, the method has the advantages that: a macromolecule fixed phase of the solid-phase microextraction column is modified, a solid-phase microextraction technology is combined with the gas chromatography-electron capture detector, sampling, extraction, concentration, sample separation, and detection are combined into a simpleprocess, automaton is easy to realized, the amount of the pre-enriched samples and the detection time are reduced, and the effect of enriching the PCBs is improved; the nature is determined by a double chromatographic column, and PCB monomers with different polarities and structures are separated; the method has the advantages of high analysis speed, low manufacturing cost, and high detection sensitivity and specificity and the like, and is easy to operate; instruments are portable; and the detection limit of the coplanar PCB monomers in water can reach 10<-8> to 10<-7> mol / L, and the field test of residues of toxication forms of six kinds of main PCBs can be realized.

Description

technical field [0001] The invention relates to the field of environmental detection, specifically adopting a modified solid-phase microextraction column to enrich trace polychlorinated biphenyls (PCBs) in water, and combining gas chromatography-electron capture detector (gas chromatography-electronic capture detector) after elution capture detector) to detect various PCBs monomer methods and solid-phase microextraction devices. Background technique [0002] Early analysis of polychlorinated biphenyls (PCBs) followed the chemical analysis methods of organochlorine pesticides in the 1960s, including colorimetry, thermal analysis, and chemical titration. At present, the analysis of PCBs monomer mainly uses gas chromatography-electron capture detector (gas chromatography-electron capture detector), gas chromatography / mass spectrometer (including: GC-MS, multistage mass spectrometry, selective ion detection method, multi-ion detection method and negative ion chemical ionization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08
Inventor 曹玉廷干宁王丹丽桑卫国
Owner NINGBO UNIV
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