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A detection method for novel nitrogen-containing disinfection by-product n-chloro-2,2-dichloroacetamide in drinking water

A technology of dichloroacetamide and disinfection by-products, which is applied in the fields of municipal water supply and drainage and environmental engineering, can solve the problems of complex detection, low concentration content, high detection cost, etc., simplify the experimental process, facilitate sample testing, and avoid peak delay tail effect

Active Publication Date: 2021-02-12
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] For the detection technology of N-Cl-DCAM, there are currently reports in the literature at home and abroad, only Yu Y and other reports (Yu, Y. and D.A. -2,2-dichloroacetamide), A Previously Overlooked Nitrogenous Disinfection Byproduct in Chlorinated Drinking Waters. Environmental Science & Technology, 2016.51(3):p.1488.) SPE-UPLC / ESI / qTOF detection method, which is mainly used For the identification of new substances, solid phase extraction is required for enrichment, the detection is more complicated and the detection cost is higher; in addition, the concentration of N-Cl-DCAM in drinking water is relatively low, so the establishment of a convenient, effective and rapid determination Method will be crucial for N-Cl-DCAM detection and control studies

Method used

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  • A detection method for novel nitrogen-containing disinfection by-product n-chloro-2,2-dichloroacetamide in drinking water
  • A detection method for novel nitrogen-containing disinfection by-product n-chloro-2,2-dichloroacetamide in drinking water
  • A detection method for novel nitrogen-containing disinfection by-product n-chloro-2,2-dichloroacetamide in drinking water

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Embodiment 1

[0046] A kind of detection method of novel nitrogen-containing disinfection by-product N-Cl-DCAM in drinking water, such as figure 1 As shown, including instrument condition optimization and operation determination.

[0047] Among them, the optimization of instrument conditions includes the determination of the best elution gradient, the best injection volume and the best temperature of the injection port.

[0048] Running assays include determination of working curves, determination of limits of detection and limits of determination.

[0049] Specific steps are as follows:

[0050] 1 Instrument condition optimization

[0051] 1.1 Optimization of chromatographic conditions

[0052] 1.1.1 Determination of the best elution gradient

[0053] In order to avoid missing peaks, the initial gradient is set to A95%, B 5%, according to the analysis results of N-Cl-DCAM, increase the B% in the starting mobile phase and decrease the B% in the ending mobile phase to remove The meaning...

Embodiment 2

[0072] A detection method for a new type of nitrogen-containing disinfection by-product N-Cl-DCAM in drinking water, using ultra-high performance liquid chromatography / triple quadrupole mass spectrometry (AB 5500 LC-MS / MS) to analyze the sample, according to The analysis chromatogram of the sample and the standard working curve of N-Cl-DCAM determine the content of N-Cl-DCAM in the sample. The method specifically includes the following steps:

[0073] (1) Adjust the pH of the sample to about 9.0;

[0074] (2) Determine the operating parameters of AB 5500 LC-MS / MS, including elution gradient, column head pressure, injection volume, inlet temperature and ion collision energy;

[0075] (3) Make the standard working curve of N-Cl-DCAM;

[0076] (a) Preparation of standard solution: Dichloroacetamide (DCAM) and sodium hypochlorite (free chlorine) are mixed in the same stoichiometric ratio (Cl) under the condition of pH=9 2 / N=1:1) mixed and prepared N-Cl-DCAM standard solution, ...

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Abstract

The invention discloses a detection method of a novel nitrogen-containing disinfection by-product N-chloro-2,2-dichloroacetamide (N-Cl-DCAM) in drinking water, which adopts ultra-high performance liquid chromatography / triple quadrupole The mass spectrometer is used for analysis, and the content of N-Cl-DCAM in the sample is determined according to the analysis chromatogram of the sample and the standard working curve of N-Cl-DCAM. N-Cl-DCAM is a newly discovered nitrogen-containing disinfection by-product, and the method of the present invention is more used for the quantitative detection of known substances, and the accuracy is higher; in addition, there is no need to enrich the N in water by solid-phase extraction. ‑Cl‑DCAM, no need to use reagents such as salt, extractant, etc., avoiding direct contact of experimenters with toxic and harmful organic solvents, and at the same time, saving sample testing time and reducing sample cost; using ultra-high performance liquid chromatography / triple quadrupole Mass spectrometry, and determined detailed instrument parameter conditions, can avoid N-Cl-DCAM peak tailing and other phenomena, ensure its normal peak, and can obtain higher detection limit (MDL) and smaller relative standard deviation (RSD).

Description

technical field [0001] The invention belongs to the technical field of municipal water supply and drainage and environmental engineering, and in particular relates to a detection method of a novel nitrogen-containing disinfection by-product N-chloro-2,2-dichloroacetamide (N-Cl-DCAM) in drinking water. Background technique [0002] Disinfection by-products (DBPs), especially nitrogen-containing disinfection by-products (N-DBPs), have attracted increasing attention in the field of drinking water treatment in recent years. Among them, trihalomethanes (THMs), haloacetic acids (HAAs), haloacetonitriles (HANs), haloacetamides (HAMs), halonitromethanes (HNMs), nitrosamines (NMs), etc., especially dichloro Acetonitrile (DCAN), dichloroacetamide (DCAM) and so on have attracted widespread attention. Studies have shown that the concentration level of N-DBPs is much lower than that of carbon-containing disinfection by-products (C-DBPs), and its cytotoxicity and genotoxicity are much hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/24G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/24G01N30/72G01N30/8634
Inventor 林涛戈梦青颜晓姝叶阳张心悦干心彦
Owner HOHAI UNIV
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