Method for analyzing contents of trace arsine and phosphine in gas-phase propylene by gas chromatograph

A gas chromatograph and trace arsenic technology, which is applied in the field of analyzing trace arsine and phosphine content in gas phase propylene, can solve problems such as difficulty in meeting process analysis requirements, and achieve timely and effective process production and fast analysis speed

Active Publication Date: 2012-07-18
CHNA ENERGY INVESTMENT CORP LTD +2
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Problems solved by technology

[0005] The present invention aims to provide a method for determining the content of trace arsine and phosphine in gas phase propylene, so as to solve the problem that

Method used

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  • Method for analyzing contents of trace arsine and phosphine in gas-phase propylene by gas chromatograph

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Set the temperature of the purifier to 400°C, the temperature of the column oven to 50°C, the temperature of the detector to 60°C, the polarization voltage of the detector to 160V, the discharge voltage to 534V, and the discharge current to 6.88 A, backflush time 7min. Determination was carried out according to the above-mentioned steps for measuring samples, and the determination was repeated four times. The measurement results of Example 1 are shown in Table 1.

[0037] Table 1

[0038] Arsenic content

Embodiment 2

[0040] Set the temperature of the purifier to 402°C, the temperature of the column oven to 48°C, the temperature of the detector to 58°C, the polarization voltage of the detector to 158V, the discharge voltage to 533V, and the discharge current to 6.85 A, backflush time 8min. The determination was carried out according to the above-mentioned steps for determining the sample, and the determination was repeated four times.

Embodiment 3

[0042] Set the temperature of the purifier to 398°C, the temperature of the column oven to 52°C, the temperature of the detector to 62°C, the polarization voltage of the detector to 162V, the discharge voltage to 535V, and the discharge current to 6.70 A, backflush time 8min. The determination was carried out according to the above-mentioned steps for determining the sample, and the determination was repeated four times.

[0043] The respective mean values ​​and relative standard deviations were obtained by calculating the experimental results of 1-3, and the calculation results are shown in Table 2.

[0044] Table 2

[0045]

[0046] It can be seen from the test results in Table 1 and Table 2 that the relative standard deviations of arsine and phosphine are small, which greatly meet the requirements of industrial analysis.

[0047] And, find out from embodiment 1, embodiment 2 and embodiment 3, utilize gas chromatograph to measure the content of arsine and phosphine in g...

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Abstract

The invention provides a method for analyzing contents of trace arsine and phosphine in gas-phase propylene by a gas chromatograph. A detector of the gas chromatograph is a helium discharge ionization detector. The method comprises the steps as follows: 1) setting the parameters of a gas purifier and the gas chromatograph; 2) preparing standard gas with the content of arsine or phosphine being Cs and measuring the peak area As which corresponds to arsine or phosphine in the standard gas by the gas chromatograph; 3) taking the propylene to be detected, preparing gas to be detected, and measuring the peak area Ai which corresponds to arsine or phosphine in the gas to be detected by the gas chromatograph; and 4) determining the content Ci of arsine or phosphine in the gas to be detected, in accordance with the formula that Ci is equal to Cs*Ai/As. By the combination of the gas chromatograph and the helium discharge ionization detector, the component changing of a sample can be sensitively, rapidly, correctly and continuously reflected, arsine and phosphine can be detected simultaneously, the amount of the needed samples is small, and other toxic and harmful chemical agents are not needed. Therefore the method is safe and sanitary and can timely and effectively guide technological production.

Description

technical field [0001] The application relates to the field of propylene polymerization to produce polypropylene resin, in particular to a method for analyzing trace arsine and phosphine content in gas phase 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 30 ppb. 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 substa...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 王玉辉何马睿
Owner CHNA ENERGY INVESTMENT CORP LTD
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