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Rapid determination method for mercury form in water

A rapid determination and speciation technology, which is applied in the direction of testing water, measuring devices, and preparation of test samples, can solve the problems of inability to accurately reflect mercury pollution in water bodies in real time, rapid on-site analysis of mercury speciation, and inability to achieve separation and determination, etc. problem, to achieve the effect of simple and quick pre-processing steps, low cost, and simple and convenient method

Pending Publication Date: 2022-03-25
INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the speciation analysis of mercury in water quality is mainly through the separation of various forms of mercury by high performance liquid chromatography (HPLC), and then the determination of different forms of mercury by serial detection instruments such as inductively coupled plasma mass spectrometry (ICP-MS) or atomic fluorescence spectrometer (AFS) content, the above method has high sensitivity and good accuracy, but there are disadvantages such as high operating cost and long detection time
Moreover, due to the need to use large precision instruments and equipment, the above method is only suitable for laboratory analysis, and cannot be applied to rapid on-site analysis of mercury species.
Therefore, the timeliness of this type of analysis method is often limited by time and space, so that the test results are not direct on-site data, and cannot accurately reflect the mercury pollution in water in real time.
The direct sample injection method of thermal desorption can realize the rapid analysis of mercury with high sensitivity. It has the advantages of low memory effect, low cost, small instrument size and strong portability. It can meet the rapid determination of mercury in the laboratory and field. A single instrument can only realize the detection of total mercury, but cannot realize the separation and determination of different mercury forms

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  • Rapid determination method for mercury form in water
  • Rapid determination method for mercury form in water
  • Rapid determination method for mercury form in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] After rinsing the wooden stick with methanol and water, soak the tip of the wooden stick in 0.2mmol / L HAuCl 4 solution for 10 minutes, and then naturally air-dried, the obtained material is the gold-loaded solid-phase extraction probe.

[0043] Take 3 headspace sampling vials, add 2mL of methylmercury (MeHg) solution with a concentration of 5μg / L, 2mL of ethylmercury (EtHg) solution with a concentration of 5μg / L, and 2mL of mercury ions with a concentration of 5μg / L Hg 2+ (inorganic mercury) solution, add 1 mL of 12% SnCl in each headspace vial 2 solution, and then add 1 mL of reduction inhibitor, the reduction inhibitor is V with a mass ratio of 1:1 5+ and Pb 2+ The mixed solution of the reduction inhibitor was 100 mg / L, and then the gold-loaded solid-phase extraction probe was inserted into the headspace sampling vial, and the adsorption was oscillating at a speed of 270 rpm for 25 minutes to enrich the elemental mercury. The experiment was repeated three times. ....

Embodiment 2

[0052] After rinsing the wooden stick with methanol and water, soak the tip of the wooden stick in 0.2mmol / L HAuCl 4 solution for 10 minutes, and then naturally air-dried, the obtained material is the gold-loaded solid-phase extraction probe.

[0053] Take 5 headspace sampling vials, add 2 mL of methylmercury (MeHg) solution with a concentration of 5 μg / L and 2 mL of ethylmercury (EtHg) solution with a concentration of 5 μg / L respectively, and then add Add 1 mL of SnCl with a mass fraction of 12% 2 The mass ratio of the solution and the reduction inhibitor is 0.25:1, 0.5:1, 1:1, 2:1, 3:1 V 5+ and Pb 2+ Ion mixed solution, the concentration of reduction inhibitor was 100mg / L, and the experiment was repeated three times. The experimental results are shown in Table 1.

[0054] The reduction inhibitors of different mass ratios of table 1 influence on the determination of organic mercury (n=3)

[0055]

[0056] It can be concluded from Table 1 that V mixed with different ma...

Embodiment 3

[0058] A kind of rapid determination method of mercury form in water quality, comprises the following steps:

[0059] S1. After washing the wooden stick with methanol and water, soak the tip of the wooden stick in 0.2mmol / L HAuCl 4 solution for 10 minutes, and then naturally air-dried, the obtained material is the gold-loaded solid-phase extraction probe.

[0060] S2, add 1mL mass fraction to the sample of 2mL and be 12% tin protochloride solution, the inorganic mercury and organic mercury in the sample are all reduced to the mercury simple substance of zero valence state, and adopt the gold-loaded solid phase prepared in step S1 The extraction probe was used to enrich the elemental mercury, the enrichment conditions were shaking speed 270rpm, and the enrichment time was 25min.

[0061] refer to figure 1 , the organic mercury (methylmercury 21 and ethylmercury 22) and inorganic mercury 23 (mercury ions) in the water sample are all reduced to zero-valent mercury element 24 un...

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Abstract

The invention discloses a rapid determination method for mercury form in water. The determination method comprises the following steps: S1, preparing a solid-phase extraction probe; s2, adding a stannous chloride solution into a sample to be detected, reducing inorganic mercury and organic mercury in the sample into zero-valence mercury elementary substances, and enriching the mercury elementary substances by adopting the solid-phase extraction probe prepared in the step S1; s3, measuring the total mercury concentration CTHg enriched in the solid-phase extraction probe; s4, taking another same sample to be detected, adding a stannous chloride solution and a reduction inhibitor into the sample, and enriching the elemental mercury by adopting the solid-phase extraction probe prepared in the step S1; s5, measuring the concentration CiHg of inorganic mercury enriched in the solid-phase extraction probe in the step S4; and S6, calculating the organic mercury concentration COHg = CTHg-CiHg in the sample. The method established by the invention is good in accuracy, high in sensitivity, low in cost, simple and rapid in pretreatment step, and capable of realizing rapid separation and enrichment of mercury forms in water without complex sample pretreatment and long-time chromatographic separation process.

Description

technical field [0001] The invention belongs to the technical field of water quality pollutant form analysis and detection, and in particular relates to a rapid determination method for mercury form in water quality. Background technique [0002] In 2020, my country's mercury production will be about 2,000 tons, accounting for about 50% of global mercury production, and atmospheric mercury emissions will account for about 33% of global emissions, making it the world's largest mercury producer and emitter. With the extensive use of mercury-containing products and the discharge and deposition of mercury-containing wastewater and waste gas, the environmental pollution risk of mercury in the water environment has increased significantly. Mercury is a highly toxic pollutant. Long-term exposure to mercury-polluted environments will cause irreversible damage to the central nervous system, digestive system, kidneys and other organs of the human body. Among them, organic mercury (suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N33/18G01N1/34G01N1/40
CPCG01N33/18G01N1/34G01N1/40G01N1/4044
Inventor 梁维新吴锐郭鹏然雷永乾赵健
Owner INST OF ANALYSIS GUANGDONG ACAD OF SCI (CHINA NAT ANALYTICAL
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