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Measuring method of methyl mercury and ethyl mercury

A method of determination, technology of ethylmercury, applied in the field of heavy metal detection, can solve the problems of good market prospect and high adsorption efficiency, achieve good extraction effect, increase adsorption efficiency, and mild reaction conditions

Inactive Publication Date: 2017-05-31
QINGDAO TECHNOLOGICAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The combination of magnetic core and shell of magnetic chitosan microspheres is mainly through hydrogen bonds, van der Waals forces, and coordination bonds. Due to the presence of a large number of amino groups and hydroxyl groups on the surface of magnetic chitosan microspheres, magnetic chitosan exhibits Good adsorption properties, there is no report that magnetic chitosan is used for methylmercury and ethylmercury speciation analysis at present, therefore a kind of methylmercury and ethylmercury determination method are involved, the method utilizes magnetic solid-phase extraction ( MSPE) technology, using thiosemicarbazide-modified magnetic chitosan as magnetic solid-phase extraction material, has high adsorption efficiency for methylmercury and ethylmercury, and has a good market prospect

Method used

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  • Measuring method of methyl mercury and ethyl mercury
  • Measuring method of methyl mercury and ethyl mercury
  • Measuring method of methyl mercury and ethyl mercury

Examples

Experimental program
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Effect test

Embodiment 1

[0061] The concrete steps of methylmercury and ethylmercury determination method that the present embodiment involves are:

[0062] Step 1: Preparation of thiosemicarbazide-modified magnetic chitosan (AT-MCS):

[0063] (1) Dissolve 2.0 g of ferric chloride hexahydrate in 40 mL of ethylene glycol, then add 6 g of sodium acetate trihydrate and 20 ml of ethanolamine, stir and dissolve to prepare a mixed solution for subsequent use;

[0064] (2) The mixed solution prepared in the step (1) was reacted for 8h at 200°C in the solvothermal reactor, and the prepared mixture in the autoclave was washed with ultrapure water to obtain ferric iron tetraoxide ( NH 2 -Fe 3 o 4 ), the prepared NH 2 -Fe 3 o 4 Vacuum dry at 60°C for 12 hours;

[0065] (3) Take 0.05gNH 2 -Fe 3 o 4 Add it to the mixture of 10mL ultrapure water and 1mL glutaraldehyde, and disperse it ultrasonically for 5-8 minutes to prepare the dispersion for later use;

[0066] (4) getting 0.03g chitosan and being dis...

Embodiment 2

[0099] This embodiment measures the residues of methylmercury and ethylmercury in the water at the tip of the tap water pipe network in Qingdao, the surface water of Xiaozhushan Reservoir in Qingdao, and the surface water of Jihongtan Reservoir in Qingdao. 120 μm rapid qualitative filter paper filtration, and then filter with 0.45 μm filter membrane; the filtered water sample is measured by the method described in Example 1, and the accuracy test is carried out by the method described in Example 2, and methylmercury is prepared respectively Carry out standard addition recovery test with the actual water samples with three concentrations of ethylmercury concentrations of 0.12μg / L, 0.4μg / L, and 1.2μg / L. Each concentration point is measured 3 times and calculated 3 times The measured average value, relative standard deviation and recovery rate of standard addition; among them, methylmercury and ethylmercury were not detected in the blanks of the three water samples; the test resul...

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Abstract

The invention belongs to the field of heavy metal detection, and relates to a measuring method of methyl mercury and ethyl mercury. According to the measuring method, chitosan is taken as a raw material to prepare aminothiourea modified magnetic chitosan (AT-MCS), MSPE is adopted, aminothiourea modified magnetic chitosan (AT-MCS) is taken as a solid phase extracting material, high performance liquid chromatography and atomic fluorescen spectrometry method are combined and adopted to measure methyl mercury and ethyl mercury in environmental water samples, and a morphological analysis method of methyl mercury and ethyl mercury in environmental water samples is established. Operation of the measuring method is simple and convenient; analysis time is shortened greatly; analysis cost is reduced greatly; average recovery rate ranges from 83.4 to 106.0%; the relative standard deviation ranges from 1.61 to 9.83%; extraction effect is excellent; analysis results are accurate; reproducibility is high; the raw materials are cheap and easily available; material preparation process is simple; reaction conditions are mild; and the measuring method is friendly to the environment.

Description

[0001] Technical field: [0002] The invention belongs to the technical field of heavy metal detection, and relates to a method for determining the speciation of mercury in water samples, in particular to a method for determining methylmercury and ethylmercury, which utilizes magnetic solid-phase extraction (MSPE) technology and adopts thiosemicarbazide to modify the method. Determination of methylmercury and ethylmercury in environmental water samples by magnetic chitosan solid phase extraction-high performance liquid chromatography-atomic fluorescence method. [0003] Background technique: [0004] Mercury is widely distributed in nature and is considered to be one of the most harmful heavy metal elements to humans and the environment. Common natural forms of mercury are elemental mercury (Hg 0 ), inorganic mercury (Hg + , Hg 2+ ) and organic mercury (methylmercury MeHg, ethylmercury EtHg, phenylmercury PhHg). The content of mercury in the aquatic environment is extremely...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/74G01N21/64G01N30/06G01N30/14
CPCG01N21/6404G01N21/643G01N30/02G01N30/06G01N30/14G01N30/74G01N2021/6406G01N2030/027G01N2030/062G01N2030/067G01N2030/146
Inventor 马继平侯丽玮吴阁格丁明
Owner QINGDAO TECHNOLOGICAL UNIVERSITY
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