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Method for analyzing arsenic hydride, phosphine and MAP (beta-Methyl vinyl phosphate) in propylene by gas chromatography

A technology of gas chromatography and gas chromatography, which is applied in the field of phosphine, MAP, and gas chromatography to analyze arsine in propylene, can solve the problems that the detection sensitivity and detection range cannot reach the trace level and trace substances, and achieve the solution The effect of insufficient lower limit of detection

Inactive Publication Date: 2018-08-28
云南云天化石化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional analysis methods and analytical instruments such as TCD (thermal conductivity detector) gas chromatograph, FID (hydrogen flame ion detector) gas chromatograph cannot be used for the analysis of trace substances because the detection sensitivity and detection range cannot reach the trace level

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The method for analyzing arsine, phosphine and MAP in propylene by gas chromatography, the detector of gas chromatography is a helium discharge ionization detector with a multidimensional valve column, and the analysis method comprises the following steps:

[0024] 1) Set the parameters of the gas purifier and the gas chromatograph, wherein the temperature of the gas purifier is 395°C, the column oven temperature of the gas chromatograph is 50°C, the detector temperature is 55°C, and the detector The polarization voltage is 155V, the discharge voltage is 530V, and the discharge current is 6.80A;

[0025] 2) Take the standard gas, the content of arsine, phosphine and MAP is Cs, and measure the peak area As corresponding to arsine, phosphine and MAP in the standard gas by the gas chromatograph;

[0026] 3) Get the propylene to be tested, prepare the gas to be tested, and measure the peak area Ai corresponding to arsine, phosphine and MAP in the gas to be tested by the gas...

Embodiment 2

[0030] The method for analyzing arsine, phosphine and MAP in propylene by gas chromatography, the detector of gas chromatography is a helium discharge ionization detector with a multidimensional valve column, and the analysis method comprises the following steps:

[0031] 1) Set the parameters of the gas purifier and the gas chromatograph, wherein the temperature of the gas purifier is 400°C, the column oven temperature of the gas chromatograph is 75°C, the detector temperature is 60°C, and the detector The polarization voltage is 160V, the discharge voltage is 535V, and the discharge current is 6.90A9;

[0032] 2) Take the standard gas, the content of arsine, phosphine and MAP is Cs, and measure the peak area As corresponding to arsine, phosphine and MAP in the standard gas by the gas chromatograph;

[0033] 3) Get the propylene to be tested, prepare the gas to be tested, and measure the peak area Ai corresponding to arsine, phosphine and MAP in the gas to be tested by the ga...

Embodiment 3

[0037] The method for analyzing arsine, phosphine and MAP in propylene by gas chromatography, the detector of gas chromatography is a helium discharge ionization detector with a multidimensional valve column, and the analysis method comprises the following steps:

[0038] 1) Set the parameters of the gas purifier and the gas chromatograph, wherein the temperature of the gas purifier is 395°C to 405°C, the column oven temperature of the gas chromatograph is 100°C, and the detector temperature is 65°C , the polarization voltage of the detector is 165V, the discharge voltage is 540V, and the discharge current is 7.00A;

[0039] 2) Take the standard gas, the content of arsine, phosphine and MAP is Cs, and measure the peak area As corresponding to arsine, phosphine and MAP in the standard gas by the gas chromatograph;

[0040] 3) Get the propylene to be tested, prepare the gas to be tested, and measure the peak area Ai corresponding to arsine, phosphine and MAP in the gas to be tes...

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Abstract

The invention belongs to the technical field of detection, and particularly relates to a method for analyzing arsenic hydride, phosphine and MAP (beta-Methyl vinyl phosphate) in propylene by gas chromatography. A detector of the gas chromatography is a helium discharge ionization detector with a multidimensional valve rod. The analysis method comprises the following steps: 1) setting the parameters of a gas purifier and a gas chromatograph; 2) taking the contents of standard gas, arsenic hydride, phosphine and MAP to be Cs, and measuring a peak area As respectively corresponding to arsenic hydride, phosphine and MAP in the standard gas through the gas chromatograph; 3) taking propylene to be detected; 4) according to a formula Ci is equal to Cs.Ai / As, determining the contents Ci of arsenichydride, phosphine and MAP in the gas to be detected. Through program temperature rise and the multidimensional valve rod, the measurement of arsenic hydride, phosphine and MAP in the propylene gas can be finished while one-time feeding is carried out.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a method for analyzing arsine, phosphine and MAP in propylene by gas chromatography. Background technique [0002] In the production process of propylene resin, the content of arsine and phosphine in propylene raw materials will affect the activity of propylene polymerization catalyst to a certain extent, and react with the titanium active center of the catalyst, thereby poisoning the catalyst, reducing the activity of the catalyst, and then affecting the activity of propylene resin. Therefore, it is usually necessary to control the content of arsine and phosphine in the propylene raw material below 30ppb. Traditional analysis methods and analytical instruments such as TCD (thermal conductivity detector) gas chromatograph, FID (hydrogen flame ion detector) gas chromatograph cannot be used for the analysis of trace substances because the detection sensitivity and det...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/64G01N30/30G01N30/60
CPCG01N30/02G01N30/30G01N30/60G01N30/64
Inventor 陈举钱树伟钱丽萍
Owner 云南云天化石化有限公司
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