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A method for measuring nitrogen concentration based on trace gas preconcentration device-isotope ratio mass spectrometry

An isotope ratio and trace gas technology, which is used in measurement devices, preparation of test samples, instruments, etc., can solve the problems of difficulty, unable to find instruments with nitrogen concentration, and high nitrogen background value, and achieves simple operation and short measurement time. Effect

Active Publication Date: 2019-03-12
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is difficult to quantitatively measure the nitrogen concentration produced during the denitrification process due to some reasons
First of all, the background value of nitrogen in the atmospheric environment is very high, and it is very difficult to accurately quantitatively measure the trace amount of nitrogen produced in the denitrification process.
In addition, because nitrogen is an inert gas, it is difficult to react with other substances. It is impossible to manufacture and provide a detector that can directly determine the nitrogen content by using the existing scientific research and analysis technology. Therefore, various scientific research units basically cannot find an instrument that can measure the nitrogen concentration.
Since there is no in situ and non-destructive method and technology to measure nitrogen produced by denitrification and anammox in natural systems, it is still impossible to quantitatively evaluate the change trend of nitrogen concentration in various circles of the earth, so it is seriously severely limited the assessment of the consequences of nitrogen accumulation

Method used

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  • A method for measuring nitrogen concentration based on trace gas preconcentration device-isotope ratio mass spectrometry
  • A method for measuring nitrogen concentration based on trace gas preconcentration device-isotope ratio mass spectrometry
  • A method for measuring nitrogen concentration based on trace gas preconcentration device-isotope ratio mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: The linear relationship between the concentration of the natural abundance nitrogen standard sample and the signal value of the m / z 28 ion current

[0022] (1) Preparation of natural-abundance nitrogen standard samples: use airtight syringes for collection, prepare 16 concentration gradients from 0.1mL to 10mL of natural-abundance air, inject it into a vacuum bottle, and balance it with high-purity helium;

[0023] (2) Using the PreCon-IRMS automatic sampling method to measure the m / z 28 ion current signal value and nitrogen isotope ratio of the naturally abundant nitrogen standard sample;

[0024] (3) Draw the correlation diagram between the concentration of the natural abundance nitrogen standard sample and the m / z 28 ion current signal value and the nitrogen isotope ratio as shown in figure 1 shown.

Embodiment 2

[0025] Embodiment 2: must 15 The linear relationship between the concentration of N abundance nitrogen standard sample and the signal value of m / z 28 ion current

[0026] (1) must 15 Preparation of N abundance nitrogen standard samples: using 15 N abundance of 10.32atom% ( 15 NH 4 ) 2 SO 4 React with NaBrO solution to produce nitrogen with an abundance of 0.8atom%, and mix it with some air to make a certain 15 N-rich nitrogen. will be sure 15 Prepare 16 concentration gradients of N-rich nitrogen from 0.1mL to 10mL, inject it into a vacuum bottle, and balance it with high-purity helium;

[0027] (2) Use the PreCon-IRMS automatic sampling method to determine a certain 15 The m / z 28 ion current signal value and nitrogen isotope ratio of the nitrogen standard sample of N abundance;

[0028] (3) draw certain 15 The correlation diagram of nitrogen standard sample concentration of N abundance and m / z 28 ion current signal intensity and nitrogen isotope ratio figure 2 sho...

Embodiment 3

[0030] Embodiment 3: verify the accuracy and precision of measuring nitrogen concentration

[0031] (1) Preparation of nitrogen samples with known concentrations: collect 0.5, 2.0, 6.0 and 10.0 mL of air and inject them into vacuum bottles respectively, and balance with high-purity helium to obtain nitrogen concentrations of 0.025, 0.100, 0.300 and 0.500 L respectively / L, each of the above concentrations made three replicate samples;

[0032] (2) Utilize the PreCon-IRMS automatic sampling method to measure the m / z 28 ion current signal value and the nitrogen isotope ratio of the nitrogen sample prepared in step (1);

[0033] (3) Bring the obtained nitrogen sample m / z 28 ion current signal values ​​into figure 1 and figure 2 The nitrogen sample concentration was calculated from the linear equation shown for the nitrogen standard sample concentration versus the m / z 28 ion current signal value. The specific results are shown in Table 1:

[0034] Table 1: The linear relationsh...

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Abstract

The invention discloses a method for measuring the nitrogen concentration based on a trace-gas preconcentration device-isotope ratio mass spectrometer (PreCon-IRMS). The method includes the steps that an isotope ratio mass spectrum serves as a nitrogen detector, the m / z 28 ion current intensity of a to-be-detected nitrogen sample is directly measured through the PreCon-IRMS, and then the concentration of the to-be-detected nitrogen sample is calculated according to the linear relationship between the m / z 28 ion current intensity of a standard nitrogen sample and the concentration. The method is easy to operate and short in measuring time.

Description

technical field [0001] The invention relates to a method for measuring nitrogen concentration, in particular to a method for measuring nitrogen concentration based on a trace gas pre-concentration device-isotope ratio mass spectrometer. Background technique [0002] Nitrogen plays an important role in soil nitrogen transformation, especially in the process of denitrification. It is of great significance to detect the amount of nitrogen produced in each stage of soil nitrogen transformation process for the research of soil nitrogen transformation. However, it is difficult to quantitatively measure the nitrogen concentration produced in the denitrification process due to some reasons. First of all, the background value of nitrogen in the atmospheric environment is very high, and it is very difficult to accurately quantitatively measure the trace amount of nitrogen produced in the denitrification process. In addition, because nitrogen is an inert gas, it is difficult to react ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/62G01N1/40
CPCG01N1/40G01N27/62
Inventor 杨帆曹亚澄戴沈艳蔡祖聪张金波王风贺
Owner NANJING NORMAL UNIVERSITY
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