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A gas chromatograph and detection method for measuring the total content of sulfide in natural gas

A technology of gas chromatography and detection method, which is applied in the gas chromatograph and detection field for determining the total content of sulfide in natural gas, can solve the problems of tedious quantification, low sensitivity, spectral interference, etc., and achieves accurate test results, wide application range, calculation easy effect

Active Publication Date: 2018-04-17
CHEM INST OF NAT INST OF MEASUREMENT & TESTING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] TCD is based on the principle that different analytical components and carrier gases have different thermal conductivity. It is a general-purpose non-destructive concentration detector, which can be applied to the detection of any component in theory, but the sensitivity is low; gas chromatography- Flame photometry (FPD) is a selective detector that uses hydrogen flame combustion to generate sulfur and phosphorus into its oxidation state, and detects sulfide by collecting the characteristic spectra of sulfur and phosphorus. However, this method is prone to quenching effects and has low sensitivity. Linear response, quantification is cumbersome; pulsed flame photometric detector (PFPD) is developed on the basis of flame photometric detector, but the signal response is not linear; atomic emission detector (AED) is very important in the chromatography of atomic emission spectroscopy The application can realize the simultaneous analysis of multiple components, but its spectral interference is serious, and the elements with the same emission line will cause great interference; although the mass selective detector (MSD) can measure trace amounts of sulfide, it is expensive, In addition, higher concentrations of sulfide will corrode the ion source and reduce its service life

Method used

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  • A gas chromatograph and detection method for measuring the total content of sulfide in natural gas
  • A gas chromatograph and detection method for measuring the total content of sulfide in natural gas
  • A gas chromatograph and detection method for measuring the total content of sulfide in natural gas

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Effect test

specific Embodiment 1

[0028] Test samples containing methane, ethylene, and propylene hydrocarbons separately, and compare them with nitrogen and air samples. The test steps are as follows:

[0029] A. The gas sample of hydrocarbons containing methane enters the hydrogen flame ionization detector 2 from the inlet through the uncoated fused silica capillary column 1 on the inner wall, and fully burns in the hydrogen flame ionization detector 2;

[0030] B. After combustion, the gas enters the sulfur chemiluminescence detector 4 for reaction, the combustion temperature is 800°C, and the air flow rate is 5mL / min;

[0031] C. The processor receives the signal transmitted by the sulfur chemiluminescence detector 4 to obtain a chromatogram;

[0032] D, with single-component sulfur dioxide gas as a standard sample, repeat steps (A) ~ (C);

[0033] E. Integrate the single peak of the chromatogram obtained in step (C) and step (D), and compare the integral values ​​to obtain the total sulfide content in na...

specific Embodiment 2

[0036] To test gas samples containing hydrogen sulfide, carbonyl sulfide, sulfur dioxide, methyl mercaptan and methyl sulfide, the specific steps are as follows:

[0037] A. The gas sample containing hydrogen sulfide enters the hydrogen flame ionization detector 2 from the inlet through the uncoated fused silica capillary column 1 on the inner wall, and fully burns in the hydrogen flame ionization detector 2;

[0038] B. After combustion, the gas enters the sulfur chemiluminescence detector 4 for reaction, the combustion temperature is 800°C, and the air flow rate is 5mL / min;

[0039] C. The processor receives the signal transmitted by the sulfur chemiluminescence detector 4 to obtain a chromatogram;

[0040] D, with single-component sulfur dioxide gas as a standard sample, repeat steps (A) ~ (C);

[0041] E. Integrate the single peak of the chromatogram obtained in step (C) and step (D), and compare the integral values ​​to obtain the total sulfide content in natural gas.

...

specific Embodiment 3

[0044] Test the mixture gas containing hydrocarbons such as methane and ethane and multi-component sulfides such as hydrogen sulfide, carbonyl sulfide and methyl mercaptan; the specific steps are as follows:

[0045] A. The mixture gas sample composed of methane, ethane and other hydrocarbons and multi-component sulfides such as hydrogen sulfide, carbonyl sulfide and methyl mercaptan enters the hydrogen flame ion from the inlet through the uncoated fused silica capillary column 1 In the ionization detector 2, fully burn in the hydrogen flame ionization detector 2;

[0046] B. After combustion, the gas enters the sulfur chemiluminescence detector 4 for reaction, the combustion temperature is 800°C, and the air flow rate is 5mL / min;

[0047] C. The processor receives the signal transmitted by the sulfur chemiluminescence detector 4 to obtain a chromatogram;

[0048] D, with single-component sulfur dioxide gas as a standard sample, repeat steps (A) ~ (C);

[0049] E. Integrate ...

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Abstract

The invention discloses a gas chromatograph and detection method for determining the total content of sulfides in natural gas. The gas chromatograph comprises a quartz capillary column, a hydrogen flame ionization detector, a temperature control unit and a sulfur chemiluminescence reactor which are successively connected, wherein the quartz capillary column is a fused silica capillary column with uncoated inner walls; and the gas chromatograph further comprises a processor which is connected with the sulfur chemiluminescence reactor and a display unit. The gas chromatograph and detection method provided by the invention eliminate influence of hydrocarbons on determination of sulfide content, are more accurate in testing and have a wider application scope.

Description

technical field [0001] The invention relates to a gas chromatographic detection technology in analytical chemistry, in particular to a gas chromatograph and a detection method for measuring the total sulfide content in natural gas. Background technique [0002] The sulfide content is one of the very important test indicators in natural gas and petrochemical industries; at present, the use of gas chromatography to determine the total sulfide content in natural gas is the most widely used method; there are many types of detectors, and the commonly used method for the determination of sulfide The detectors are Thermal Conductivity Detector (TCD), Flame Photometric Detector (FPD), Pulsed Flame Photometric Detector (PFPD), Atomic Emission Detector (AED), Electrochemical Detector (ED) and Mass Selective Detector (MSD), etc. [0003] TCD is based on the principle that different analytical components and carrier gases have different thermal conductivity. It is a general-purpose non...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/60G01N30/64G01N30/68
CPCG01N30/02G01N30/6078G01N30/64G01N30/68G01N2030/025
Inventor 方正潘义李志昂周鑫王维康
Owner CHEM INST OF NAT INST OF MEASUREMENT & TESTING TECH
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