Device and method for detecting sulfur isotopes in gas in continuous flow mode

A technology for sulfur isotope and gas detection, which is applied in measurement devices, material analysis by electromagnetic means, instruments, etc., can solve the problems of environmental pollution, strong viscosity of pipelines, and difficult to store, and achieves convenient and fast operation and corrosion resistance. Strong performance and the effect of reducing retention

Pending Publication Date: 2021-02-12
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods all include two or more steps of chemical reaction. In order to prevent isotope fractionation, the chemical reaction must be thorough. Therefore, the operation requirements are very strict, and there are many factors that cause errors in the response.
At the same time, the chemical pretreatment containing sulfur is more harmful
And in the process of isotope mass spectrometry, SO 2 As a working reference gas, due to SO 2 It is a highly toxic sulfuric acid gas, not easy to store, and has strong viscosity in the pipeline, which is easy to cause corrosion to the pipeline and pollute the environment

Method used

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  • Device and method for detecting sulfur isotopes in gas in continuous flow mode

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Experimental program
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Effect test

Embodiment 1

[0041] This embodiment provides a device for detecting sulfur isotopes in gas in continuous flow mode. See figure 1 , figure 1 A schematic diagram of the device for detecting sulfur isotopes in gas under continuous flow mode provided by the present invention is shown. Such as figure 1As shown, the device includes: a gas storage tank 1 for storing gas samples, a cold trap 2, an element analyzer 3, an isotope mass spectrometer 4, a six-way valve F1, a four-way valve F2, a first helium delivery pipeline A, a second Two helium delivery pipelines B, the first inlet pipeline C, the vent pipeline D, the oxygen delivery pipeline E, and the second inlet pipeline F; the element analyzer includes: a solid autosampler 301, a combustion furnace 302, and a reduction Furnace 303; the first helium delivery pipeline A, the gas storage tank 1, the cold trap 2, the first intake pipeline C, the combustion furnace 302, the reduction furnace 303, the second Two intake pipelines F and the isotop...

Embodiment 2

[0043] This embodiment provides a method for detecting sulfur isotopes in gas in continuous flow mode. This method is carried out in the device that embodiment 1 mentions, and described method comprises the following steps:

[0044] S1. Helium carries the gas sample released from the gas storage tank 1 through the first helium delivery line A into the cold trap 2 for cooling and adsorption, and the gas that is not cooled and adsorbed in the gas sample is discharged from the vent line D The device is ejected.

[0045] S2. Place the solid standard substance in the solid autosampler 301, enter the combustion furnace 302 through the solid autosampler 301, and simultaneously oxygen is transported to the combustion furnace through the oxygen delivery pipeline E In 302, the solid standard substance is fully burned to generate gas containing sulfur dioxide and sulfur trioxide, and then sent to the reduction furnace 303 to reduce the sulfur trioxide in the gas to sulfur dioxide.

[0...

Embodiment 3

[0051] Utilize the method that embodiment 2 provides to H in natural gas 2 The sulfur isotope of S was determined.

[0052] Adopt high-pressure aluminum alloy steel cylinders to collect natural gas, and natural gas is passed through the cold trap 2 of liquid nitrogen freezing (such as figure 1 shown), H in natural gas 2 S is frozen and enriched in cold trap 2, He, N 2 , and CH 4 After the gas not absorbed by freezing is emptied, the solid standard substance is sent into the element analyzer-isotope mass spectrometry system through the solid sampler 301, and the signals of m / e=36 and m / e=34 are measured.

[0053] Switching the six-way valve F1 to heat up the cold trap 2 will make the enriched H 2 Gases such as S are carried by He into the element analyzer-isotopic mass spectrometer, and the signals of m / e=36 and m / e=34 are measured; the signal of the sulfur isotope is compared with the signal of the sulfur isotope of the solid standard substance, according to the existing ...

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Abstract

The invention belongs to the technical field of isotope analysis and detection, and relates to a device for detecting sulfur isotopes in gas in a continuous flow mode. The device comprises a gas storage tank for storing a gas sample, a cold trap, an element instrument, an isotope mass spectrometer, a first helium conveying pipeline, a second helium conveying pipeline, a first gas inlet pipeline, an emptying pipeline, an oxygen conveying pipeline and a second gas inlet pipeline; the elemental instrument comprises an automatic solid sample injector, a combustion furnace and a reduction furnace;the first helium conveying pipeline, the gas storage tank, the cold trap, the first gas inlet pipeline, the combustion furnace, the reduction furnace, the second gas inlet pipeline and the isotope mass spectrometer are sequentially communicated; the cold trap is communicated with an emptying pipeline; the second helium conveying pipeline is communicated with the gas inlet end of the cold trap; andthe oxygen conveying pipeline is communicated with the combustion furnace. According to the device, a gas sample does not need to be pretreated, and the sulfur isotope in the gas sample can be calibrated by utilizing the solid standard substance.

Description

technical field [0001] The invention belongs to the technical field of isotope analysis and detection, and more specifically relates to a device and method for detecting sulfur isotopes in gas in a continuous flow mode. Background technique [0002] Continuous flow mass spectrometry (CF-IRMS) is a new type of instrument developed on the basis of gas isotope mass spectrometry. It connects the element analyzer and the isotope ratio mass spectrometer through a continuous flow interface to realize the on-line analysis of stable isotopes. The continuous flow mass spectrometer directly collects the target gas into the mass spectrometer ion source under the helium flow. Since the sample processing and measurement are carried out continuously on-line, it can reduce the loss of the sample during the analysis process and improve the analysis speed and sensitivity. [0003] The analysis method of continuous flow mass spectrometry to detect sulfur isotopes is based on the principle of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/626
CPCG01N27/62
Inventor 腾格尔陶成杨华敏王杰王萍把立强李广友
Owner CHINA PETROLEUM & CHEM CORP
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