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Mercury morphological analysis method based on liquid cathode discharge and mercury vapor generating device

A liquid cathode and morphological analysis technology, applied in the direction of electric excitation analysis, material analysis by electromagnetic means, material analysis, etc., can solve the problems of complex instruments and devices, and achieve the effects of small equipment size, low energy consumption, and simple operation

Inactive Publication Date: 2011-04-27
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The development of ultraviolet oxidation technology can oxidize organic mercury to inorganic mercury without the addition of oxidants, but it makes the equipment more complicated

Method used

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  • Mercury morphological analysis method based on liquid cathode discharge and mercury vapor generating device
  • Mercury morphological analysis method based on liquid cathode discharge and mercury vapor generating device
  • Mercury morphological analysis method based on liquid cathode discharge and mercury vapor generating device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A tungsten rod is selected as the anode, and a platinum wire is selected as the cathode material. The discharge distance between the anode and the sampling capillary is 2.0mm, the inner diameter of the sampling capillary is 0.18mm, the discharge medium is nitric acid, the pH value is 1.3, and the flow rate of the discharge medium is 1.5ml / min. The voltage of the DC power supply is 1000V, and the discharge current is 55mA. The carrier gas is argon with a flow rate of 400ml / min. The liquid chromatographic column is ZORBAX SB-C18 post (2.1 * 50mm, 5 μ m), the ammonium acetate+0.1% (v / v) mercaptoethanol of liquid chromatographic mobile phase is 0.06mol / l, and mobile phase flow rate is 0.4ml / min . The three mercury signals were detected by atomic fluorescence. It was found that the detection signal varied linearly with the sample concentration. image 3 For adopting the method of the present invention to measure the standard spectrogram of methylmercury, ethylmercury, in...

Embodiment 2

[0028]A titanium rod is selected as the anode, and graphite is selected as the cathode material. The discharge distance between the anode and the sampling capillary is 0.5mm, the inner diameter of the sampling capillary is 0.1mm, the discharge medium is sulfuric acid, the pH value is 2.0, and the flow rate of the discharge medium is 1.0ml / min. The voltage of the DC power supply is 500V, and the discharge current is 20mA. The carrier gas is air with a flow rate of 200ml / min. The liquid chromatography column is a Dikma-C18 column (4.6×150mm, 5 μm), and the liquid chromatography mobile phase is: 5% (v / v) acetonitrile+0.462% (m / v) ammonium acetate+0.12% (m / v) Cysteine, the mobile phase flow rate is 1.0ml / min. Atomic fluorescence was used to detect three mercury signals in cuttlefish samples, and the signals varied linearly with different sample concentrations.

Embodiment 3

[0030] Platinum-titanium alloy is selected as the anode, and stainless steel is selected as the cathode material. The discharge distance between the anode and the sampling capillary is 2mm, the internal diameter of the sampling capillary is 0.3mm, and the discharge medium is phosphoric acid+0.1% (v / v) formic acid (here is the volume percent concentration of formic acid in the discharge medium is 0.1%), the pH value is 2.5, and the flow rate of the discharge medium is 2ml / min. The voltage of the DC power supply is 1200V, and the discharge current is 90mA. The carrier gas is helium, and the flow rate is 800ml / min. The liquid chromatography column is a CLC-ODS C18 column (150×6mm, 10μm), and the mobile phase is 50% (v / v) methanol+10mmol l -1 Tetrabutylammonium bromide+0.1mol l -1 Sodium chloride, the mobile phase flow rate is 1.2ml / min. Atomic fluorescence was used to detect three mercury signals in tuna samples, and the signals varied linearly with different sample concentra...

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Abstract

The invention discloses a mercury morphological analysis method based on liquid cathode discharge and a mercury vapor generating device. The method comprises: a mercury-containing sample solution is introduced into a chromatographic column of a liquid chromatograph; a discharge medium carrier flow passes through a sample introduction device and is introduced into a sample introduction capillary tube of a discharge pool with the effluence of the chromatographic column through a tee joint; by taking a metal electrode as an anode, and graphite, platinum or a stainless steel material as a cathode, liquid cathode discharging is carried out to generate vapor which is carried by a carrier gas into a gas-liquid separator; and finally the separated gas is detected by an atomic fluorescence spectrometer to obtain the morphology of mercury. Through the method provided by the invention, organic mercury and inorganic mercury in an object to be detected are effectively separated and detected; and the method has the advantages of small volume, low energy consumption, high mercury vapor generation efficiency and low matrix interference, is simple in operation and can be used for analyzing the morphology of mercury in a biological sample.

Description

technical field [0001] The invention relates to a mercury speciation analysis method based on liquid cathode discharge and a mercury vapor generating device, belonging to the field of analytical chemical speciation analysis. Background technique [0002] The speciation analysis method of mercury is generally realized by the combined method. It first uses chromatography to achieve the separation of the different mercury species, followed by detection using sensitive element-selective detectors. Among them, the combination of high performance liquid chromatography and atomic spectroscopy, especially atomic fluorescence, is a common mercury speciation analysis method, because atomic fluorescence has the advantages of good selectivity and high sensitivity. The principle is: after atomic fluorescence detection, each fluorescent peak represents a form of mercury, that is, different forms of mercury correspond to different retention times, and the retention times of the three merc...

Claims

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Application Information

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IPC IPC(8): G01N27/68G01N21/64G01N30/02
CPCG01N21/67G01N21/6404G01N21/69
Inventor 朱振利何倩
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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