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Quick chromatographic analysis method for trace ammonia in gas

A chromatographic analysis and gas chromatographic separation technology, applied in the field of rapid chromatographic analysis of trace ammonia in gas, can solve problems such as difficulty in ammonia detection, and achieve the effects of shortening analysis time, high separation efficiency and good technical effect

Active Publication Date: 2013-04-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is the difficult problem of ammonia detection when the existing gas chromatography technology analyzes the NO raw material gas with an ammonia content lower than 1000ppm, and a fast chromatographic analysis method for trace ammonia is proposed

Method used

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  • Quick chromatographic analysis method for trace ammonia in gas
  • Quick chromatographic analysis method for trace ammonia in gas

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Embodiment 1

[0028] Adopt the method of the present invention, NO content is 10%, the standard gas that ammonia content is in the scope of 0.008%-0.1% is analyzed, and the content of ammonia is calculated by external standard method, and typical chromatographic analysis condition is shown in Table 1, and typical chromatogram sees figure 1 , and the analysis results are shown in Table 2.

[0029] Table 1 Typical chromatographic analysis conditions

[0030]

[0031] Table 2 Standard gas analysis results

[0032]

[0033] It can be seen from Table 2 that the relative error between the measured content and the actual content of ammonia in the standard gas is not more than 10%. The standard gas with an ammonia content of 0.02% (V / V) was analyzed, and the relative standard deviation of five repeated measurements was less than 2%. It has been determined that the minimum detection limit of the method for ammonia is about 0.005% (V / V).

Embodiment 2

[0035] Adopt the method of the present invention, analyze the ammonia in NO actual sample gas, calculate the content of trace ammonia by external standard method, typical chromatographic conditions see Table 1, the chromatogram of sample 1 sees figure 1 , and the analysis results are shown in Table 3.

[0036] Table 3 actual sample gas analysis results

[0037]

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Abstract

The invention relates to a quick chromatographic analysis method for trace ammonia in gas, and provides a quick chromatographic analysis method for the trace ammonia by mainly solving the problem in the traditional gas chromatography technology that ammonia is difficult to detect when the ammonia content in the NO raw material gas is lower than 1000ppm. The quick chromatographic analysis method for the trace ammonia in the gas successively comprises the following steps of: (1) introducing sample gas into a sampling pipeline and a sample ring via a vacuum pump; (2) leading gas in the sample ring into a chromatographic system by carrier gas, and separating the ammonia in the sample gas from other components by a pre-dissociation column and an analysis column; and (3) detecting the separated ammonia in a high-sensitive thermal conductivity detector. The problem is better solved by the technical scheme of external standard method quantitation, and the quick chromatographic analysis method for the trace ammonia in the gas can be used for the industrial production of preparing ethylene glycol by synthesis gas.

Description

technical field [0001] The invention relates to a fast chromatographic analysis method for trace amounts of ammonia in gas, in particular to a fast chromatographic analysis method for ammonia in NO gas with an ammonia content lower than 0.1 percent (ie 1000 ppm). Background technique [0002] In recent years, with the shortage of petroleum resources, the process of producing ethylene glycol from synthetic gas through oxalate has become a research hotspot, and is considered to be the main development direction of non-petroleum route production of ethylene glycol technology. [0003] The process of producing ethylene glycol from synthesis gas through oxalate is very complicated. The main reaction principle is: O2, NO react with methanol to form methyl nitrite, methyl nitrite and CO undergo coupling reaction to obtain dimethyl oxalate, and then Polyester grade ethylene glycol products are obtained through hydrogenation and refining processes. NO raw material gas can be prepare...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 张育红彭振磊王川
Owner CHINA PETROLEUM & CHEM CORP