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Trace nitrogen isotope analysis system and method

An analysis system and nitrogen isotope technology, applied in the analysis system of trace nitrogen isotopes, the field of trace nitrogen isotope analysis, can solve the problems of cumbersome experimental process, sample loss, small analysis error, etc., achieve simple and controllable process, reduce detection limit, Analysis of the effect of small errors

Inactive Publication Date: 2019-08-20
INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the existing off-line analysis technology of trace nitrogen isotopes, which has large analysis errors, harsh operating conditions for low background, high analytical detection limit of mass spectrometer, high sample consumption, cumbersome experimental process and low efficiency. And the existing online continuous flow analysis technology has limitations when analyzing solid samples, and there will be sample loss during the sampling process, the inability to maximize the use of sample gas, high detection limits of instruments, and low precision. Provide a An analysis system for trace nitrogen isotopes in gaseous samples or solid samples and a method for analyzing trace nitrogen isotopes in gaseous samples or solid samples using the analysis system, the system can realize rapid analysis of trace nitrogen isotopes in gaseous samples or solid samples, and solves the problem of When the content of nitrogen in the sample is too low, it is difficult to analyze accurately, and the process of using this system to analyze trace nitrogen isotopes in gaseous samples or solid samples is simple, controllable, easy to operate, and can maximize the use of sample gas. Low, high sensitivity, small analysis error, high accuracy, and adopts the method of individual packaging, can prepare multiple samples at the same time, realize continuous testing of multiple samples, and will not cause memory effect

Method used

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Examples

Experimental program
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Effect test

preparation example S-I

[0101] Preparation of a sample collection tube encapsulating a gaseous sample containing nitrogen to be measured

[0102] Place the capillary in the atmosphere of the gaseous sample to be tested at 20°C for 5 hours, and then use a liquefied gas torch to heat the two ends of the capillary to melt and seal the two ends of the capillary, so as to obtain the sealing of the two ends of the gaseous sample to be tested containing nitrogen. A capillary sample collection tube with a length of 5-8cm, an outer diameter of 1-2mm, and a wall thickness of 0.1-0.2mm is ready for use.

preparation example S-II

[0104] Preparation of a sample collection tube encapsulating a gaseous sample to be tested obtained by carrying out a nitrogen element transfer reaction on a solid sample to be tested containing nitrogen

[0105] Put the solid sample, 100mg copper wire and 150mg copper oxide wire into a quartz tube with a flat mouth and a round bottom, the top of the quartz tube is provided with a sealing joint and a vacuum gauge, and then the quartz tube is connected to the vacuum pipeline through the sealing joint. The quartz tube is vacuumized, and the quartz tube is heated to 150°C during the vacuuming process, and the vacuum degree in the quartz tube reaches 1×10 -4 Pa, use a liquefied gas torch to heat below the connection of the quartz tube and the sealing interface of the vacuum pipeline, and the distance from the connection is 10-20% of the total length of the quartz tube to make it melt and seal, thereby obtaining A sample collection tube with both ends of the sealed solid sample con...

Embodiment 1

[0107] (i) press figure 1 The connections shown were used to assemble the trace nitrogen isotope analysis system.

[0108] The analysis system includes: primary purification unit U-I, control unit U-II and secondary purification sampling unit U-III, wherein the primary purification unit U-I, control unit U-II and secondary purification sampling unit U- III is sequentially connected through the connecting pipeline; wherein, the control unit U-II and the secondary purification sampling unit U-III are pre-vacuumized before being connected to the system,

[0109] The primary purification unit U-I includes: a first carrier gas cylinder 1-1, a first cold trap 2-1, a ripple breaker 3 and a second cold trap 2-2 connected in sequence, wherein the first carrier gas Bottle 1-1 is a high-purity helium (99.999% by volume) bottle, and 5A molecular sieve 1-2g is filled in the first cold trap 2-1;

[0110] The secondary purification sampling unit U-III includes: the second carrier gas bottl...

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Abstract

The invention belongs to the technical field of isotope analysis and discloses a trace nitrogen isotope analysis system and a trace nitrogen isotope analysis method using the same. The analysis systemcomprises a primary purification unit (U-I), a control unit (U-II) and a secondary purification sampling unit (U-III), wherein the primary purification unit (U-I), the control unit (U-II) and the secondary purification sampling unit (U-III) are sequentially connected with one another through a connecting pipeline. With the system and method provided by the invention adopted, the analysis of tracenitrogen isotope in a gaseous sample or a solid sample can be realized. The system and the method have the advantages of high precision, high accuracy and the like.

Description

technical field [0001] The invention relates to the technical field of stable isotope analysis, in particular to a trace nitrogen isotope analysis system and a method for using the system to conduct trace nitrogen isotope analysis. Background technique [0002] Nitrogen isotope analysis technology in samples is an important means to reconstruct the earth's nitrogen cycle and soil nitrogen cycle. The analysis technology of nitrogen isotope usually needs to completely convert the nitrogen in solid samples such as rock and soil into nitrogen gas, and then introduce the nitrogen gas into the gas isotope mass spectrometer through the sampling device for nitrogen isotope analysis, and gaseous samples can be directly introduced into the gas isotope Nitrogen isotope analysis was performed in mass spectrometry. [0003] There are generally two sampling methods and setups for introducing nitrogen into the mass spectrometer. One is to collect nitrogen through a vacuum system, and con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/20G01N30/06
CPCG01N30/06G01N30/20G01N30/88G01N2030/201G01N2030/8868
Inventor 冯连君李洪伟
Owner INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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