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Mercury vapour generation method and device

A generating device and mercury vapor technology, which is applied in the field of mercury vapor generation by liquid cathode discharge, can solve the problems of hindering the reduction reaction, failing to realize the reduction of organic mercury, and not being able to use flow injection analysis, so as to achieve small matrix interference and save energy. Effects of analysis steps and time, reduction of reagent loss and contamination

Inactive Publication Date: 2009-10-14
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A disadvantage of this method is that the oxidizing agent (MnO 4 - , Cr 2 o 7 2- ) can hinder the occurrence of reduction reaction, even if the concentration of oxidant in the sample is very low, it can significantly inhibit the reduction of Hg
In addition, this method is only suitable for batch operation and cannot be used for flow injection analysis, nor can the reduction of organic mercury be achieved by this method

Method used

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Embodiment 1

[0023] A tungsten rod is selected as the metal anode, and the diameter of the discharge end is 1 mm. The cathode material is platinum wire. The distance between the tungsten electrode and the capillary is 1 mm, and the inner diameter of the capillary is 0.1 mm. First, the electrolyte solution is introduced into the discharge device through the capillary until the electrolyte liquid level is even with the tip of the capillary. Then the nitric acid of the mercury-containing sample with a pH value of 1 was introduced into the discharge device through the capillary at a flow rate of 0.5 ml / min. The power supply is 700V, and the discharge current is 50mA. The carrier gas is argon, and the flow rate is 400mL / min. The signal is detected by atomic emission, and the signal changes linearly with the sample concentration. figure 2 The flow injection-liquid cathodic discharge mercury vapor generation-atomic emission signal diagram for the determination of 100ng / mL Hg(II) of mercury is...

Embodiment 2

[0025] A titanium rod is selected as the metal anode, and the diameter of the discharge end is 3mm. The cathode material is graphite. The distance between the titanium electrode and the capillary is 4 mm, and the inner diameter of the capillary is 5 mm. First, the electrolyte solution is introduced into the discharge device through the capillary until the electrolyte liquid level is 2mm away from the tip of the capillary. Then, the sulfuric acid of the mercury-containing sample with a pH value of 3 is introduced into the discharge device through the capillary at a flow rate of 10ml / min, the power supply is 2000V, and the discharge current is 150mA. The carrier gas is air with a flow rate of 3000 mL / min. The signal is detected by atomic absorption, and the signal varies linearly with the methylmercury sample concentration.

Embodiment 3

[0027] Platinum is selected as the metal anode, and the diameter of the discharge end is 0.2 mm. The cathode material is stainless steel. The distance between the platinum electrode and the capillary is 2 mm, and the inner diameter of the capillary is 2 mm. First, the electrolyte solution is introduced into the discharge device through the capillary until the electrolyte liquid level is 1mm away from the tip of the capillary, and then the formic acid of the mercury-containing sample with a pH value of 2 is introduced into the discharge device through the capillary at a flow rate of 2ml / min, and the power supply is 200V. The discharge current is 10mA. Helium was used as carrier gas with a flow rate of 30 mL / min. The signal is detected by atomic fluorescence, and the signal varies linearly with the concentration of ethylmercury sample.

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Abstract

The invention discloses a mercury vapour generation method and a device; the method realizes the generation of mercury in liquid sample in vapour form by the discharge of liquid cathode, comprising the following steps: first putting an anode and a cathode connected with two electrodes of a direct current power supply in a sealed discharging device, leading electrolyte solution of the sample containing mercury in the discharging device by a capillary, generating the discharging between the anode and the liquid sample on the sharp end of the capillary so as to generate the mercury vapour. The invention also provides a mercury vapour generation device, comprising the anode and the cathode connected with the two electrodes of the direct current power supply, wherein the anode and the cathode are placed in the discharging device; the discharging device is provided with the capillary with inner diameter of 01-5mm; the sample containing mercury is led in the discharging device by the capillary; the distance between the opening of the capillary and the anode is 1-4mm. The invention realizes the vapour generation of mercury by discharging without any reducing agent so as to reduce the reagent wastage and pollution danger.

Description

technical field [0001] The invention relates to a method and device for generating mercury vapor, in particular to a method and device for generating mercury vapor through liquid cathode discharge, and belongs to the technical field of analytical chemical vapor generating methods. Background technique [0002] Mercury is a global pollutant, and people pay great attention to the monitoring and determination of mercury. Cold vapor generation technology (CVG) can significantly improve the efficiency of sample introduction and realize the separation of samples and substrates. Cold vapor generation-atomic spectroscopy (CVG-AAS, CVG-AFS) is currently the most common method for detecting trace mercury. The usual method of cold steam generation is to use a reducing agent (such as NaBH 4 or SnCl 2 ) to reduce Hg(II) in the liquid to Hg 0 . This reduction method is highly efficient, and it is easy to realize batch or continuous operation, so it is widely used. SnCl is used in the...

Claims

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Application Information

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IPC IPC(8): G01N21/62G01N21/31G01N27/62G01N21/64
CPCG01N21/67G01N21/69
Inventor 朱振利
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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