Method and system for measuring concentration of sulfide in gas by adopting multi-point calibration curve

A multi-point correction and sulfide technology, applied in the field of detection and analysis, can solve problems affecting the efficiency and safe operation of fuel cell vehicles, poisoning and inactivation of proton exchange membranes, and low detection efficiency, so as to improve accuracy and analysis efficiency and avoid Adsorption loss, the effect of improving the accuracy of analysis

Pending Publication Date: 2021-07-09
CHEM INST OF NAT INST OF MEASUREMENT & TESTING TECH
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0002] As a common toxic and harmful substance, sulfide is the main cause of acid rain in the ambient air; sulfide in natural gas can cause pipeline corrosion and catalyst poisoning; sulfide in fuel cell hydrogen can cause poisoning of proton exchange membranes Deactivation, affecting the efficiency and safe operation of fuel cell vehicles
However, the environmental standard HJ 1078-2019 "Determination of 8 kinds of sulfur-containing organic compounds such as methyl mercaptan in stationary pollution source exhaust gas bag sampling-pre-concentration gas chromatography-mass spectrometry", the natural gas product standard GB 17820-2018 "Natural Gas", fuel cell The hydrogen standard GB / T 37244-2018 "Proton Exchange Membrane Fuel Cell Vehicle Fuel Hydrogen" and other standards have different types of sulfides, limit requirements and analysis methods and other indicators. Low detection efficiency for sulfur compounds

Method used

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  • Method and system for measuring concentration of sulfide in gas by adopting multi-point calibration curve
  • Method and system for measuring concentration of sulfide in gas by adopting multi-point calibration curve
  • Method and system for measuring concentration of sulfide in gas by adopting multi-point calibration curve

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Experimental program
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Effect test

Embodiment

[0027] Systems for the determination of sulfide concentrations in gases using multi-point calibration curves, including:

[0028] Gas sample dilution system: used to dilute the sample, dilute the known concentration of sulfur-containing gas standard substance (100ppb and 100ppm gas standard substance) to a lower concentration to establish two concentration ranges of 1-40ppb and 40ppb-10ppm standard curve;

[0029] Pre-concentration pre-treatment system: used to concentrate samples, the samples described here include standard gas or samples to be tested, and concentrate the trace sulfide in the sample in the focusing tube; if the content of sulfide is high, it is enough to reach Limits for direct chromatographic analysis do not need to be concentrated and focused;

[0030] Sampling selection system: used to deliver the sulfur-containing gas standard substance or the sample to be tested to the pre-concentration pre-treatment system and / or gas chromatographic analysis and proces...

experiment example 1

[0052] The by-product hydrogen of a petroleum refinery is purified by pressure swing adsorption (PSA). The sample is directly entered into the gas chromatography analysis and processing system for qualitative and quantitative analysis of the components through the selected sampling system, such as Figure 4 As shown, according to the peak time, it is determined that the sulfides corresponding to each peak are CH 3 SH, C 4 h 4 S, the peak area value corresponding to each peak is first brought into the linear equation of the standard curve II of the sulfide for verification. If the verification fails, the sample enters the pre-concentration pre-treatment system for concentration and enrichment, and then enters the gas chromatography analysis and processing system For analysis, the peak area value corresponding to each peak was brought into the standard curve I to calculate the concentration, and the concentration is shown in Table 4.

[0053] Table 4. Analysis data sheet of by...

experiment example 2

[0056] When the sample is injected and analyzed, since the concentration of the components in the sample cannot be determined, the sample directly enters the gas chromatography analysis and processing system through the selected sampling system for qualitative and quantitative analysis of the components, such as Figure 5 As shown, according to the peak time, it is determined that the sulfides corresponding to each peak are H 2 S, COS, CH 3 SH, C 2 h 5 SH, CH 3 SC 2 h 5 、C 2 h 5 SC 2 h 5 , put the peak area values ​​corresponding to each peak into the linear equation of the standard curve II of the sulfide for verification, and if the verification is passed, the concentration of each sulfide is obtained, as shown in Table 5.

[0057] Table 5. Analysis data table of sulfide in a natural gas purification plant

[0058] Peak time / min components Peak area Calculated value / ppm 3.987 h 2 S

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Abstract

The invention discloses a method and a system for measuring the concentration of sulfide in gas by adopting a multi-point calibration curve. The method comprises the following steps of (1) establishing a 1-40ppb standard curve I and a 40ppb-10ppm standard curve II, (2) sample introduction: directly introducing the sample into a gas chromatographic analysis processing system for qualitative and quantitative analysis of components, determining sulfide corresponding to each peak according to peak appearance time, then introducing a peak area value corresponding to each peak into a linear equation of a standard curve II of the sulfide for verification, and if the verification is passed, obtaining the sulfide concentration X, and if the verification is not passed, entering a pre-concentration pretreatment system, then entering a gas chromatographic analysis treatment system for analysis, and substituting peak area values corresponding to all peaks into the standard curve I to calculate the concentration. According to the method disclosed by the invention, automatic qualitative and quantitative analysis on conventional sulfides in different concentration ranges in ambient air, natural gas and hydrogen for fuel cells is realized, and the analysis accuracy and the analysis efficiency are improved.

Description

technical field [0001] The invention belongs to the field of detection and analysis, and in particular relates to a method and a system for measuring the concentration of sulfide in gas by using a multi-point calibration curve. Background technique [0002] As a common toxic and harmful substance, sulfide is the main cause of acid rain in the ambient air; sulfide in natural gas can cause pipeline corrosion and catalyst poisoning; sulfide in fuel cell hydrogen can cause poisoning of proton exchange membranes Deactivation affects the efficiency and safe operation of fuel cell vehicles. However, the environmental standard HJ 1078-2019 "Determination of 8 kinds of sulfur-containing organic compounds such as methyl mercaptan in stationary pollution source exhaust gas bag sampling-pre-concentration gas chromatography-mass spectrometry", the natural gas product standard GB 17820-2018 "Natural Gas", fuel cell The hydrogen standard GB / T 37244-2018 "Proton Exchange Membrane Fuel Cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/04G01N30/08G01N30/20G01N30/86
CPCG01N30/02G01N30/06G01N30/04G01N30/08G01N30/20G01N30/8679G01N30/8634G01N2030/042
Inventor 潘义张婷邓凡锋林俊杰王维康方正
Owner CHEM INST OF NAT INST OF MEASUREMENT & TESTING TECH
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