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Method for separating and detecting organo-mercuric compound content

An organic mercury and compound technology, which is applied in the field of separation and detection of organic mercury compound content, can solve the problems of unstable reagents, easy interference of transition metal ions, etc., and achieves the effects of low operating cost, environmental friendliness, and reduction of waste liquid.

Active Publication Date: 2011-02-09
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reagents (such as potassium persulfate and potassium borohydride) used in this method are unstable, and transition metal ions are prone to interference, which has certain limitations.

Method used

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  • Method for separating and detecting organo-mercuric compound content
  • Method for separating and detecting organo-mercuric compound content
  • Method for separating and detecting organo-mercuric compound content

Examples

Experimental program
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Embodiment 1

[0039] Example 1: Determination of the form of organic mercury in fish and shellfish samples, using ammonium formate and 2-mercaptoethanol in the mobile phase as photochemical reaction reagents to determine the organic mercury in the sample.

[0040] Experimental equipment see Figure 4

[0041] The steps are:

[0042] (1) Extraction of organic mercury: Weigh 0.2 g of sample into a 40 mL glass centrifuge tube, add 2 mL of KOH in methanol (1:4, w: v) and shake overnight. Add 6mL CH 2 Cl 2 , and then added 1.5 mL of concentrated hydrochloric acid dropwise, shaken for 45 min and then centrifuged (3000 rpm, 15 min). Take 3.0-4.0mL organic phase and transfer to 10mL glass centrifuge tube, add 1mL Na 2 S 2 o 3 solution. After shaking for 45min, centrifuge (3500 rev / min, 15min), get the upper layer aqueous phase sample injection, the effluent of high performance liquid chromatography enters in the polytetrafluoroethylene pipeline 4, under the irradiation of ultraviolet lamp, ...

Embodiment 2

[0054] Example 2 Determination of methylmercury in fish and shellfish samples using ammonium acetate and 2-mercaptoethanol in the mobile phase as photochemical reaction reagents.

[0055] The steps are:

[0056] (1) Extraction of organic mercury: Weigh 0.2 g of sample into a 40 mL glass centrifuge tube, add 2 mL of KOH in methanol (1:4, w: v) and shake overnight. Add 6mL CH 2 Cl 2 , and then added 1.5 mL of concentrated hydrochloric acid dropwise, shaken for 45 min and then centrifuged (3000 rpm, 15 min). Take 3.0-4.0mL organic phase and transfer to 10mL glass centrifuge tube, add 1mL Na 2 S 2 o 3 solution. After oscillating for 45 minutes, centrifuge (3500 r / min, 15 minutes), take the upper aqueous phase and inject samples for liquid chromatography-atomic fluorescence measurement.

[0057] (2) Determination: Prepare four forms of mercury mixed standard concentration: 5, 10, 20, 50, 100, 200μgL -1 . The measuring conditions of the instrument are shown in Table 4. The...

Embodiment 3

[0069] The present embodiment is substantially the same as embodiment 1, and the difference is the mobile phase of the present embodiment, ammonium formate 10mmol L -1 , 2-mercaptoethanol was 0.05% (v / v).

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Abstract

The invention provides a test method for organic mercury compounds, which comprises the following steps: first the organic mercury sample and separates the sample are extracted through high performance liquid chromatography, the mobile phase of which comprises:2-mercaptoethanol, one or more lower fatty acids and lower fatty acid salts, leads the chromatographic column draw off to cause chemical reaction under the ultraviolet light, the reaction solution is mixed with inert gases, the gas-liquid mixture is separated through a gas-liquid separator, the highly performance liquid chromatography chart is obtained through testing the separated sample gas phase through atomic fluorescence spectrometer; according to the standard curve between the organic mercury density and the peak area, the organic mercury concentration in the sample to be tested is figured out through the separated sample gas phase peak area in the highly performance liquid chromatography chart. The invention provides a separating and testing method for a plurality of organic mercury in the sample to be tested.

Description

technical field [0001] The invention relates to a method and equipment for separating and detecting the content of organic mercury compounds. Background technique [0002] Since the Industrial Revolution, mercury concentrations in the environment have increased significantly. As a global pollutant, mercury exists in various environmental media and food, posing a threat to human, animal and plant health. Due to man-made mercury release and alkylation in natural processes, there are many forms of mercury in environmental media, which not only affect the toxicity and accumulation of mercury to organisms, but also affect the migration and transmission of mercury in various environmental media. Therefore, the development of sensitive and specific analytical methods for the analysis of mercury speciation is of great significance for elucidating the toxicity and geochemical behavior of mercury. [0003] Mercury compounds include inorganic mercury and organic mercury. Inorganic m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 江桂斌阴永光刘景富河滨史建波
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI