Solid phase extraction method of N-nitrosodimethylamine in water

A nitrosodimethylamine, solid-phase extraction column technology, applied in separation methods, chemical instruments and methods, extraction water/sewage treatment, etc., can solve the problem of expensive materials, low recovery efficiency, and large environmental pollution. problems, to achieve the effect of simple and easy operation, avoiding easy emulsification of the interface, and reducing processing costs

Inactive Publication Date: 2010-09-15
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Using this method to remove NDMA in water, the removal rate can reach more than 92%, but the filler ratio in this method is complicated, and methods such as pressing are also used in the preparation
If this method is applied to solid-phase extraction technology, it will expose the problems of complicated manufacturing process and high cost.
[0004] Among the current sample processing methods designed for the physical and chemical properties of NDMA, the traditional liquid-liquid extraction requires multiple extractions, and at least 1 / 3 of the sample volume of organic solvent is used each time. Therefore, this method consumes a large amount of solvent, which is harmful to The degree of environmental pollution is large; and the interface is prone to emulsification during the liquid-liquid extraction process, which affects the extraction efficiency
Foreign Charrois et al. applied solid phase extraction (SPE) to deal with NDMA content in aqueous solution. In this method, Lichrolut EN and Ambersorb 572 were used as adsorbents. The operation process was somewhat cumbersome and the recovery efficiency was not high.
There are also studies to improve the use of Carboxen 564 as an adsorbent, and the adsorption efficiency has been significantly improved, but due to the high price of the material, it has not been widely used.

Method used

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  • Solid phase extraction method of N-nitrosodimethylamine in water

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Experimental program
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Effect test

Embodiment 1

[0024] (1) Select a tube with a size of 5mL, and place a polypropylene sieve plate (purchased from Tianjin Bona Aijieer Technology Co., Ltd.) on the bottom, select 400mg of a particle size of 20 mesh, and a specific surface area of ​​1000m 2 / g of activated carbon (purchased from Supelco company, its English name is activated coconut charcoal), the activated carbon is washed and stirred into a paste, then suction filtered until it is nearly dry and in the form of agglomerates, and then transferred to the tube for filling. Soak and wash with methanol and deionized water in sequence, drain, and then compress the upper layer with a layer of sieve plate, and package it for later use.

[0025] (2) Activate the above-prepared solid-phase extraction column with methanol and deionized water of one column volume in turn, drain it under negative pressure, measure 5 mL of the aqueous solution of the NDMA standard with a concentration of 1 ng / μL, and use 2-5 mL Pass the sample through the...

Embodiment 2

[0027] The particle size of activated carbon is 40 mesh, and other steps are the same as implementation 1.

Embodiment 3

[0029] The specific surface area of ​​activated carbon is 1500m 2 / g, other steps are the same as implementation 1.

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Abstract

The invention relates to a solid phase extraction method of N-nitrosodimethylamine in water. The method comprises preparing a solid phase extraction column and a using method of the solid phase extraction column. The prepared solid phase extraction (SPE) column is prepared by using 400 to 600 milligrams of active carbon with a particle size of 20 to 40 meshes and a specific surface area of 1,000 to 1,500m<2> / g, processing the active carbon, filling the active carbon, compressing the active carbon and sealing the active carbon for later use; and the using method comprises the processes of activation by methanol and deionized water, loading, leaching with normal hexane, and eluting with dichloromethane or methanol. The method of the invention has the advantages that: the SPE column can be manufactured simply and conveniently at low cost; and in use, the SPE column is high in yield, stable and environmentally-friendly and prevents interface emulsification effectively; and the adaptability of the SPE column is improved.

Description

technical field [0001] The invention relates to a solid phase extraction method of N-nitrosodimethylamine in water. technical background [0002] N-Nitrosodimethylamine (NDMA) can form electrophilic alkyl free radicals under the action of enzymes in organisms, which can lead to alkylation of DNA in cells, cause gene mutations, and exhibit carcinogenicity. In the current research on NDMA, there are still many deficiencies in the processing methods of NDMA. [0003] Chinese patent CN101596447A (disclosure date: December 9, 2009) discloses a filter medium for removing NDMA in water and a preparation method thereof. The mixture is mixed first, then the mixture is pressed, sintered and cooled. This method is used to remove NDMA in water, and the removal rate reaches more than 92%, but the filling ratio in this method is complicated, and methods such as pressing are also used in the preparation. If this method is applied to solid-phase extraction technology, the problems of rel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/08B01D15/22B01J20/20B01J20/30B01J20/34C02F1/26C02F101/38
Inventor 刘永东刘清明周全钟儒刚
Owner BEIJING UNIV OF TECH
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