Detection of different mercury forms in environmental water body based on HPLC-ICP-MS coupling technology

A technology of HPLC-ICP-MS and ICP-MS, which is applied in the field of water quality environmental monitoring, can solve problems such as not meeting the measurement requirements, and achieve the effects of excellent peak shape, reduced impact, and short separation time

Active Publication Date: 2019-09-27
河北省地质环境监测院
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

For environmental water samples, the above detectio

Method used

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  • Detection of different mercury forms in environmental water body based on HPLC-ICP-MS coupling technology
  • Detection of different mercury forms in environmental water body based on HPLC-ICP-MS coupling technology
  • Detection of different mercury forms in environmental water body based on HPLC-ICP-MS coupling technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: Optimization of liquid chromatography separation conditions

[0036] When using HPLC-ICP-MS to analyze mercury species in samples, the selection and optimization of liquid chromatographic separation conditions are very critical. The present invention is from following four aspects to four kinds of mercury forms (Hg 2+ , methylmercury, ethylmercury, phenylmercury) were investigated.

[0037] 1.1 Selection of chromatographic column

[0038] The four forms of mercury are all positively charged, represented by Hg 2+ , MeHg + , EtHg + and PhHg + Form exists, the present invention adopts ZORBAX SCX strong cation exchange column to carry out the separation of the cation of mercury of four forms under acidic conditions. In the presence of L-cysteine, [Cys-Hg-Cys] is formed 2+ , MeHg-Cys + , EtHg-Cys + and PhHg-Cys + Ionic groups interact with strong cation exchange columns to achieve baseline separation, and the order of peaks is MeHg + , EtHg + 、PhHg +...

Embodiment 2

[0046] Example 2: Research on Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Analytical Conditions

[0047] The present invention chooses 202 The debugging solution with Hg concentration of 10ppb is used for experiments on conditions such as the power of the instrument plasma radio frequency generator (RF), carrier gas flow, sampling depth, and auxiliary gas flow; the measurement process simultaneously monitors the mass number of double charge and the mass number of oxides 70 and 156. Calculate the double ion yield and oxide yield.

[0048] 2.1 Effect of plasma RF power

[0049] When the plasma RF power was changed, the intensity count of the element to be detected was detected, and the measured data are shown in Table 1. And take the RF power as the abscissa, the left side takes the intensity of mercury as the ordinate, and the right side takes the double charge of Ce and the oxide yield as the ordinate for the plotting see image 3 . The graph shows that with the ...

Embodiment 3

[0064] Example 3: Indicator Confirmation of HPLC-ICP-MS Determination of Different Forms of Mercury

[0065] 3.1 Detection limit and linear range of mercury-linked method

[0066] Prepare a blank sample and add a small amount of standard water sample to be tested for analysis, measure 7 times continuously, and calculate the method detection limit (MDL=3.143δ) according to 3 times the relative standard deviation of the measurement result, the specific data is shown in Table 5.

[0067] Table 5 Detection limit data of four different forms of mercury

[0068]

[0069] The detection limits (in Hg) of the four different forms of mercury are in order: Hg 2+ , 0.03μg / L; MeHg + , 0.06μg / L; EtHg + , 0.04μg / L; PhHg + , 0.05μg / L, according to the US EPA SW-846 regulations 4 times the detection limit concentration as the lower limit of determination, the lower limit of determination is: Hg 2+ , 0.2μg / L; MeHg + , 0.3μg / L; EtHg + , 0.2μg / L; PhHg + , 0.2 μg / L.

[0070] Prepare mi...

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Abstract

The invention provides a method for detecting different mercury forms in an environmental water body based on HPLC-ICP-MS coupling. The method comprises the concretely steps of: (1) preparation of a mixed standard solution: preparing a mercury mixed standard solution by taking a mobile phase L-cysteine as a solvent; (2) drawing of a standard curve: taking the mixed standard solution prepared in the step (1), determining the concentration of the mercury form by using HPLC-ICP-MS, and drawing a standard curve of the mercury form according to the concentration of the mercury form in the mixed standard solution and the corresponding signal intensity; (3) sample pretreatment: prior to sampling, allowing a water sample to be tested to be filtered by a 0.45 [mu]m filter membrane, adding a KOH solution, storing the water sample at a low temperature of 4 DEG C after sampling, during an experiment, measuring the sample to be tested, putting the sample to be tested into a centrifuge tube, adding a mobile phase as a solution of the sample to be tested, and performing a blank test; and (4) sample detection: determining and analyzing the concentration of the mercury form in the solution of the sample to be tested by using HPLC-ICP-MS, and calculating and analyzing the concentration value of the mercury form in the sample to be tested according to the relative standard deviation RSD of the calculated signal intensity and the respective standard curve of the mercury form.

Description

technical field [0001] The invention relates to a detection method for different mercury forms in environmental water, in particular to a detection method for different mercury forms in environmental water based on HPLC-ICP-MS, and belongs to the field of water quality environmental monitoring. Background technique [0002] Poor water environment quality, severely damaged water ecology, and many environmental hazards are very prominent in some areas of our country, which affect and damage the health of the people and are not conducive to sustainable economic and social development. With the development of environmental science, biomedicine and other disciplines, many scholars have realized that the bioavailability, toxicity and chemical activity and remigration of heavy metals in the environment are not only related to the total amount of heavy metals, but also to a greater extent. Determined by its form, different forms produce different environmental effects. Specific ele...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 董会军侯军亮董建芳李义赵峰赵俊梅刘亚平刘璐李梓瑶毕海超董琳琳赵雄英
Owner 河北省地质环境监测院
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