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Determination method for OCPs in environmental sample

A technology of environmental samples and determination methods, which is applied in the field of detection of OCPs, can solve problems such as the inability to accurately determine the content of OCPs in environmental samples, and achieve the effects of improving accuracy and sensitivity, improving recovery rate and accuracy, and reducing the degree of decomposition

Active Publication Date: 2013-11-27
CSD IDEA BEIJING INST OF ENVIRONMENTAL INNOVATION
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  • Claims
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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to provide a method for measuring OCPs in environmental samples, which can accurately measure the content of OCPs in environmental samples, thereby solving the problem that existing measuring methods cannot accurately measure the content of OCPs in environmental samples

Method used

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  • Determination method for OCPs in environmental sample
  • Determination method for OCPs in environmental sample
  • Determination method for OCPs in environmental sample

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Embodiment 1

[0043] An embodiment of the present invention provides a method for determining OCPs in a soil or sediment sample, comprising the following steps:

[0044] Sample extraction steps: Weigh about 10g of ordinary soil or sediment as the sample to be tested, add 13C-OCPs to purify the internal standard, and use 300mL toluene and acetone (9:1, V / V) mixed solvent Soxhlet extraction for 16-24h to obtain Extraction solution;

[0045] TBA-Sulfite sulfur removal: Concentrate the extract to 10mL, add 10mL tetrabutylammonium sulfite aqueous solution and 10mL isopropanol, shake for 1min, if there is no precipitation (sodium sulfite crystal) in the lower layer solution, add a small amount of sodium sulfite solid powder , until there will be solid residues after repeated shaking, discard the solid residues in the lower layer and keep the organic phase, wash the organic phase with water, remove water with anhydrous sodium sulfate, and wait for the next step of purification;

[0046] Florisil ...

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Abstract

The invention discloses a determination method for OCPs in an environmental sample, which belongs to the field of detection of OCPs. The determination method comprises the following steps: carrying out Soxhlet extraction on a to-be-determined environmental sample so as to obtain a liquid extract containing OCPs; carrying out separation and purification, i.e., concentrating the liquid extract to a constant volume, adding an aqueous solution of tetrabutyl ammonium sulfite and isopropanol, carrying out oscillation until a solid residue is generated after repeated shaking every time, discarding a lower layer, retaining an organic phase, washing the organic phase, removing water by using anhydrous sodium sulfate, carrying out purification by using a Florisil column so as to obtain an eluate, concentrating the eluate to a constant volume and dividing the concentrated eluate into two groups which are used as samples for subsequent detection, wherein one of the groups is a sample of OCPs stable in sulfuric acid and is purified by using a sulfuric acid silica gel column so as to obtain a purified sample, and the other of the groups is a sample of OCPs instable in sulfuric acid and is purified by using an Envi-carb SPE small column so as to obtain a purified sample; and carrying out determination, i.e., respectively analyzing and determining the two groups of purified samples by using an HRGC-HRMS apparatus so as to obtain determination results of the content of OCPs in the two groups of purified samples. The determination method provided by the invention enables accuracy and sensitivity of determination to be improved.

Description

technical field [0001] The invention relates to the field of detecting OCPs, in particular to a method for measuring OCPs content in samples such as soil and sediment. Background technique [0002] Due to the high toxicity, persistence, accumulation and long-distance migration of persistent organic pollutants (POPs), it has attracted widespread attention in the field of environmental science. In 2001, the first batch of 12 POPs were listed as priority pollutants. So far, 21 substances have been included in the "blacklist". These 21 substances can be divided into pesticides (OCPs), industrial chemicals and unintentional discharge by-products. Three categories. [0003] OCPs exist in the environment at trace and ultra-trace levels, and there may be a variety of high-concentration interfering substances in a large number of extramatrix samples: polychlorinated naphthalene (PCN), polychlorinated diphenyl ethers (PCDPEs), polychlorinated Triphenylene (PCTs), studies have shown ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/14
Inventor 李文超陆勇山崎教正杨静宋娇娜孙武
Owner CSD IDEA BEIJING INST OF ENVIRONMENTAL INNOVATION
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