Water polychlorinated biphenyl dispersive solid-phase extraction gas chromatography detection method

A technology of polychlorinated biphenyls and gas chromatography, applied in the field of water pollution detection, to achieve high sensitivity, accurate results, satisfactory recovery and reproducibility

Inactive Publication Date: 2015-11-11
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Looking at the current domestic and foreign literature, there is no literature report on the combination of automatic liquid-liquid extraction and dispersive solid-phase extraction for pretreatment of PCBs in water.

Method used

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  • Water polychlorinated biphenyl dispersive solid-phase extraction gas chromatography detection method
  • Water polychlorinated biphenyl dispersive solid-phase extraction gas chromatography detection method
  • Water polychlorinated biphenyl dispersive solid-phase extraction gas chromatography detection method

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Experimental program
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Effect test

Embodiment 1

[0047] Step (1). Sample collection:

[0048] The collected water samples were packed in 4L brown narrow-mouthed glass bottles with silica gel seals, and then transported back to the laboratory in a portable refrigerator for testing.

[0049] Step (2). Sampling and automatic liquid-liquid extraction:

[0050] Measure 1L of the sample to be tested, put it in a 2L separatory funnel, add 30g of sodium chloride (seawater samples do not need to be added), use 40mL of n-hexane to extract twice with a vertical oscillator, each time for 5min, and let it stand for separation. layer, discarding the aqueous phase.

[0051] When selecting the extraction method, it is considered that although direct solid-phase extraction or solid-phase membrane extraction of water samples can enrich large-volume water samples, the activation, adsorption, and desorption processes of the solid-phase extraction column / membrane take a long time. When the water sample contains a lot of suspended solids, it is...

Embodiment 2

[0082] Embodiment 2. Determination of 7 kinds of polychlorinated biphenyls in lake water of Qiandao Lake

[0083] (1) Collection of samples: the collected Qiandao Lake water was put into a 4L brown narrow-mouthed glass bottle with a silicone gasket, and then transported back to the laboratory in a portable refrigerator for testing.

[0084] Spiked Qiandao Lake water: add 12.5, 100, 1000 μL of 100 μg / L PCB mixed standard solution to 1 L of the treated Qiandao Lake water, and make low (0.00125 μg / L), medium (0.01 μg / L L) and high (0.1 μg / L) three levels of spiked Qiandao Lake water.

[0085] (2) Sampling and automatic liquid-liquid extraction: Weigh 1L of Qiandao Lake water or spiked Qiandao Lake water treated in the above step (1), put it in a 2L separating funnel, add 30g of sodium chloride, and use 40mL of n-hexane Use a vertical oscillator to automatically oscillate and extract twice, each time for 5 min, let stand to separate layers, and discard the water phase.

[0086](...

Embodiment 3

[0093] Example 3. Determination of 7 kinds of polychlorinated biphenyls in the seawater of Zhoushan Daiquyang multiplication and release seawater

[0094] (1) Collection of samples: The collected seawater from Zhoushan Daiquyang multiplication and release sea area was put into a 4L brown narrow-mouth glass bottle with a silicone gasket, and then transported back to the laboratory in a portable refrigerator for testing.

[0095] Adding standard seawater in Zhoushan Daiquyang multiplication and release sea area: add 12.5, 100, 1000μL of 100μg / L PCB mixed standard solution to 1L of the treated Zhoushan Daiquyang multiplication and release seawater to prepare a low (0.00125 μg / L), medium (0.01μg / L) and high (0.1μg / L) three added concentration levels of spiked Zhoushan Daiqu Yang multiplication release seawater.

[0096] (2) Sampling and automatic liquid-liquid extraction: Weigh 1L of Zhoushan Daiquyang multiplication and release seawater treated in the above step (1) or spiked Zho...

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Abstract

The invention relates to a water polychlorinated biphenyl dispersive solid-phase extraction gas chromatography detection method and belongs to the technical field of water pollution detection. The method comprises adding 30g of common salt into a water sample, wherein if the water sample is a seawater sample, the salt addition process is avoided, carrying out automatic liquid-liquid extraction twice by 30-50mL of n-hexane, merging the extract, carrying out rotary evaporation on the extract until drying, adding 1mL of n-hexane into the extract for dissolution, transferring the solution into an injection tube filled with 100-200mg of an N-propylethylenediamine adsorbent, carrying out dispersion solid phase extraction, carrying out filtration after vortex treatment for 30-60s, taking 1 microliter of the filtrate, feeding the filtrate into a gas chromatography-electron capture detector and carrying out detection. The method has seven polychlorinated biphenyl detection limits of 0.0002-0.0003 micrograms per liter, has a recovery rate of 71-107% and has relative standard deviation (n=5) of 3.1-6.2%. The method is simple and sensitive and can realize fast batch detection polychlorinated biphenyl in water.

Description

technical field [0001] The invention belongs to the technical field of water pollution detection and relates to a dispersive solid-phase extraction gas chromatography detection method for PCB28, PCB52, PCB101, PCB118, PCB153, PCB138 and PCB1807 "indicative polychlorinated biphenyls" monomers in a water body. Background technique [0002] Polychlorinated biphenyls, as a class of synthetic chlorinated persistent organic pollutants, have so far discovered 209 isomers, which have the characteristics of high toxicity, long-distance migration, environmental persistence and bioaccumulation, and are easy to dissolve in water, It remains in the atmosphere, soil and other environmental media, and accumulates in human and animal bodies through the food chain, posing a huge threat to human health. It is one of the 12 priority pollutants under the Stockholm Convention in May 2001. Although since 1972, the use and production of PCBs have been gradually stopped globally, their persistence ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 胡红美郭远明孙秀梅金衍健钟志郝青
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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