Unlock instant, AI-driven research and patent intelligence for your innovation.

Method and device for determining 15N isotope abundance of nitric acid or nitrate

A technology of isotope abundance and nitrate, applied in measuring devices, material analysis by electromagnetic means, instruments, etc., can solve the problems of large sample consumption and high cost, achieve less consumption, improve efficiency, and shorten sample pretreatment the effect of time

Pending Publication Date: 2020-11-24
SHANGHAI RES INST OF CHEM IND
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the amount of samples increases, the test time increases proportionally, and certain optimization is required in the detection of high-throughput samples, and 15 The consumption of N-labeled samples is large, and the relative cost is high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method and device for determining 15N isotope abundance of nitric acid or nitrate
  • Method and device for determining 15N isotope abundance of nitric acid or nitrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] 0.5mol / L nitric acid- 15 N chemical reagent isotope abundance analysis, comprising the following steps:

[0076] (1) Preparation 15 N marks nitrogen

[0077] The reaction equipment used in this embodiment is as figure 1 As shown in the reaction tube 1, the reaction tube 1 can be filled with isotope-labeled samples, oxides and reducing agents. At the same time, the opening end of the reaction tube 1 can be connected with other external equipment. The alkane gas torch is sealed at the position of the sealing section 4 of the reaction tube 1 .

[0078] The sampling tube 2 used in this embodiment is as figure 2 As shown, the reaction tube 1 is placed in the sample tube 2, and the fragile section 3 is inserted into the round hole 8 of the adjustment handle 7 in the sample tube 2, and the sample tube section 5 and the sample tube two Section 6 is connected, and the sampling system of the gas isotope mass spectrometer is connected to section 5 of the sampling tube, and t...

Embodiment 2

[0086] 8mol / L nitric acid- 15 N chemical reagent isotope abundance analysis, comprising the following steps:

[0087] (1) Preparation 15 N marks nitrogen

[0088] Load 50mg calcium oxide, 50mg copper powder, 5μL nitric acid- 15 The N sample is placed in the reaction tube 1, and the vacuum system is connected to the reaction tube 1, and the vacuum degree in the reaction tube 1 is reduced to below 50 Pa through the vacuum system to evacuate, and a butane gas spray gun is used to seal the tube section of the reaction tube 1. 4 positions to seal the tube. Put the sealed reaction tube 1 into a muffle furnace at a high temperature of 650°C for 3 hours to generate 15 N 2 ;

[0089] (2) Instrument parameter setting

[0090] Electron bombardment ion source (EI); scanning range (m / z) is 18-45; ion source temperature is 100°C; electron energy is 70eV; high voltage is 6kV, trap voltage is 100V; the signal receiver is a Faraday cup.

[0091] (3) Calculation of isotope abundance

...

Embodiment 3

[0095] Nitrate in water samples 15 N isotope abundance analysis, including the following steps:

[0096] (1) Pretreatment of water quality samples

[0097] Water quality samples need to add a small amount of magnesium oxide solution to make the pH 7-9. When the nitrate content is lower than 0.1% (volume > 10mL), heat and concentrate at 90°C to about 1mL.

[0098] (2) Preparation 15 N marks nitrogen

[0099] Put 50mg of alumina, 50mg of zinc powder, and 15μL of water quality sample into reaction tube 1 respectively, connect the vacuum system to reaction tube 1, and reduce the vacuum degree in reaction tube 1 to below 50Pa through the vacuum system to evacuate, use The butane gas torch is sealed at the position of the sealing section 4 of the reaction tube 1 .

[0100] Put the sealed reaction tube 1 into a muffle furnace at a high temperature of 750°C for 3 hours to generate 15 N marks nitrogen;

[0101] (3) Instrument parameter setting

[0102] Electron bombardment ion s...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
strengthaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method and a device for determining 15N isotope abundance of nitric acid or a nitrate, and the method comprises the following steps: (1) taking a 15N labeled nitric acid ornitrate sample, an oxide and a reducing agent, putting into a reaction tube, vacuumizing and sealing; (2) heating the reaction tube to react to generate 15N labeled nitrogen; (3) after the reaction tube is cooled to room temperature, putting the reaction tube into a sample injection tube, and then continuing to vacuumize the sample injection tube and a sample injection pipeline of a gas isotope mass spectrometer connected with the sample injection tube; (4) breaking the reaction tube, so that 15N labeled nitrogen in the reaction tube is introduced into the gas isotope mass spectrometer; and (5) detecting and recording the relative strength with the mass numbers of 28, 29 and 30 respectively, and calculating to obtain the abundance of the 15N isotope in the sample. Compared with the prior art, the method has the advantages of simple operation process, low economic cost, high test data accuracy and precision and the like, and the sample pretreatment time can be greatly shortened when thenumber of samples is more than or equal to 5.

Description

technical field [0001] The invention belongs to 15 The technical field of N isotope abundance detection relates to a method for determining nitric acid or nitrate 15 Method and apparatus for N isotopic abundance. Background technique [0002] Nitrogen cycle refers to the material cycle process of the ecosystem in the process of mutual conversion between simple nitrogen and nitrogen-containing compounds in nature. It is an important part of the material and energy cycle of the entire biosphere. Nitrogen enters into The terrestrial ecosystem undergoes transformation process of nitrifying bacteria and denitrifying bacteria in the soil, and then leaves the terrestrial ecosystem through leaching or gas. The nitrogen cycle mainly includes nitrogen fixation, ammonification, nitrification, assimilation and denitrification. These processes cycle back and forth in the ecosystem, resulting in the continuous migration and transformation of nitrogen in the ecosystem composed of the atm...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62
CPCG01N27/62
Inventor 解龙宋明鸣雷雯杜晓宁姜永悦李杰周驰成
Owner SHANGHAI RES INST OF CHEM IND