Ion method for measuring trace chloride ions in triethyl aluminum

A technology of triethylaluminum and chloride ions is applied in the field of chemical analysis, which can solve the problems of pollution and damage of chromatographic columns and suppressors, and achieve the effects of high sensitivity, solving pollution damage and simple operation.

Active Publication Date: 2017-03-22
中国检验认证集团山东检测有限公司
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Problems solved by technology

Therefore, the establishment of a pretreatment method is simple, easy to repeat, and the method has high sensitivity. At the same time, it solves the problem of heavy metal aluminum pollution and damage to the chromatographic column and suppressor during the determination process, which is of great significance for the determination of trace chloride ions in TEAL.

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  • Ion method for measuring trace chloride ions in triethyl aluminum
  • Ion method for measuring trace chloride ions in triethyl aluminum
  • Ion method for measuring trace chloride ions in triethyl aluminum

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Embodiment Construction

[0057] 1.1 Instruments and reagents

[0058] AnL-IC2600 ion chromatograph (Qingdao Aili Analysis Experimental Technology Co., Ltd.); anion suppressor; conductivity detector; H-type pretreatment column (Qingdao Aili Analysis Experimental Technology);

[0059] TEAL sample (provided by the customer); sodium carbonate (baseline reagent); sodium bicarbonate (excellent grade); isopropanol (chromatographically pure).

[0060] 1.2 Chromatographic conditions

[0061] Chloride ion quasi-stock solution 1000mg / L; flow rate: 1.0mL / min; conductivity detector temperature: 40°C; column temperature: 30°C; inhibition current: 30mA; injection volume: 20μL.

[0062] 1.3 Configuration of the solution

[0063] (1) Preparation of eluent

[0064] Accurately weigh 0.1918g sodium carbonate reference reagent and 0.1344g sodium bicarbonate, place in a 1000mL volumetric flask, dissolve with secondary deionized water and set the volume to the mark to obtain 1.8mmol / L sodium carbonate and 1.6mmol / L carbo...

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Abstract

The invention provides an ion chromatography method for measuring trace chloride ions in triethyl aluminum. The method includes the steps of 1, pretreatment of a sample to be measured, wherein the TEAL sample is dissolved with isopropanol, the volume is kept at scales with secondary deionized water, ultrasonic and centrifugal treatment is carried out, and supernatant is taken, passes through a 0.22-micrometer pin type filter and an H-type pretreatment column, and then enters an ion chromatography system for analysis; 2, preparation of a work curve solution; 3, analysis of a standard addition method solution, wherein the repetitive solution is continuously injected 6 times, a chromatogram of Cl- standard addition solution analysis is obtained, the pretreated triethyl aluminum sample solution is subjected to ion chromatography analysis, the peak area of Cl- is obtained, and the content of Cl- in triethyl aluminum is obtained according to a work curve and the peak area of Cl-. The method is easy to operate, good in repeatability and high in sensitivity, the content of chlorine ions in TEAL can be effectively measured, and the problem that in the measuring process, heavy metal aluminum contaminates and damages the chromatographic column and a suppressor is solved.

Description

technical field [0001] The invention relates to an ion chromatography method for determining trace chloride ions, in particular to an ion chromatography method for determining trace chloride ions in triethylaluminum, and belongs to the technical field of chemical analysis. Background technique [0002] Triethylaluminum TEAL can be used as a catalyst, initiator and rocket fuel, and can also be used as a raw material for MOVCD technology, and can be used to make precipitated aluminum films in the production of diodes, transistors and integrated circuits. In these applications, the content of chloride ions is required to be within a certain range in order to meet the use requirements. Therefore, it is necessary to establish a method for the determination of trace chloride ions in TEAL products and production processes to ensure the performance of the products. [0003] There are no reports about trace chloride ions in TEAL. Therefore, the establishment of a pretreatment metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/96
CPCG01N30/96
Inventor 王鹏功马绪丽赵庆磊王军刘倩倩王芹黄小沛
Owner 中国检验认证集团山东检测有限公司
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