Method for measuring content of trace chlorine in high pure, ultra pure ammonia

A technology of ultra-pure ammonia and chlorine content, which is applied in the direction of chemical analysis by titration, which can solve the problems of cumbersome operation and poor repeatability, and achieve the effects of high measurement accuracy, fast analysis speed and simple operation

Inactive Publication Date: 2012-11-28
SUZHOU JINHONG GAS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The current testing methods mainly include UV spectrophotometer method, turbidimetric method or ICP-MS method. However, the operation of these methods is very cumbersome and the repeatability is poor.

Method used

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  • Method for measuring content of trace chlorine in high pure, ultra pure ammonia
  • Method for measuring content of trace chlorine in high pure, ultra pure ammonia

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Embodiment Construction

[0014] 1. Reagents

[0015] (1) Primary distilled water or high-purity water;

[0016] (2) Glacial acetic acid;

[0017] (3) Potassium iodide;

[0018] (4) Sodium azide;

[0019] (5) Iodine: Use 20-40 mesh particles to prepare reference electrodes;

[0020] (6) Isooctane (chlorine-free);

[0021] (7) Dimethyl dichloroether (for preparing standard samples);

[0022] (8) Electrolyte: Dissolve 0.5g of potassium iodide and 0.6g of sodium azide in 1000ml of 0.5% acetic acid aqueous solution, put it in a brown bottle, and put it in a dark and ventilated place for later use; the validity period is two weeks.

[0023] 2. Instruments and equipment

[0024] RPA-200A Micro Coulomb Analyzer Jiangsu Jianghuan Analytical Instrument Co., Ltd.

[0025] 3. Fundamentals

[0026] The sample is injected into the cracking tube, mixed with oxygen and burned, and the organic chlorine in the sample is converted into chloride ion, which is carried into the titration cell by the carrier gas and...

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Abstract

The invention relates to a method for measuring content of trace chlorine in high pure, ultra pure ammonia, comprising the following steps: quantitatively feeding high pure, ultra pure ammonia samples into a crack tube from a silicon rubber separator by a microliter injector, vaporizing the samples and entering the cracking tube together with a carrier gas, mixing with oxygen, burning the oxygen-mixed samples to convert organic chlorine into chloride ions, adding the burnt samples into a titration cell, thus the chloride ion reacts with silver ion and the amount of the consumed silver ion is electrolytically supplemented by a coulometer, and the electric amount required by electrolytic generation of the silver ion is the content of the chlorine injected into the samples. The electric amount for electrolysis is measured by a computer and the content of the chlorine in the high pure and ultra pure ammonia samples is calculated according to Faraday's law of electrolysis. The method is used for measuring the content of the chlorine in the high pure, ultra pure ammonia and has advantages of simple operation, no need of special process of the samples, quick analysis speed, high measurement precision and low detection limit of the method.

Description

technical field [0001] The invention relates to a method for detecting impurities in gas, in particular to a method for detecting trace chlorine content in ammonia gas. Background technique [0002] Electronic grade ultra-pure ammonia is a very important new optoelectronic material, and it is also an important basic material for GaN prepared by MOCVD technology. It is widely used in the manufacture of light-emitting diodes (LEDs), flat panel displays (FPDs), semiconductors and polysilicon solar cells. Especially during the growth of LED chips, ultra-high-purity ammonia is used in the epitaxial growth process of metal organic compound chemical vapor deposition (MOCVD), and it is combined with the precursor of metal organic compounds, trimethylgallium (Ga(CH3)3) A chemical reaction occurs under high temperature and pressure to form gallium nitride: [0003] Ga(CH3)3(g)+NH3(g)→GaN(s)+3CH4(g) [0004] Therefore, the higher the purity of the ammonia used, the lower the power c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N31/16
Inventor 金向华王磊王海
Owner SUZHOU JINHONG GAS CO LTD
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