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Pretreatment method for determining polycyclic aromatic hydrocarbon and polychlorinated biphenyl organic pollutants in marine sediments

A technology for marine sediments and organic pollutants, applied in the application field of environmental organic pollutant analysis methods, can solve the problems of large solvent consumption, influence of experimental results, and many interfering substances, so as to achieve less solvent consumption and avoid interfering substances. The introduction and analysis methods are simple and effective

Inactive Publication Date: 2020-05-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above methods are time-consuming, labor-intensive, and consume a large amount of solvent, and the more cumbersome the pre-treatment process, the more interferences are introduced, which will affect the experimental results.

Method used

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  • Pretreatment method for determining polycyclic aromatic hydrocarbon and polychlorinated biphenyl organic pollutants in marine sediments
  • Pretreatment method for determining polycyclic aromatic hydrocarbon and polychlorinated biphenyl organic pollutants in marine sediments
  • Pretreatment method for determining polycyclic aromatic hydrocarbon and polychlorinated biphenyl organic pollutants in marine sediments

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Take three empty ASE extraction cells of 1#, 2#, and 3#, add septa and perform pre-extraction on an accelerated solvent extraction apparatus, and use the system solvent n-hexane: dichloromethane (1 :1,v / v) for cleaning.

[0022] (2) Add 0.5 g of the florisil previously calcined in a muffle furnace (500° C., 4.5 h) into the extraction pool, and put a clean septum into the extraction pool. The marine sediment samples were naturally air-dried, weighed 1g, and placed in the above-mentioned two ASE extraction pools 1# and 2# respectively, and the 3# extraction pool was used as the experimental blank.

[0023] (3) Add 80 μL of 16 kinds of polycyclic aromatic hydrocarbon standard solutions and 7 kinds of polychlorinated biphenyl standard solutions into the 2# extraction cell by weight loss method as quality control samples to determine the recovery rate of addition.

[0024] (4) Accelerated solvent extraction method (ASE): Pre-extraction: extract the ASE extraction cell a...

Embodiment 2

[0028] (1) Take three empty ASE extraction cells of 1#, 2#, and 3#, add septa and perform pre-extraction on an accelerated solvent extraction apparatus, and use the system solvent n-hexane: dichloromethane (1 :1,v / v) for cleaning.

[0029] (2) Add 0.5 g of the silica gel previously calcined in a muffle furnace (500° C., 4.5 h) into the extraction pool, and put a clean septum into the extraction pool. The marine sediment samples were naturally air-dried, weighed 1g, and placed in the above-mentioned two ASE extraction pools 1# and 2# respectively, and the 3# extraction pool was used as the experimental blank.

[0030] (3) Add 80 μL of 16 kinds of polycyclic aromatic hydrocarbon standard solutions and 7 kinds of polychlorinated biphenyl standard solutions into the 2# extraction cell by weight loss method as quality control samples to determine the recovery rate of addition.

[0031] (4) Accelerated solvent extraction method (ASE): Pre-extraction: extract the ASE extraction cell a...

Embodiment 3

[0035] (1) Take three empty ASE extraction cells of 1#, 2#, and 3#, add septa and perform pre-extraction on an accelerated solvent extraction apparatus, and use the system solvent n-hexane: dichloromethane (1 :1,v / v) for cleaning.

[0036] (2) Add 0.5 g of the neutral alumina previously calcined in a muffle furnace (500° C., 4.5 h) into the extraction pool, and put a clean septum into the extraction pool. The marine sediment samples were naturally air-dried, weighed 1g, and placed in the above-mentioned two ASE extraction pools 1# and 2# respectively, and the 3# extraction pool was used as the experimental blank.

[0037] (3) Add 80 μL of 16 kinds of polycyclic aromatic hydrocarbon standard solutions and 7 kinds of polychlorinated biphenyl standard solutions into the 2# extraction cell by weight loss method as quality control samples to determine the recovery rate of addition.

[0038] (4) Accelerated solvent extraction method (ASE): Pre-extraction: extract the ASE extraction...

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Abstract

The invention belongs to the field of an application of environmental organic pollutant analysis methods, and particularly relates to an application of integrated accelerated solvent extraction and purification in a pretreatment method for determining polycyclic aromatic hydrocarbon and polychlorinated biphenyl organic pollutants in marine sediments and quality control of interferents. A marine sediment sample can achieve integration of extraction and purification through the method, an extraction solvent is n-hexane: dichloromethane (1: 1, v / v), an extraction temperature is 80-140 DEG C, a cycle index is 3-8, and static extraction time is 5-20 min; a purification adsorbent is 0.5-2g of Florisil, the silica gel, neutral aluminum oxide, alkaline aluminum oxide, acidic aluminum oxide and Mg-Al-LDO; and an isotope dilution gas chromatography-tandem mass spectrometry method is adopted for detection, an adding standard recovery rate of 16 PAHs in a sample is 80%-120%, the adding standard recovery rate of 7 PCBs is 85%-120%, and a relative standard deviation is 0.5%-6.0%. The pretreatment method is a green, simple, convenient and rapid method for detecting the organic pollutants in the marine sediment sample.

Description

technical field [0001] The invention belongs to the field of application of analysis methods for environmental organic pollutants, in particular to the application of integrated accelerated solvent extraction and purification in the pretreatment method for the determination of polycyclic aromatic hydrocarbons and polychlorinated biphenyl organic pollutants in marine sediments and the application of Quality control of interferents. Background technique [0002] With the continuous development of the marine industry and the acceleration of coastal industrialization and urbanization, the quality of the marine environment is facing the danger of deteriorating. The monitoring results of the sediment and marine biomass in the coastal waters show that: the main pollution in marine sediments The substances are mercury, copper, arsenic, cadmium, lead, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), etc. Polycyclic aromatic hydrocarbons (PAHs) are a class o...

Claims

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Application Information

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IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/062
Inventor 李蕾李婧
Owner BEIJING UNIV OF CHEM TECH
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