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Capillary solid phase microextraction device and extracting method

A solid-phase microextraction column and extraction device technology, applied in the extraction field, can solve the problems of difficulty in ensuring the repeatability of analysis results, unsatisfactory extraction and enrichment multiples, and short service life of extraction fibers, avoiding sample adsorption and high prices. , The effect of increasing the extraction enrichment ratio and speeding up the extraction balance speed

Inactive Publication Date: 2004-06-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, the amount of adsorbed stationary phase in conventional fiber-needle solid-phase microextractors is ≤1 μL, which limits the extraction enrichment factor and cannot meet the requirements of many trace analysis; in addition, the manual offline operation mode is still used in the operation process, which is difficult to guarantee the analysis The reproducibility of the results; and the short service life of the extraction fiber in the extractor (≤30 times) also increases the analysis cost

Method used

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  • Capillary solid phase microextraction device and extracting method
  • Capillary solid phase microextraction device and extracting method
  • Capillary solid phase microextraction device and extracting method

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The parameters of the sample pretreatment device for extraction and enrichment of volatile and semi-volatile organic pollutants in drinking water and surface water are as follows:

[0033] The capillary solid-phase microextraction column is a 5M×0.53mm inner diameter×1.5μm film thickness OV-1 elastic quartz capillary column; the desorption temperature is 220°C; the transfer tube uses an elastic quartz capillary with an inner diameter of 1M×120μm, and the temperature of the jacket heating tube is 120°C.

[0034] A 20mL water sample is equipped with a concentration of 10μg / L naphthalene, passed through a capillary solid-phase microextraction column at a flow rate of 0.6mL / min, and analyzed with an Agilent 6890-Plus gas chromatograph. The obtained analysis spectrum is as follows figure 2 .

Embodiment 2

[0036] Extraction and enrichment of organochlorine pesticide residues in water. The desorption temperature of the extraction column is 270° C., and other conditions are the same as in Example 1. Its analytical spectrum is as image 3 .

Embodiment 3

[0038] Extraction and enrichment of organophosphorus pesticide residue components in water. The capillary solid-phase microextraction column uses a 5M×0.53mm inner diameter×1.5μm film thickness SE-54 (polydimethylsiloxane containing 5% phenyl) quartz capillary column; the desorption temperature of the extraction column is 250°C. Others are with embodiment 2. Its analytical spectrum is as Figure 4 .

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Abstract

The solid phase capillary miniature extractor includes mainly one four-way valve and one six-way valve connected via gas path; one capillary extracting column made of elastic hollow quartz capillary, stainless steel capillary or stainless steel capillary with inside quartz lining, connected to the six-way valve and with cross-linking coated fixing phase in the inside wall; one heater outside the extracting column for heating; one miniature three-way pipe connected to the extracting column, the six-way valve and conveying gas path for the desorption sample; and one conveying pipe inserted into the gas chromatographic sample injector. The liquid sample pushed by the auxiliary carrier gas enters first to the extracting column via the four-way valve and the six-way valve; the four-way valve is then turned and the extracting column is heated; and the six-way valve is finally turned for the desorbed component to enter the gas chromatographic sample injector.

Description

technical field [0001] The invention relates to a liquid-solid extraction and gas-solid adsorption technology, which is used for sample pretreatment and target component extraction and enrichment in chromatographic analysis and instrumental analysis. Specifically, it relates to a capillary solid-phase microextraction device. [0002] The present invention also relates to an extraction method realized by using the above-mentioned device. Background technique [0003] In terms of environmental protection, analysis of organic pollutants contained in drinking water, beverages, food, etc., and component analysis in animal and plant extracts, different forms of liquid-liquid, liquid-solid extraction and headspace gas-solid adsorption technology have been used. , in order to realize the sample pretreatment functions such as phase transfer and selective enrichment of the target components in the sample, and meet the requirements of the analytical instrument for sample analysis and ...

Claims

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Application Information

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IPC IPC(8): B01D11/02
Inventor 关亚风王涵文朱道乾王海龙
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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