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Method and device for on-line enrichment and determination of ultra-trace methyl mercury and/or divalent mercury

A technology of methylmercury and divalent mercury, applied in the field of environmental analytical chemistry, can solve the problems of inability to achieve high multiple enrichment of small-volume samples, which is not conducive to practical application, and cumbersome processing methods, so as to improve green safety and shorten the The time required for the experiment, the effect of reducing the use of toxic reagents

Active Publication Date: 2020-06-09
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the pretreatment method of reduction / derivatization purge and trap is too cumbersome, which is not conducive to practical application
The films used in the gradient diffusion film method are expensive and cannot be used for large-scale detection of actual environmental samples
The offline solid-phase extraction method is also relatively cumbersome, and the reagents used for elution require a large volume, so high-fold enrichment of small-volume samples cannot be achieved.

Method used

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  • Method and device for on-line enrichment and determination of ultra-trace methyl mercury and/or divalent mercury
  • Method and device for on-line enrichment and determination of ultra-trace methyl mercury and/or divalent mercury
  • Method and device for on-line enrichment and determination of ultra-trace methyl mercury and/or divalent mercury

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0108] (1) Use a 10 mL glass flat-tip syringe to draw 5 mL of dithizone solution with a content of 12.5 μg, filter it, and put it into a 5 mL first quantitative loop through the first valve.

[0109] (2) Turn the first valve to inject mode, turn on pump A, the carrier liquid flows through the first quantitative loop at a flow rate of 5mL / min and carry dithizone to the enrichment column for modification, and turn off pump A after 84s, Switch the first valve back to load mode.

[0110] (3) Draw up 5 mL of a mixed solution containing 10 ng / L methylmercury and 10 ng / L divalent mercury with a 10 mL glass flat-tip syringe, filter it and put it into the 5 mL first quantitative loop through the first valve.

[0111] (4) Switch the first valve to the inject mode, turn on pump A, and the carrier liquid flows through the first quantitative loop at a flow rate of 5mL / min to carry methylmercury and divalent mercury to the enrichment column for enrichment, 84s Finally, turn off pump A and sw...

Embodiment 2-7

[0114] Using the enrichment detection steps as in Example 1, the difference is that in Examples 2-7, the dithizone content is 0.05 μg, 0.5 μg, 1 μg, 2.5 μg, 25 μg and 50 μg, corresponding to dithizone The concentrations of the hydrazone solution were 0.01 mg / L, 0.1 mg / L, 0.2 mg / L, 0.5 mg / L, 5 mg / L and 10 mg / L. The test results see figure 2 shown.

[0115] Such as figure 2 As shown, as can be seen from the test results of Examples 1-7, when the quality of the modification activator increases, the enrichment effect of methylmercury and / or divalent mercury is better; but when the quality of the modification activator is greater than a certain value When , the enrichment effect gradually remained stable. Considering comprehensively, 12.5 μg is the optimal addition quality of the modified activator, that is, the ratio of the loaded amount of the modified activator to the carbon load of the enrichment column is 1.39 (μg w(%) -1 ).

Embodiment 8

[0117] (1) Use a 10 mL glass flat-tip syringe to draw 5 mL of dithizone solution with a content of 12.5 μg, filter it, and put it into a 5 mL first quantitative loop through the first valve.

[0118] (2) Turn the first valve to inject mode, turn on pump A, the carrier liquid flows through the first quantitative loop at a flow rate of 5mL / min and carry dithizone to the enrichment column for modification, and turn off pump A after 84s, Switch the first valve back to load mode.

[0119] (3) Draw up 5 mL of methylmercury solution with a concentration of 10 ng / L using a 10 mL glass flat-tip syringe, filter it and put it into the 5 mL first quantitative loop through the first valve.

[0120] (4) Turn the first valve to inject mode, turn on pump A, the carrier liquid flows through the first quantitative loop at a flow rate of 5mL / min and carry methylmercury to the enrichment column for enrichment, and turn off pump A after 84s , turn the first valve back to load mode.

[0121] (5) ...

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Abstract

The invention discloses a method and a device for the on-line enrichment and determination of ultra-trace methyl mercury and / or divalent mercury. The method comprises the following steps: modifying and activating an enrichment column; carrying out extraction and enrichment on methyl mercury and / or divalent mercury by utilizing the modified and activated enrichment column; eluting the methyl mercury and / or the divalent mercury enriched on the enrichment column by utilizing eluent; and separating the enriched methyl mercury and / or divalent mercury by using the eluent, and carrying out online ultra-trace determination on the methyl mercury and / or divalent mercury desorbed from the separation column by using a detector. According to the method and the device disclosed by the invention, the enrichment and elution steps are greatly simplified, the use of toxic reagents is reduced, and the green safety of the method is improved while the method and the device are suitable for detecting ultra-trace methyl mercury and divalent mercury; and on the basis of small sample size, a better detection limit effect is achieved. Therefore, the invention provides the method and the device for on-line enrichment and determination of ultra-trace methyl mercury and / or divalent mercury, which are efficient, convenient and good in performance.

Description

technical field [0001] The invention relates to the field of environmental analytical chemistry, in particular to a method and device for online enrichment and determination of ultra-trace methylmercury and / or divalent mercury. Background technique [0002] Mercury and its compounds are regarded as an important class of global pollutants due to the characteristics of long-distance transport in the atmosphere, accumulation in the food chain, and high toxicity. In recent years, the formal entry into force of the Minamata Convention indicates that it is urgent to strengthen research on mercury. Methylmercury and divalent mercury have been widely concerned by scholars at home and abroad because of their high toxicity and strong mobility. Because the concentration of mercury ions in the environment is mostly at ultra-trace level, it is difficult to analyze and detect it directly with existing instruments. The existing pretreatment methods for the analysis and detection of ultra...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08G01N30/86
CPCG01N30/02G01N30/08G01N30/8679
Inventor 阴永光王颖方莹莹蔡勇谭志强
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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