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Gas phase-liquid phase on-line combined dioxin sample purification device

A dioxin-based and purification device technology, which is applied in the preparation of test samples, measuring devices, instruments, etc., can solve the problems of complicated sample purification and quantitative analysis process, unreusable chromatography column, and increased experimental cost, etc. Achieve the effect of reducing experimental costs, reducing health hazards, and reducing the amount of waste solvents

Active Publication Date: 2013-01-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dioxin-like pollutants are often at trace levels in environmental samples, and the coexisting interference components are often several orders of magnitude higher, so the sample purification and quantitative analysis process is very complicated
The FMS automatic purification instrument has the advantages of saving time and effort, increasing the reliability of the results, and reducing the harm to the operator, but the instrument is expensive, the commercial chromatography column cannot be reused, and the solvent consumption is as high as 400mL, and the experimental cost is nearly increased compared with the traditional method. double

Method used

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  • Gas phase-liquid phase on-line combined dioxin sample purification device
  • Gas phase-liquid phase on-line combined dioxin sample purification device
  • Gas phase-liquid phase on-line combined dioxin sample purification device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Such as Figure 1~5 Schematic diagram of the structure of the dioxin sample purification device in different states for gas-liquid on-line coupling.

[0035] I readiness status:

[0036] The carrier gas is introduced, the pressure of the pressure stabilizing valve 5 is 0.22Mpa, and the pressure of the stabilizing flow valve 6 is 0.15Mpa. Inject the sample added with the extracted internal standard into the quantitative tube 8, at this time, the closed cavity where the retention gap column 10 and the GC analysis column 13 are located is heated to 280°C, and the closed cavity where the four-way valve 14 is located is heated to 80°C The ③ position and the ⑥ position of the injection valve 9 are connected to the two ends of the quantitative tube 8 respectively, and the ④ position is connected to the ⑤ position of the first six-way switching valve 3 through the pipeline, and the ⑤ position is connected to the retention gap through the pipeline The inlet end of the column 1...

Embodiment 2

[0049] The experimental device and method conditions are the same as in Example 1, 90 μL of fly ash extract is added with 10 μL of 15 kinds of 13 C 12 The labeled 2, 3, 7, 8-substituted PCDD / Fs is extracted as an internal standard, and the device of the present invention is used for gas chromatography separation and liquid chromatography purification separation, and the collected PCDD / Fs fractions are determined. The total toxic equivalent of 90μL fly ash extract was 855.486ng / L, of which 15 13 C 12 The recovery results of labeled 2,3,7,8-substituted PCDD / Fs were: 2,3,7,8-TCDD was 51.84%, 1,2,3,7,8-PeCDD was 74.21%, 1 , 2,3,4,7,8-HxCD is 84.94%, 1,2,3,6,7,8-HxCDD is 80.43%, 1,2,3,4,6,7,8-HpCDD is 51.12 %, OCDD is 56.43%, 2,3,7,8-TCDF is 46.11%, 1,2,3,7,8-PeCDF is 64.94%, 2,3,4,7,8-PeCDF is 68.62%, 1,2,3,4,7,8-HxCDF is 76.13%, 1,2,3,6,7,8-HxCDF is 72.72%, 1,2,3,7,8,9-HxCDF is 82.26% , 2, 3, 4, 6, 7, 8-HxCDF is 76.22%, 1, 2, 3, 4, 6, 7, 8-HpCDF is 44.50%, 1, 2, 3, 4, 7, 8, ...

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Abstract

The invention relates to a purification device for dioxin sample pretreatment, in particular to a gas chromatogram (GC) separation and liquid chromatogram (LC) purification on-line combined dioxin sample purification device. The device consists of a high pressure pump, a sample valve, a six-way switching valve, a retention gap column, a GC analysis column, a box body provided with a heating element and an exhaust fan, a four-way valve provided with a heating element, an LC column and the like. According to the device, a sample of big volume is introduced into the gas chromatogram by adopting a loop sample injection technology and the retention gap column, the semi-volatile component of a target is separated by the gas chromatogram, the target component is transferred to the liquid chromatogram and purified, and the friction of the target dioxin compound is selectively collected so as to finish automatic purification of the dioxin sample. The device for purifying the dioxin sample has the advantages of low solvent consumption, simple purification step, high analysis speed, low experiment cost, low health hazard and the like. The device has the same purification effect on other semi-volatile organic pollutants by proper condition change and optimization, and is suitable for separation and analysis of trace semi-volatile durable organic pollutants.

Description

technical field [0001] The invention relates to a purification device used in the pretreatment of dioxin samples, in particular to a dioxin sample purification device for gas chromatography separation and liquid chromatography purification on-line. Background technique [0002] Dioxins (PCDD / Fs) usually refer to polychlorinated dibenzo-dioxins (polychlorinated dibenzo-pdioxins, PCDDs) and polychlorinated dibenzofurans (polychlorinated dibenzofurans, PCDFs), according to the number of chlorine atoms and the substitution position Different, there are 210 isomers of these compounds, and there are 17 kinds of toxic dioxins, most of which are 2, 3, 7, 8-chlorinated compounds, of which 2, 3, 7, 8-TCDD is the most toxic powerful. Because the chemical structure and toxicological properties of coplanar polychlorinated diphenyls (co-PCBs) are similar to dioxins, they are also called dioxin-like PCBs. They are all persistent organic pollutants (POPs), which have a bioaccumulative eff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/34G01N30/02
Inventor 汤凤梅倪余文张海军苏凡陈吉平车迅黄威东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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