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Pyrolysis-chemical vapor generation sampling device and analysis method for element determination

A technology of a vapor generation and sample injection device, which is applied in the field of instrument analysis, can solve problems such as production stoppage detection tasks, contamination and scarring, and complicated devices, and achieves the effects of ensuring precision and accuracy, low maintenance costs, and simple and practical devices.

Inactive Publication Date: 2016-11-02
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] (1) The sample container of the device is directly placed in the heating chamber, so that the sample is prone to sputtering during rapid heating and cracking. Although this setting does not affect the measurement results in a short period of time, the number of measured samples is large Therefore, the furnace cavity is easily polluted, which will cause contamination and scarring, resulting in poor measurement accuracy and accuracy; in addition, frequent disassembly of the liner to clean the furnace cavity will not only cause production stoppages and interrupt normal testing tasks, but also cause serious problems. The possibility of damage to the furnace chamber increases the replacement of the furnace chamber; (2) The device includes a condensation device and a fine particle dust removal device, which makes the device too complicated and is not conducive to the determination of samples that are aqueous solutions and the volume of the solution is relatively small Rapid determination

Method used

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  • Pyrolysis-chemical vapor generation sampling device and analysis method for element determination
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  • Pyrolysis-chemical vapor generation sampling device and analysis method for element determination

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Effect test

Embodiment 1

[0049] Elemental determinations are performed using the first preferred embodiment device. Accurately draw 0.1 ml of water sample into a small glass beaker, then add 0.05 ml of 10% sodium formate and 0.05 ml of 10% thiourea to the water sample. Then place the small beaker on the platform of the support frame, put the liner on, quickly put the sample and the liner into the heating chamber that has been heated to 500°C for pyrolysis, and carry out the pyrolysis under the flow rate of carrier gas (argon) at 300 ml / Under the condition of 10 minutes, the element volatiles produced by pyrolysis are directly sent to the atomic fluorescence instrument for detection without condensation and other purification devices (the atomic fluorescence atomizer and a hydrogen vapor generator generate 250 ml / min of hydrogen vapor generator to provide a source of hydrogen for proper ignition of the atomizer). The content of arsenic, mercury, antimony, and bismuth in water was determined by the ex...

Embodiment 2

[0051] Elemental determinations are performed using a second preferred embodiment. Accurately draw 0.1 ml of gold-containing sample solution into a small glass beaker, and then add 0.05 ml of 15% sodium borohydride aqueous solution to the water sample. Then place the small beaker on the platform of the support frame, put the liner on, quickly put the sample and the liner into the heating chamber that has been heated to 600°C for pyrolysis, and carry out the pyrolysis at the flow rate of the carrier gas (argon) at 250 ml / Under the condition of 10 minutes, the elemental volatiles produced by pyrolysis were sent to the electrothermal quartz tube atomic absorption spectrophotometer to be detected. The gold content in the sample solution was determined by the external standard method, and the measured results were in good agreement with the ICP-AES method.

Embodiment 3

[0053] Elemental determinations are performed using a third preferred embodiment. Accurately draw 0.1 ml of zinc and cadmium sample solution into a 25 ml test tube, and then add 0.05 ml of 15% hydrogen iodide aqueous solution to the water sample. Then place the small beaker on the platform of the support frame, put the liner on, quickly put the sample and the liner into the heating chamber that has been heated to 600°C for pyrolysis, and carry out the pyrolysis at the flow rate of the carrier gas (argon) at 250 ml / Under the condition of 10 minutes, the elemental volatiles produced by pyrolysis were sent to the electrothermal quartz tube atomic absorption spectrophotometer to be detected. The gold content in the sample solution was determined by the external standard method, and the measured results were in good agreement with the ICP-MS method.

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Abstract

The invention discloses a cracking-chemical steam generation sample-introduction apparatus for element determination and an analysis sample-introduction method for elements in a water solution. The apparatus comprises that a movable liner is arranged in a fixed heating chamber, and the liner is capable of completely covering a sample container and enabling a sputtering product to only be sputtered to the side wall of the movable liner without polluting a furnace chamber when a cracking reaction happens. The invention also discloses the determination method for elements in the water solution. The determination method comprises that under the condition of relatively small solution volume, the cracking-chemical steam generation process is used for determining elements in the water solution, and after being processed by using the cracking-chemical steam generation process, the solution is directly connected with the apparatus for element determination without performing condensation water removal and other purification steps. Compared with the prior art, the apparatus and the method have the characteristics of being relatively clean, convenient and practicable, the apparatus is simplified, pollution of the cracking product to the furnace chamber is eliminated, also determination precision and accuracy are improved, and the practicality is relatively high.

Description

technical field [0001] The invention belongs to the technical field of instrument analysis, and in particular relates to a cracking-chemical vapor generation sampling device for element determination and an element analysis method in aqueous solution. Background technique [0002] Recently, an invention patent proposed by the present inventor, which utilizes the hydrogen produced during the cracking of organic matter to directly react with some elements in the sample to form elemental volatiles for elemental determination, has been reported (CN103411892A). However, there are deficiencies in the thermal cracking device used in this patent, which are mainly reflected in: [0003] (1) The sample container of the device is directly placed in the heating chamber, so that the sample is prone to sputtering during rapid heating and cracking. Although this setting does not affect the measurement results in a short period of time, the number of measured samples is large Therefore, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N21/25G01N21/64
Inventor 段旭川
Owner TIANJIN NORMAL UNIVERSITY