Method for analyzing sulfur-containing compound in liquefied gas

An analytical method and technology for sulfur compounds, which are applied in the direction of analyzing materials, analyzing by chemical reaction of materials, chemiluminescence/bioluminescence, etc., can solve problems such as inaccurate composition and content, and achieve simple and easy-to-operate methods and accurate measurement results. The effect of reliability, strong operability and application prospect

Active Publication Date: 2018-06-26
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main purpose of the present invention is to provide a method for analyzing sulfur-containing compounds in liquefied gas, so as to overcome the problem of inaccurate composition and content caused by uneven gasification of gaseous samples when analyzing sulfur-containing compounds in the prior art

Method used

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  • Method for analyzing sulfur-containing compound in liquefied gas
  • Method for analyzing sulfur-containing compound in liquefied gas
  • Method for analyzing sulfur-containing compound in liquefied gas

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Prepare liquefied gas standards containing 35 sulfur compounds. A high-pressure liquid sampling valve was used to analyze the composition of the liquefied gas standard. The operating pressure of the high-pressure liquid sampling valve was 23 psi, and the valve capacity specification was 1 μL. GC-SCD operating conditions are: inlet temperature 250°C, split ratio 80:1; constant pressure operation, pressure 15psi; heating program: initial temperature is 50°C, after constant temperature for 4 minutes, the temperature is raised to 100°C at 10°C / min , after 6 minutes of constant temperature, the temperature was raised to 180°C at 15°C / min, and the temperature was kept constant for 10 minutes. Under these conditions, the chromatograms of each sulfur-containing compound are shown in figure 1 and figure 2 , the retention time of each compound is shown in Table 1.

[0031] This method can provide morphological information of 35 sulfur-containing compounds, and the resolution ...

Embodiment 2

[0035] Qingyang Petrochemical liquefied gas samples were collected according to the SH / T 0233 liquefied gas sampling method.

[0036] The qualitative analysis of the liquefied gas samples of Qingyang Petrochemical was carried out under the conditions described in Example 1: the composition of the liquefied gas samples was analyzed using a high-pressure liquid sampling valve, the operating pressure of the high-pressure liquid sampling valve was 23 psi, and the valve capacity specification was 1 μL. GC-SCD operating conditions are: inlet temperature 250°C, split ratio 80:1; constant pressure operation, pressure 15psi; heating program: initial temperature is 50°C, after constant temperature for 4 minutes, the temperature is raised to 100°C at 10°C / min , after 6 minutes of constant temperature, the temperature was raised to 180°C at 15°C / min, and the temperature was kept constant for 10 minutes. The obtained liquefied gas samples contained six sulfur-containing compounds, and the ...

Embodiment 3

[0041] Collect liquefied gas samples according to SH / T 0233 liquefied gas sampling method.

[0042] The process and conditions described in Example 1 were used to determine the composition of the liquefied gas, and the results are shown in Table 3.

[0043] Use a high-pressure liquid sampling valve to analyze the relative percentage of liquefied gas. The external standard sample of liquefied gas with a concentration of dimethyl sulfide (calculated based on sulfur content) is 51.67 μg / g. The analysis condition is that the operating pressure of the high-pressure liquid sampling valve is 18psi. , The valve capacity specification is 0.5μL. The operating conditions of GC-SCD are: the inlet temperature is 200°C, the split ratio is 30:1; the front pressure of the column is 20psi; °C, and then heated up to 170 °C at 20 °C / min. The content of sulfur compounds in liquefied gas is shown in Table 3.

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Abstract

The invention discloses a method for analyzing the sulfur-containing compound in liquefied gas. The method adopts a gas chromatography-sulfur chemiluminescence detector, and comprises: (1) sample collection; (2) sample determination: feeding liquefied gas in a liquid state into a gas chromatograph through a high-pressure liquid sample injection valve, and obtaining a sample detection spectrum through a sulfur chemiluminescence detector; (3) qualitative analysis: comparing the sample detection spectrum to the sulfur standard substance retention time database obtained under the same sample determination chromatography conditions, and determining the type of the sulfur compound in the liquefied gas according to the retention time; and (4) quantitative analysis: selecting an organic sulfide asan external standard substance, determine the quantitative response factor under the sample determination chromatography conditions, integrating the peak area of the sulfur compound in the detectionspectrum, and obtaining the sulfur content corresponding to the peak area of the sulfur compound according to the quantitative response factor. According to the present invention, with the method, thecontent and the composition of the sulfur-containing compound in the liquefied gas can be accurately analyzed, and the accuracy of the quantitation is high.

Description

technical field [0001] The invention relates to the field of petrochemical industry, in particular to a qualitative and quantitative method for measuring sulfur-containing compounds in liquefied gas by using a gas chromatography-sulfur chemiluminescence detector. Background technique [0002] With the implementation of the quality upgrade of gasoline products, the demand for low-sulfur methyl tert-butyl ether (MTBE) is becoming stronger and stronger. The sulfur-containing compounds in methyl tert-butyl ether products are mainly derived from its synthetic raw material liquefied petroleum gas, so the production of qualified low-sulfur liquefied petroleum gas is the key to the production of low-sulfur methyl tert-butyl ether products. Studying the form of sulfur-containing compounds in liquefied petroleum gas can provide information on the form and content of sulfur-containing compounds for the development of low-sulfur liquefied petroleum gas technology, thereby providing a re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/20G01N21/76
CPCG01N21/766G01N30/20G01N30/88G01N2030/8859
Inventor 史得军陈菲肖占敏薛慧峰杨晓彦王春燕陈芬芬修远徐华徐昆仑汪艳
Owner PETROCHINA CO LTD
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