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Method for detecting methyl mercury, ethyl mercury and inorganic mercury in water of aquaculture pond

A technology for cultivating pond water and methyl mercury, which is applied in the fields of extraction and detection of ethyl mercury and inorganic mercury, methyl mercury in cultivating pond water, and detection of methyl mercury, ethyl mercury and inorganic mercury in cultivating pond water, and can solve the problem. Interference, insufficient method sensitivity, complex sample matrix, etc., to achieve the effect of strong anti-interference ability, outstanding matrix separation ability, and accurate analysis

Active Publication Date: 2016-05-11
四川威尔检测技术股份有限公司 +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for detecting methylmercury, ethylmercury and inorganic mercury in water in aquaculture ponds. This method innovatively applies vortex-assisted micro-extraction technology to the pretreatment of samples in water samples in aquaculture ponds, overcoming the Complex sample matrix, serious interference, insufficient sensitivity of the method, etc., the sample is pretreated and then tested with the HPLC-CVAFS system, which can meet the requirements of simple operation, fast, low cost, environmental protection and high efficiency, high enrichment efficiency, outstanding anti-interference ability, etc. Advantages, suitable for speciation analysis of trace mercury in aquaculture pond water samples

Method used

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  • Method for detecting methyl mercury, ethyl mercury and inorganic mercury in water of aquaculture pond
  • Method for detecting methyl mercury, ethyl mercury and inorganic mercury in water of aquaculture pond
  • Method for detecting methyl mercury, ethyl mercury and inorganic mercury in water of aquaculture pond

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Embodiment 1

[0054] A method for detecting methylmercury, ethylmercury and inorganic mercury in water in a culture pond, comprising the following steps:

[0055] A. Add CH to the sample 2 Cl 2 , after vortex shaking and centrifugation, take the sediment phase and add L-cysteine, then after extraction and centrifugation, transfer the supernatant to prepare the sample to be tested.

[0056] B. After preparing the sample to be tested into a test solution with a concentration of 2 μg / L, use high-performance liquid chromatography-cold vapor generation atomic fluorescence system for detection, and the detection conditions meet:

[0057] Injection volume: 100μL,

[0058] Mobile phase: ammonium acetate of 50mmol / L,

[0059] Mobile phase flow rate: 0.8mL / min,

[0060] Carrier gas: Ar,

[0061] Reducing agent: KBH with a mass volume ratio of 1% 4 and 0.1% NaOH,

[0062] Oxidant: K with a mass volume ratio of 1.5% 2 S 2 o 8 and 0.1% NaOH,

[0063] Carrier liquid: 3% HCl by volume,

[0064...

Embodiment 2

[0067] A method for detecting methylmercury, ethylmercury and inorganic mercury in water in a culture pond, comprising the following steps:

[0068] A. Add CH to the sample 2 Cl 2 , after vortex shaking and centrifugation, take the sediment phase and add L-cysteine, then after extraction and centrifugation, transfer the supernatant to prepare the sample to be tested.

[0069] B. After preparing the sample to be tested into a test solution with a concentration of 20 μg / L, use high performance liquid chromatography-cold vapor generation atomic fluorescence system for detection, and the detection conditions meet:

[0070] Injection volume: 500μL,

[0071] Mobile phase: ammonium acetate of 100mmol / L,

[0072] Mobile phase flow rate: 1.2mL / min,

[0073] Carrier gas: Ar,

[0074] Reductant: KBH with a mass volume ratio of 2.5% 4 and 0.5% NaOH,

[0075] Oxidant: K with a mass volume ratio of 2.5% 2 S 2 o 8 and 0.1-0.5% NaOH,

[0076] Carrier liquid: 7% HCl by volume,

[0...

Embodiment 3

[0080] This embodiment proposes on the basis of embodiment 1, in step A, CH 2 Cl 2 The mass ratio of the added amount of the sample to the sample is 7.7:3.8.

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Abstract

The invention discloses a method for detecting methyl mercury, ethyl mercury and inorganic mercury in water of an aquaculture pond. The method comprises the following steps: adding CH2Cl2 into a sample, carrying out vortex shake and centrifugation, taking out a sedimentary phase, adding L-cysteine into the sedimentary phase, extracting, centrifuging, and then removing supernatant liquid to obtain the sample to be detected; preparing the sample to be detected into 2-20 micrograms / L of liquid to be detected, and then detecting by a high performance liquid chromatography (HPLC)-cold vapor generation atomic fluorescence system. The method adopts a vortex-assisted liquid-liquid microextraction way to carry out pretreatment on the aquaculture pond water sample for the first time, thus solving the problems that the sample matrix is complicated, interference is serious, the method is lack of sensitivity, and the like; HPLC separation and sequential injection-cold vapor generation atomic fluorescence system (SI-CVAFS) sample introduction are utilized, so that the method fills into the blank of analyzing the methyl mercury, the ethyl mercury and the inorganic mercury in water of the aquaculture pond at the same time; the method has the characteristics of being simple and rapid in operation, low in cost, environment-friendly, efficient, high in enrichment efficiency, remarkable in interference resistance, high in precision and accuracy, low in detection limit, and the like.

Description

technical field [0001] The invention relates to a method for detecting methylmercury, ethylmercury and inorganic mercury in aquaculture pond water, specifically relates to the extraction and detection technology of methylmercury, ethylmercury and inorganic mercury in aquaculture pond water, and belongs to the field of heavy metal detection. Background technique [0002] Mercury is highly volatile and highly toxic, can cause harm to the health of the nervous system, and can be enriched in organisms. At present, all countries have included mercury in the blacklist of priority pollutants. However, the toxicity, bioavailability, mobility and re-migration of mercury are closely related to its chemical form. Generally speaking, the toxicity of organic mercury is greater than that of inorganic mercury. Mercury and its compounds can be enriched in organisms and biomagnified through the food chain. Therefore, accurate and efficient analysis of mercury species in aquaculture pond wat...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08G01N2030/027G01N2030/062
Inventor 张凤枰冷庚刘耀敏焦宝玉李林高饶瑾瑜王殷洁
Owner 四川威尔检测技术股份有限公司
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