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A kind of gas-liquid phase on-line combined method for purifying dioxin-like samples

A dioxin-based, liquid-phase technology, applied in the preparation of test samples, measuring devices, instruments, etc., can solve the problems of complex sample purification and quantitative analysis process, non-reusable 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: 2011-12-28
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 found in ultra-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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  • A kind of gas-liquid phase on-line combined method for purifying dioxin-like samples
  • A kind of gas-liquid phase on-line combined method for purifying dioxin-like samples
  • A kind of gas-liquid phase on-line combined method for purifying dioxin-like samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Using nitrogen as the carrier gas, the quantitative tube 8 has a volume of 100 μL, the retention gap column 10 is a 4m×0.53mm ID quartz capillary column, and the GC analysis column 13 is DB-5 (30m×0.32mm×0.25μm), using a self-made LC column, Put 3g of 18-32μm basic alumina packing into a 15cm×0.46mmID LC empty column tube, use wet homogenization to pack the column, and equilibrate the column with n-hexane.

[0032] The pressure of the pressure stabilizing valve 5 is 0.22Mpa, the length and inner diameter of the pipelines through which the first carrier gas and the second carrier gas reach the tee joint 11 are the same, and the inlet of the first carrier gas and the second carrier gas The gas pressure is 0.15Mpa, and the carrier gas flow rate is 1mL / min, so that the pressure of the first carrier gas and the second carrier gas at the tee joint 11 are consistent;

[0033] Sampling: the concentrated soil, sediment, solid waste, air and waste gas, biological sample extracts ...

Embodiment 2

[0042] Experimental method conditions and devices are the same as in Example 1, 90 μL of fly ash extract solution is added to 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 12The 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, ...

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Abstract

The invention relates to a method for purifying dioxin type sample, in particular to a method for purifying sample through the following steps: based on the properties of dioxin type semi-volatile organic pollutant, combining GC separation with LC purification, introducing samples with large volume to GC through circular sampling and retention gap column; separating volatile ingredients from non-volatile ingredients through gasification and blowing; separating semi-volatile ingredients from easily volatile ingredients through GC separation, collecting the semi-volatile ingredients through stream switching; and separating the dioxin type semi-volatile organic pollutant from the semi-volatile ingredients through LC separation. Used matching equipment is composed of a high pressure pump, a sample valve, a six-way switching valve, a retention gap column, a GC analytical column, a four-way valve and an LC column. When purifying the dioxin type sample, the invention is advanced in solvent saving, simple operation and low experiment cost, and is applicable to separation and analysis of trace semi-volatile durable organic pollutant.

Description

technical field [0001] The invention relates to a method for purifying dioxin samples in combination with on-line GC separation and LC purification. Background technique [0002] Dioxins generally refer to polychlorinated dibenzo-dioxins (polychlorinated dibenzo-pdioxins, PCDDs) and polychlorinated dibenzofurans (polychlorinated dibenzofurans, PCDFs), according to the number of chlorine atoms and substitution positions, such compounds There are 210 isomers in total, and there are 17 toxic dioxins, most of which are 2, 3, 7, and 8-chlorinated compounds, of which 2, 3, 7, 8-TCDD is the most toxic. 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 effect and can enter the human body through the skin, digestive tract, respiratory tract, etc., causing skin chloracne, headache, inso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34G01N30/02
Inventor 倪余文汤凤梅张海军陈吉平苏凡车迅黄威东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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