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Method for detecting trace N, N-dimethyldithiocarbamate in water

A technology for sodium dimethyl dithiocarbamate and determination of water, which is applied in the field of environmental analytical chemistry, can solve problems such as difficult separation and difficult retention of DMDC, and achieve the effects of good repeatability, mild derivatization reaction conditions, and accurate detection

Active Publication Date: 2013-02-06
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far there is no relevant report about the determination of trace DMDC concentration in water by high performance liquid chromatography, because DMDC has strong polarity and strong hydrophilicity, and the stationary phase C 18 The polarity is weak, DMDC is difficult to retain in the chromatographic column, and it is difficult to separate by direct injection

Method used

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  • Method for detecting trace N, N-dimethyldithiocarbamate in water
  • Method for detecting trace N, N-dimethyldithiocarbamate in water
  • Method for detecting trace N, N-dimethyldithiocarbamate in water

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The first step is to draw a standard curve

[0030] A: Weigh 0.855mL (1.00g) of commercially available analytically pure DMDC, dissolve it in 1L of ultrapure water, and prepare a 1.00g / L DMDC solution, which is used as a standard stock solution for subsequent tests. Pipette 0.025mL, 0.1mL, 0.25mL, 0.5mL, 1.0mL, 2.5mL and 5.0mL standard stock solutions into 500mL volumetric flasks respectively, and dilute to the mark line with ultrapure water to obtain DMDC concentrations of 0.05mg / L, 0.2mgL, 0.5mgL, 1.0mgL, 2.0mg / L, 5.0mg / L and 10.0mgL standard solutions.

[0031] B: Weigh 2.538g of analytical pure I 2 and 33.20g of analytically pure KI, dissolved in 1L of water, where I 2 The content of KI is 0.010mol / L, the content of KI is 0.20mol / L, and this solution is used as a derivatization reagent.

[0032] Take 50mL of each of the standard solutions prepared above with DMDC concentrations of 0.05mg / L, 0.2mg / L, 0.5mg / L, 1.0mg / L, 2.0mg / L, 5.0mg / L and 10.0mg / L , add 0.004mL, 0....

Embodiment 2

[0047] The drawing and accuracy check of standard curve are the same as the first step and second step in Example 1. Take 500mL of the influent water sample of a sewage plant in Shanghai, add derivatization reagent dropwise until the water sample turns light yellow, carry out liquid chromatography detection according to the method described in the first step C of Example 1, the chromatogram of this detection as attached image 3 As shown, the chromatographic peak at 4.796min represents the target peak, its peak height is 7.41mAu, and its peak area is 71.98mAu*min (the results of peak height and peak area are both processed and output by Agilent 1200LC ChemStation). The output peak area results were analyzed according to the standard curve described in the first step D of Example 1. The test results showed that the concentration of DMDC in the sewage plant influent was 689 μg / L.

[0048] Substituting the measured peak area into the formula to calculate the concentration of sod...

Embodiment 3

[0050] The drawing and accuracy check of standard curve are the same as the first step and second step in Example 1. Take 500mL of the influent water sample of a sewage plant in Shanghai, add derivatization reagent dropwise until the water sample turns light yellow, carry out liquid chromatography detection according to the method described in the first step C of Example 1, the chromatogram of this detection as attached Figure 4 As shown, the chromatographic peak at 4.786min represents the target peak, its peak height is 17.82mAu, and its peak area is 124.17mAu*min (the results of peak height and peak area are both processed and output by Agilent 1200LC ChemStation). The output results were analyzed according to the standard curve described in the first step D of Example 1. The test results showed that the concentration of DMDC in the influent of the sewage plant was 1358 μg / L.

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Abstract

The invention relates to a method for detecting trace N, N-dimethyldithiocarbamate in water. The method comprises the following steps: derivatively reacting a water sample containing N, N-dimethyldithiocarbamate with a derivatization reagent at pH value of 7.0-10.0 for 10-40 min, so as to obtain flavescent derivative tetramethyl thiuram disulfide; next, detecting tetramethyl thiuram disulfide by using an efficient liquid chromatography, so as to obtain a chromatogram; inputting a chromatographic peak appearing time into an Agilent 1200 LC chemical workstation and processing the chromatographic peak appearing time in the chemical workstation so as to obtain peak height and peak area; and finally, first finding out the peak area on a longitudinal coordinate in a standard curve graph and then finding out data on a horizontal ordinate, which represents the concentration of N, N-dimethyldithiocarbamate in the water, on a curve corresponding to the longitudinal coordinate representing the peak area. The method for detecting trace N, N-dimethyldithiocarbamate in the water, provided by the invention, has the advantages of mild and rapid derivative reaction, no interference peak, rapidness, simplicity, convenience, high accuracy and good repetitiveness; and trace N, N-dimethyldithiocarbamate in municipal sewage can be effectively detected.

Description

technical field [0001] The invention relates to a method for measuring trace amounts of sodium N,N-dimethyldithiocarbamate in water, which belongs to the technical field of environmental analysis chemistry. Background technique [0002] Sodium N,N-dimethyldithiocarbamate (DMDC for short) is an important chemical raw material and organic synthesis intermediate, widely used in the production of rubber, pesticides and fungicides. When producing rubber, DMDC is often used as a rubber vulcanization accelerator and a terminator for emulsion polystyrene butadiene rubber and styrene butadiene latex. DMDC is the intermediate of pesticide thiram and thiram zinc. As an important bactericide, it can be used to control bacteria, fungi and slime in industrial circulating cooling water towers, and can also be used as a bactericide and algicide in the petroleum and paper industry. In addition, DMDC can also be used as a collector in the mineral flotation process. DMDC can flow into the u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 李咏梅曹先仲
Owner TONGJI UNIV
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