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Detection method of hydride and special device

A hydride, atomizing gas technology, applied in the preparation of test samples, thermal excitation analysis, material excitation analysis, etc., can solve the problems of high element ionization, low element content, low sensitivity, etc., to achieve broad application value, simplify Experimental procedure, the effect of improving sensitivity

Pending Publication Date: 2018-08-21
INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the hydride elements such as As and Se have always been a difficult problem in ICP-OES testing. The main performance is that the content of these elements is extremely low, which is lower than the detection limit of the instrument, the test intensity is low, and there are also strong interfering elements that affect Accurate determination of these elements, these elements have high ionization energy, are difficult to ionize, have low sensitivity and high detection limit

Method used

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  • Detection method of hydride and special device
  • Detection method of hydride and special device

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Such as figure 1 As shown, the ICP-OES hydride atomization system includes a gas-liquid sampling tube 1, a gas-liquid separation unit 3, a gas center tube 4, an atomized gas inlet tube 5, and a liquid level balance unit 10, wherein the gas-liquid separation unit 3 It communicates with the bottom of the liquid level balance unit 10, and the upper part of the gas-liquid separation unit 3 communicates with the gas-liquid sampling tube 1 and the gas central tube 4, and the end of the gas central tube 4 is accommodated at the nozzle 6 of the atomizing gas inlet tube 5 , One side of the liquid level balance unit 10 is provided with a drain port, and the drain port is connected to the drain pipe 8 .

[0024] Further, the gas-liquid separation unit 3 is provided with a draft tube 2 communicating with the gas-liquid sampling tube 1 . The draft pipe 2 is inclined downwards and has an open structure above. The reacted gas-liquid mixture flows through the gas-liquid sampling pipe...

Embodiment 2

[0031] Determination of As, Sb, Sn elements in soil

[0032] 1. Accurately weigh 100mg of soil sample into a 15ml polytetrafluoroethylene liner;

[0033] 2. Add 2.5ml HF and 0.5ml HCl, pre-digest on a 150°C electric heating plate for 2 hours, open the cover to release the pressure;

[0034] 3. Seal the pre-digested sample and place it in an antiseptic high-efficiency sample dissolution tank;

[0035] 4. Digest in an anti-corrosion electric oven at 180°C for 12 hours and cool down;

[0036] 5. Take out the liner, add 1ml of HCl on a 150°C electric heating plate to catch the acid until it is completely dry;

[0037] 6. Add 1ml HCl and 2ml 18.2MΩ pure water, and digest at 150℃ for 12 hours;

[0038] 7. Cool, take out the liner, add 1ml of 10% thiourea, dilute to 5g (the dilution factor is about 50 times).

[0039] The 1% potassium borohydride introduced through the injection tube reacts with the reducing agent tube to generate hydrogen, which forms hydrides with As, Sb and Sn...

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Abstract

The invention relates to a hydride detection technology, in particular to a detection method of hydride and a special device. The device comprises a gas-liquid sample injection pipe, a gas-liquid separation unit, a gas central pipe, an atomized gas inlet pipe and a liquid level balancing unit, wherein the bottoms of the gas-liquid separation unit and the liquid level balancing unit are communicated, the upper part of the gas-liquid separation unit is communicated with the gas-liquid sample injection pipe and the gas central pipe, the tail end of the gas central pipe is accommodated at a sprayport of the atomized gas inlet pipe, and a liquid drainage port is formed in one side of the liquid level balancing unit. Elements such as Ge, As, Se, Te, Sb, Sn, Hg and the like can be directly measured. According to the method, a hydride atomizer system is used, the experimental procedure is simplified, the sensitivity of the method is improved, the detection limit is reduced, and rapid, simple,efficient and accurate testing of hydride elements is realized with ICP-OES, research and application of combination of ICP-OES and a hydride direct sampling system are opened, and the method and thedevice have very broad application value in the testing industry. Besides, higher reference value is provided for valence analysis of elements.

Description

technical field [0001] The invention relates to the detection technology of hydrides, in particular to a detection method and a special device for hydrides. Background technique [0002] In recent years, with the development of spectral testing and analysis technology, ICP-OES has been widely used, and its routine functions have been brought into full play. Because of its fast testing speed, simple operation, stable and accurate data, etc., it has attracted more and more attention, especially Its extended function development has attracted the attention of analysts. At present, the hydride elements such as As and Se have always been a difficult problem in ICP-OES testing. The main performance is that the content of these elements is extremely low, which is lower than the detection limit of the instrument, the test intensity is low, and there are also strong interfering elements that affect For the accurate determination of these elements, these elements have high ionization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/38G01N1/44
CPCG01N1/38G01N1/44G01N21/73
Inventor 殷学博陈帅王晓媛曾志刚
Owner INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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