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Decomposition method for analyzing trace impurities of metal organic compounds

A technology for organic compounds and trace impurities, applied in the field of chemical analysis, which can solve problems such as long decomposition reaction time, deviation of analysis results, and complicated hydrogen chloride gas preparation process

Pending Publication Date: 2021-07-06
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of using hydrogen chloride gas to decompose, solves the problem of long decomposition reaction time and different crystals that cannot be completely dissolved, resulting in deviation of analysis results, but the preparation process of hydrogen chloride gas is complicated, and the prepared hydrogen chloride gas may also contain other trace impurities. Analysis of metal organic compound products with a purity greater than 99.99995% (6.5N) is likely to cause deviations in results

Method used

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  • Decomposition method for analyzing trace impurities of metal organic compounds
  • Decomposition method for analyzing trace impurities of metal organic compounds
  • Decomposition method for analyzing trace impurities of metal organic compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Put the dry sampling bottle and quartz dropper that have been accurately weighed into the inert atmosphere operation box. The oxygen content in the inert atmosphere operation box is maintained between 0.3 and 0.6ppm. in the bottle. The total weight of the sampling bottle and the metal-organic compound therein was accurately weighed on an analytical balance, so that the weight of the metal-organic compound in the sampling bottle was 0.1 g. Press as figure 1 The shown structure connects the sampling bottle, the buffer bottle, the absorbing bottle and the drying bottle in sequence. Water is housed in the absorption bottle as an absorbent, and the temperature of the water is maintained at 0°C. The desiccant bottle is filled with color-changing silica gel or calcium oxide desiccant. The buffer bottle is an empty bottle.

[0019] Heat the ultrapure water, and when more and stable water vapor is generated, then pass it into the sampling bottle 2 with a thin catheter, and a...

Embodiment 2

[0035] Put the dry sampling bottle and stainless steel sampling spoon that have been accurately weighed into an inert atmosphere operation box. The oxygen content in the inert atmosphere operation box is maintained between 0.3 and 0.6ppm. Use a stainless steel sampling spoon to take 0.1 g in the sampling bottle. The total weight of the sampling bottle and the metal-organic compound therein was accurately weighed on an analytical balance, so that the weight of the metal-organic compound in the sampling bottle was 0.1 g. Press as figure 1 The shown structure connects the sampling bottle, the buffer bottle, the absorbing bottle and the drying bottle in sequence. Wherein the absorption bottle is equipped with water as an absorbent, and the temperature of the water is kept at 20±5°C. The desiccant bottle is filled with color-changing silica gel or calcium oxide desiccant. The buffer bottle is an empty bottle.

[0036] Heat the ultrapure water, and when more and stable water vap...

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Abstract

The invention discloses a decomposition method for analyzing trace impurities of a metal organic compound, which comprises the following steps of feeding a dry sampling bottle and a sampling device which are accurately weighed into an inert atmosphere operation box, taking the metal organic compound by using the sampling device, and putting the metal organic compound into the sampling bottle, accurately weighing a sampling bottle and the total weight of the metal organic compounds in the sampling bottle, then sequentially connecting the sampling bottle, a buffer bottle, an absorption bottle and a drying bottle in the inert atmosphere operation box, slowly introducing ultrapure water into the sampling bottle in the form of water vapor, and after complete decomposition, preparing a corresponding to-be-detected solution by absorbing a nitric acid or hydrochloric acid solution with the mass percentage of 5% for substance in the bottle and detecting. The water vapor is adopted to decompose the metal organic source to form the soluble hydroxide, and the method has the advantages of easiness in operation, good safety, short detection time, no environmental pollution, good analysis result repeatability, wide applicability and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to a decomposition method for analyzing trace impurities of metal organic compounds. Background technique [0002] Metal-organic compound is a very important raw material for epitaxial growth. Its chemical properties are very active, and it explodes when it meets water and burns when it meets oxygen. Therefore, it must be decomposed into mild inorganic substances in a specific atmosphere before they can enter the instrument for the determination of impurity elements. Take trimethylaluminum as an example: trimethylaluminum spontaneously ignites when it encounters air, and completely reacts to form aluminum oxide, carbon dioxide and water, etc.: [0003] 2(CH 3 ) 3 Al+12O 2 =Al 2 O 3 (α, β, γ)+9H 2 O+6CO 2 ; [0004] Trimethylaluminum reacts violently with liquid water and releases flammable gas. When it meets oxygen, it can cause combustion and explosion. It reacts...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N27/62
CPCG01N1/28G01N27/62
Inventor 雷志伟廖维林谢贤清芮培欣刘德永胡石金
Owner JIANGXI NORMAL UNIV
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