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Dispersive solid-phase extraction gas chromatography method for polychlorinated biphenyls in soil and sediment

A technique of polychlorinated biphenyls and gas chromatography, applied in the field of soil and sediment pollution detection, achieves high sensitivity, satisfactory recovery rate and reproducibility, and simple operation

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

However, according to the current literature at home and abroad, there is no literature report on the application of dispersive solid-phase extraction to the analysis and purification of PCBs in soil or sediment samples.

Method used

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  • Dispersive solid-phase extraction gas chromatography method for polychlorinated biphenyls in soil and sediment
  • Dispersive solid-phase extraction gas chromatography method for polychlorinated biphenyls in soil and sediment
  • Dispersive solid-phase extraction gas chromatography method for polychlorinated biphenyls in soil and sediment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Step (1). Sample collection and sample preparation:

[0056] Pack the collected soil and sediment samples with clean aluminum foil and seal them in polyethylene bags, then transport them back to the laboratory in a portable refrigerator, dry the samples in a freeze dryer for 24 hours, and take them out through a 100-mesh stainless steel sieve , placed in a desiccator for testing.

[0057] Step (2). Sampling and ultrasonic extraction:

[0058] Weigh 10.00g of the sample to be tested, put it in a 50mL centrifuge tube, add 30mL of n-hexane, vortex for 2min, and extract with 480W ultrasonic wave at 30°C for 30min. Ultrasonic desulfurization of copper powder, 6000r / m high-speed centrifugation for 5min; observe the color of the extract, if it is basically colorless and transparent, directly proceed to step (4) concentration and constant volume, that is, only one step of purification is required, otherwise, proceed to step (3) concentrated sulfuric acid purification, that is ...

Embodiment 2

[0097] Example 2. Determination of 7 kinds of polychlorinated biphenyls in the soil samples collected from Zhujiajianjia vegetable field in Zhoushan

[0098] (1) Sample collection and sample preparation: The soil samples collected from the Jia vegetable field in Zhujiajian, Zhoushan were packed with clean aluminum foil and sealed in a polyethylene bag, and then transported back to the laboratory in a portable refrigerator, and then placed in a Dry it in a freeze dryer for 24 hours, take it out and pass it through a 100-mesh stainless steel sieve, and place it in a desiccator for testing.

[0099] Adding standards to the soil samples collected from the Zhujiajian vegetable field in Zhoushan: add 12.5, 100, and 1000 μL of 100 μg / L PCB mixed standard to 10.00 g of the treated soil samples collected from the Zhujiajian vegetable field in Zhoushan Soil samples collected from Zhujiajian Jiacai field in Zhoushan were prepared into low (0.125μg / kg), medium (1.00μg / kg) and high (10.0μg...

Embodiment 3

[0109] Example 3. Determination of 7 kinds of polychlorinated biphenyls in the mud sample collected in the sea area of ​​Zhoushan Daiquyang multiplication and release

[0110] (1) Sample collection and sample preparation: The mud samples collected in the Zhoushan Daiquyang multiplication and release sea area were packed with clean aluminum foil and sealed in polyethylene bags, and then transported back to the laboratory in a portable refrigerator, and then the samples were placed in Dry it in a freeze dryer for 24 hours, take it out and pass it through a 100-mesh stainless steel sieve, and place it in a desiccator for testing.

[0111] Adding standards to the mud samples collected from the Zhoushan Daiquyang breeding and releasing sea area: add 12.5, 100, and 1000 μL of 100 μg / L PCB mixed standard to 10.00 g of the treated mud samples collected in the Zhoushan Daiquyang breeding and releasing sea area. solution, prepared into low (0.125μg / kg), medium (1.00μg / kg) and high (10.0...

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Abstract

Belonging to the technical field of soil and sediment pollution detection, the invention relates to a dispersive solid-phase extraction gas chromatography method for polychlorinated biphenyls (PCBs) in soil and sediment. The method includes: adding n-hexane into a soil or sediment sample to conduct ultrasonic extraction, when the extraction liquid is basically colorless and transparent, subjecting the extraction liquid to rotary evaporation till dry, adding n-hexane, then adding 50-200mg of a N-propylethylenediamine solid phase adsorption agent to carry out dispersive solid-phase extraction, performing centrifugal layering, and introducing 1microliter of the supernatant into a gas chromatography-electron capture detector to conduct detection, otherwise adding a concentrated sulfuric acid purification step after ultrasonic extraction. The detection limit of 7 polychlorinated biphenyls is 0.02-0.03 microgram / kg, the recovery rate is 72-115%, and the relative standard deviation (n=5) is 3.5-6.9%. The method provided by the invention is simple and sensitive, and can quickly realize batch detection of PCBs in soil and sediment.

Description

technical field [0001] The invention belongs to the technical field of soil and sediment pollution detection, and relates to a gas-phase dispersed solid-phase extraction of PCB28, PCB52, PCB101, PCB118, PCB153, PCB138, PCB1807 "indicative polychlorinated biphenyl" monomers in soil and sediment Chromatographic detection method. Background technique [0002] As a typical persistent organic pollutant, polychlorinated biphenyls are widely distributed in environmental media such as water, air, soil, sediment, and organisms, and have strong "three-effects" on the human body. Important chemical products such as exchangers, lubricants, insulating media in transformers and capacitors, plasticizers, paraffin wax extenders, adhesives, organic diluents, dust removers, cutting oils, and carbonless copy paper are widely used in electric power, The fields of plastic processing, chemical industry and printing pose a huge threat to human health and the ecological environment. It is one of t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 胡红美郭远明郝青孙秀梅金衍健钟志
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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