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Analysis method for simultaneously detecting iodoacetic acid and aromatic iodide disinfection by-product in water

A technology of disinfection by-products and analytical methods, applied in the field of environmental analytical chemistry, can solve the problems of high detection limit and low recovery rate of iodoacetic acid, and achieves the effects of easy operation and less reagent consumption

Inactive Publication Date: 2019-01-15
NANJING UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to aim at the low recovery rate of iodoacetic acid (monoiodoacetic acid: 25-43%; diiodoacetic acid: 57-67%) and high detection limit in the existing liquid-liquid extraction method, and to establish a method that is more suitable for Solid Phase Extraction Method for Analysis of Iodoacetic Acid in Water

Method used

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  • Analysis method for simultaneously detecting iodoacetic acid and aromatic iodide disinfection by-product in water
  • Analysis method for simultaneously detecting iodoacetic acid and aromatic iodide disinfection by-product in water
  • Analysis method for simultaneously detecting iodoacetic acid and aromatic iodide disinfection by-product in water

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Embodiment 1

[0038] Select a solid phase extraction column, the steps are: respectively pass 1L of water sample (100ng / L) containing monoiodoacetic acid and diiodoacetic acid through three different solid phase extraction columns, namely Oasis HLB column, Oasis MAX column, and Oasis MCX column. Elute with 6 mL of methanol solution containing 2% formic acid, blow the eluent to 0.2 mL with nitrogen, and add 0.3 mL of acetonitrile. Before detection, 0.5 mL of ultrapure water was added to the sample and filtered through a 0.45 μm filter membrane; the sample was detected by HPLC-MS / MS, and then the recovery rate was calculated. The result is as figure 1 As shown, the recoveries obtained by treatment with Oasis MAX column are relatively high, the recovery rate of monoiodoacetic acid is 57%, and the recovery rate of diiodoacetic acid is 45%. The recoveries obtained with both Oasis HLB and Oasis MCX columns were less than 10%. Therefore, the most suitable solid-phase extraction column for iodoa...

Embodiment 2

[0040]To optimize the eluent volume, the steps are as follows: pass 1L of water sample (100ng / L) containing monoiodoacetic acid and diiodoacetic acid through the OasisMAX solid phase extraction column. Use 3 mL, 6 mL, and 9 mL of methanol solution containing 2% formic acid to elute respectively, blow the eluent to 0.2 mL with nitrogen, and add 0.3 mL of acetonitrile. Before detection, 0.5 mL of ultrapure water was added to the sample and filtered through a 0.45 μm filter membrane; the sample was detected by HPLC-MS / MS, and then the recovery rate was calculated. The result is as figure 2 As shown, the results show that the eluent volume has little effect on the recovery rate, so in order to reduce reagent consumption, 3mL is selected as the optimal eluent volume.

Embodiment 3

[0042] To optimize the eluent components, the steps are as follows: pass 1L of water sample (100ng / L) containing monoiodoacetic acid and diiodoacetic acid through the OasisMAX solid phase extraction column. Elute with 3 mL of eluent (1–5%) containing different concentrations of formic acid, blow the eluent to 0.2 mL with nitrogen, and add 0.3 mL of acetonitrile. Before detection, 0.5 mL of ultrapure water was added to the sample and filtered through a 0.45 μm filter membrane; the sample was detected by HPLC-MS / MS, and then the recovery rate was calculated. The result is as image 3 As shown, with the formic acid concentration increasing from 1% to 4%, the recovery rate of iodoacetic acid increases continuously; when the formic acid concentration increases from 4% to 5%, the recovery rate of iodoacetic acid has no significant change. Therefore, the optimal formic acid concentration was selected to be 4% according to the recovery rate. Thus, the optimal elution condition was o...

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Abstract

The invention discloses an analysis method for simultaneously detecting iodoacetic acid and aromatic iodide disinfection by-products in water, belongs to the field of chemical analysis, and solves theproblems in the existing liquid-liquid extraction method of low iodoacetic acid recovery rate, high detection limit and the like. The analysis method takes an Oasis MAX (Waters) column as a solid phase extraction column, and optimizes the extraction conditions including eluent component, eluent volume, sample pH and the like, wherein the recovery rates of monoiodoacetic acid and diiodoacetic acidare all greater than 70%. Compared with the traditional liquid-liquid extraction method, the analysis method for simultaneously detecting the iodoacetic acid and aromatic iodide disinfection by-products in water is more suitable for analyzing the iodoacetic acid in water, is also suitable for the analysis of the aromatic iodide disinfection by-products in water, and is simple and convenient to operate, and high in recovery rate, sensitivity and accuracy.

Description

technical field [0001] The invention relates to the field of environmental analysis chemistry, in particular to an analysis method for simultaneously detecting iodoacetic acid and aromatic iodine disinfection by-products in water. Background technique [0002] To eliminate pathogens in water and prevent the spread of aquatic diseases, disinfection of drinking water has become an essential public safety measure. However, during the disinfection process, the organic matter and bromine and iodide ions in the source water will react with the disinfectant to form disinfection by-products. Specifically, iodide ions in water source water will be rapidly oxidized by disinfectant to hypoiodous acid, and hypoiodous acid will further react with organic matter to form iodized disinfection by-products. The reported iododisinfection byproducts are mainly divided into: iodotrihalomethane, iodofatty acid, iodoacetamide and aromatic iododisinfection byproducts. Toxicological studies have s...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/7233G01N2030/009G01N2030/027
Inventor 龚婷婷胡绍洋王俊杰鲜啟鸣
Owner NANJING UNIV
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