Method for simultaneously quickly detecting diversified organic phosphate ester flame retardants in soil

A technology of organic phosphate ester and flame retardant, which is used in measurement devices, instruments, scientific instruments, etc., can solve problems such as poor selectivity and sensitivity, long pretreatment time, and complicated operation, so as to reduce operation time and reduce human interference. , the effect of simplifying the operation process

Active Publication Date: 2017-10-17
丹东龙泽化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The extraction and purification in the experimental process are carried out in two steps, the pretreatment time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The invention is used to analyze the organophosphate in the soil of the riparian zone of the main stream of the Liaohe River.

[0026] 1. Take an appropriate amount of riparian soil and freeze-dry it for 24 hours, then grind it and pass it through a 1 mm sieve.

[0027] 2. Accurately weigh 5.00 g of activated silica gel that has been activated at 200 °C for 24 hours and deactivated with 3% deionized water by weight, and place it in a 34 mL stainless steel accelerated solvent extraction that has been placed in a cellulose filter membrane. In the pool, put 2.00 g of activated copper powder that has been activated with dilute sulfuric acid and washed with water and acetone until neutral, then cover a cellulose filter membrane on the copper powder, and accurately weigh 10.00 g of sieved soil sample placed in the extraction cell, and then added 20 ng of TnBP- d 27 and TPhP- d 15 , stir well. The remaining space of the extraction tank is filled with diatomaceous earth, a...

Embodiment 2

[0037] The invention is used to analyze the organophosphate in the wetland soil of Liaohe Estuary.

[0038] 1. Take an appropriate amount of wetland soil and freeze-dry it for 24 hours, then grind it and pass it through a 1 mm sieve.

[0039] 2. Accurately weigh 5.00 g of activated silica gel that has been activated at 200 °C for 24 hours and deactivated with 3% deionized water by weight, and place it in a 34 mL stainless steel accelerated solvent extraction that has been placed in a cellulose filter membrane. In the pool, put 2.00 g of activated copper powder that has been activated with dilute sulfuric acid and washed with water and acetone until neutral, then cover a cellulose filter membrane on the copper powder, and accurately weigh 10.00 g of sieved soil sample placed in the extraction cell, and then added 20 ng of TnBP- d 27 and TPhP- d 15 , stir well. The remaining space of the extraction tank is filled with diatomaceous earth, and then accelerated solvent extract...

Embodiment 3

[0049] The invention is used to analyze the organic phosphate in the farmland soil of Shenyang City.

[0050] 1. Take an appropriate amount of farmland soil and freeze-dry it for 24 hours, then grind it and pass it through a 1 mm sieve.

[0051] 2. Accurately weigh 5.00 g of activated silica gel that has been activated at 200 °C for 24 hours and deactivated with 3% deionized water by weight, and place it in a 34 mL stainless steel accelerated solvent extraction that has been placed in a cellulose filter membrane. In the pool, put 2.00 g of activated copper powder that has been activated with dilute sulfuric acid and washed with water and acetone until neutral, then cover a cellulose filter membrane on the copper powder, and accurately weigh 10.00 g of sieved soil sample placed in the extraction cell, and then added 20 ng of TnBP- d 27 and TPhP- d 15 , stir well. The remaining space of the extraction tank is filled with diatomaceous earth, and then accelerated solvent extr...

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PUM

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Abstract

The invention discloses a method for simultaneously quickly detecting diversified organic phosphate ester flame retardants in soil, and relates to a method for detecting soil. The method includes carrying out freeze drying on soil samples, grinding the soil samples, sieving the soil samples by sieves with the mesh sizes of 1mm, then placing the soil samples in glass bottles calcined at the temperatures of 450 DEG C and storing the glass bottles with the soil samples in refrigerators at the temperatures of 4 DEG C; simultaneously extracting and purifying the soil samples by the aid of accelerated solvent extraction apparatuses and qualitatively and quantitatively analyzing 13 types of organic phosphate esters by the aid of gas chromatography-tandem ion trap mass spectrometry. The method has the advantages that the samples are simultaneously extracted and purified, operation procedures are simple, and the method is low in organic solvent consumption and short in consumed time; the selectivity and the sensitivity of target compounds can be improved by the gas chromatography-tandem ion trap mass spectrometry; the standard recovery rates of the 13 types of organic phosphate esters range from 81.71% to 106.91%, the relative standard deviation is lower than 12%, and accordingly the method is excellent in accuracy and precision; the detection limit of the method ranges from 0.10 ng/g to 0.22 ng/g, the quantification limit of the method ranges from 0.33 ng/g to 0.72 ng/g, and accordingly trace analysis can be carried out by the aid of the method.

Description

technical field [0001] The invention relates to a method for detecting soil, in particular to a method for rapidly detecting multiple organic phosphate flame retardants in soil at the same time. Background technique [0002] Organophosphate esters (Organophosphate esters, OPEs) are widely used as flame retardants or plasticizers in furniture and home decoration materials, electronic equipment, plastic products and floor polishes. OPEs are mainly added to materials by means of addition rather than chemical bonding, and most of them are semi-volatile, and can easily enter various environmental media through volatilization, product wear and leakage. At present, OPEs have been detected in various environmental samples such as sewage and sludge, surface water, indoor and outdoor air, atmospheric particles and dust, sediment and soil. However, OPEs are not safe, and many studies have shown that organophosphates have potential biotoxic effects and can be enriched in organisms. Fo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/062G01N2030/146
Inventor 罗庆王诗雨孙丽娜王辉
Owner 丹东龙泽化工有限责任公司
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