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Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms

A high-performance liquid chromatography and atomic fluorescence spectrometry technology, applied in the field of environmental analytical chemistry, can solve the problems of complicated instruments and easy aging of post-column pipelines, and achieve the effects of simple instruments, environmental friendliness and convenient operation.

Inactive Publication Date: 2011-03-30
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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Problems solved by technology

However, the use of external energy sources such as ultraviolet rays and microwaves complicates the instrument, and the use of strong oxidants also makes the post-column pipelines prone to aging

Method used

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  • Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms
  • Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms
  • Efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0021] Determination of mercury speciation in fish and human hair samples.

[0022] The steps are:

[0023] (1) Extraction of mercury species in the sample:

[0024] ① Alkaline extraction method: Weigh 0.2 g of the 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.

[0025] The above alkali extraction method cannot quantitatively extract divalent inorganic mercury in the sample. To extract the divalent inorganic mercury in the sample, the following acid extraction method can be used.

[0026] ②Ac...

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Abstract

The invention discloses an efficient liquid chromatogram-atomic fluorescence spectrum method for measuring mercury forms, and belongs to environment analysis technology. The efficient liquid chromatogram-flame atomization-atomic fluorescence spectrum-based method for measuring the mercury forms of methyl mercury, bivalent inorganic mercury, ethyl mercury and the like comprises that: after multiple mercury forms are separated by efficient liquid chromatogram, the mercury is mixed with acid and hydroboron in turn, the organic mercury is converted into hydrogenated organic mercury, the hydrogenated organic mercury is subjected to gas-liquid separation, mercury atoms are further converted in the argon-hydrogen flame, and the mercury is measured by adopting an atomic fluorescence spectroscope. A device for implementing the method comprises a liquid chromatogram pump, a chromatogram column, a peristaltic pump, a three-way valve, a gas-liquid separator, a flame atomizer, the atomic fluorescence spectroscope and a polytetrafluoroethylene tube. The method does not need to use strong oxidant such as potassium sulfate and the like after column treatment or use degradation equipment of ultraviolet, microwave and the like, has the advantages of simple instruments, convenience for operation and environment friendliness, and is suitable for form analysis of the mercury in environments and biological samples.

Description

technical field [0001] The invention relates to the technical field of environmental analytical chemistry, and relates to a high-performance liquid chromatography-atomic fluorescence spectrometry method for determining the form of mercury. Background technique [0002] As a toxic element, mercury exists widely in various environmental media and food, which brings great risks to the ecological environment and human health. The toxicity, migration and geochemical behavior of mercury are closely related to its form. In the environment, inorganic mercury can be converted to the more toxic methylmercury through biomethylation or chemical methylation. In recent years, there have been reports of the discovery of ethylmercury in the actual environment. Therefore, the speciation analysis of mercury is very important to evaluate the toxicity and environmental chemical behavior of mercury in the environment. The combination of high performance liquid chromatography, gas chromatograp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/68
Inventor 阴永光王振华刘景富何滨江桂斌
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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