CN109734063B

CN109734063B - A method for preparing a composition with certain properties15N abundance N2Method of O

Info

Publication number: CN109734063B
Application number: CN201811637408.4A
Authority: CN
Inventors: 宫平; 武志杰; 张丽莉; 李东坡; 宋玉超; 薛妍; 武开阔; 杨立杰; 崔亚兰
Original assignee: Institute of Applied Ecology of CAS
Current assignee: Institute of Applied Ecology of CAS
Priority date: 2018-12-29
Filing date: 2018-12-29
Publication date: 2022-02-08
Anticipated expiration: 2038-12-29
Also published as: CN109734063A

Abstract

The invention belongs to the technical field of chemistry, and particularly relates to a method for simply preparing a peptide with definite properties¹⁵N abundance N₂O, a process for producing the same. The invention has simple operation and economic cost, can be carried out in a laboratory, and proposes the use of the method with determination¹⁵Potassium nitrate or sodium nitrate in N abundance as substrate to obtain the potassium nitrate or sodium nitrate with determined abundance¹⁵N₂O gas, can be prepared in specific abundance according to needs¹⁵N₂And (4) O gas. Prepared by the method¹⁵N₂The O gas can be used for the research of nitrogen circulation, the quantitative and qualitative detection is carried out, and the result accuracy and precision are high.

Description

A method for preparing a composition with certain properties15N abundance N2Method of O

Technical Field

The invention belongs to the technical field of chemistry, and particularly relates to a method for simply preparing a peptide with definite properties¹⁵N abundance N₂O, a process for producing the same.

Background

N isotope tracing technology for researching nitrogen circulationOne effective method is that the rate and flux of each process of nitrogen cycle turnover can be better distinguished through a tracing technology, and then the nitrogen cycle turnover can be observed qualitatively and quantitatively. At present N₂The methods for preparing O gas mainly comprise a thermal decomposition method of ammonium nitrate, a contact oxidation method of ammonia and a penicillium janthinillum method, and all the methods have certain limitations, such as potential safety hazards, insufficient synthetic purity, unstable raw materials, complex operation and the like.

And how to prepare the compound quickly, safely and conveniently in a laboratory has determination¹⁵N abundance N₂O gas, which is also a real problem that workers working in this field are urgently required to solve. Through research, trivalent titanium can react with nitrate to generate N₂O gas, which removes impurities (NO and NO) under the action of a strong alkaline substance₂) Finally obtaining N₂And (4) O gas. And of nitrates¹⁵N abundance determines N₂Of O gas¹⁵N abundance, can be selected differently according to need¹⁵N-rich nitrates were prepared.

Disclosure of Invention

The object of the present invention is to provide a method for preparing a liquid crystal display device having a definite preparation¹⁵N abundance N₂O, to facilitate passage through¹⁵The nitrogen cycle is measured by N-isotope tracer method. The invention has simple operation and economic cost, can be carried out in a laboratory, and proposes the use of the method with determination¹⁵The nitrate with determined N abundance is prepared under the action of trivalent titanium¹⁵N abundance N₂O, a process for producing the same.

In order to achieve the purpose, the invention adopts the technical scheme that:

the invention aims to provide a method for simply, conveniently and quickly preparing a polypeptide with determined abundance¹⁵N₂A process comprising the steps of:

20mg of N L^-1K of¹⁵NO₃Or Na¹⁵NO₃The solution is mixed with TiCl with the mass solubility of 20%₃Or Ti₂(SO₄)₃Mixing the two solutions, placing in a glass bottle, covering tightly, shaking lightly, standing at room temperature for 5-12 hr, pumping gas from its upper part, and transferring to another sealed containerSealing in a vacuum glass bottle with KOH or NaOH particles (2-4 particles) at the bottom, standing at room temperature for 24-48 h to obtain¹⁵N₂And (4) O gas.

1) Measuring 20-60ml 20mg N L^-1K¹⁵NO₃Or Na¹⁵NO₃The solution was placed in a 120ml glass bottle with a butyl stopper;

2) preparing a butyl plug and a sealing aluminum ring;

3) to contain K¹⁵NO₃Adding 1-3ml of titanium trichloride or Ti into a glass bottle of the solution₂(SO₄)₃A reagent;

4) immediately covering a butyl plug, and sealing the butyl plug by using a capping machine;

5) slightly shaking to mix;

6) standing for 5-12 hours to allow the reaction to be complete;

7) preparing a 20ml glass bottle with a butyl plug, and adding 2-4 potassium hydroxide or NaOH granules at the bottom;

8) applying a butyl plug on the glass bottle cap in the step 7) and pressing and tightly covering an aluminum ring;

9) vacuumizing the glass bottle in the step 8);

10) extracting headspace gas (mainly N) from the glass bottle of step 6)₂O, and also small amounts of NO and NO₂)20ml, and transferring into the glass bottle in the step 9);

11) standing the glass bottle obtained in the step 10) at room temperature for 24-48 h to obtain¹⁵N₂O。

12) Obtainable by step 11¹⁵N₂Diluting O, and determining the concentration sum on the computer¹⁵The N abundance. Prepared with defined concentration¹⁵N₂The O gas can be diluted and put on a machine to measure the specific concentration, and is used for qualitative and quantitative research of the nitrogen circulation process.

The principle of the invention is as follows: reduction of nitrate ions to NO under the action of trivalent titanium₂NO and N₂O, the latter being purified to N by the action of potassium hydroxide₂And O. To obtain¹⁵N₂Of O¹⁵Abundance of N in selected nitrates¹⁵N abundance was almost uniform (null)A little bit in qi¹⁵N)。

The innovation of the invention is mainly compared with the prior preparation¹⁵N₂Compared with the method of O, the method is safer (pyrolysis of ammonium nitrate, over-high temperature of ammonium nitrate in the heating process and easy explosion), more convenient (simpler operation compared with the denitrification generation method of penicillium), and economic (the selected reagents are all more economic, the required test equipment is conventional equipment, and strains and expensive equipment are not needed) so as to have the advantages of definite determination¹⁵Potassium nitrate or sodium nitrate in N abundance as substrate to obtain the potassium nitrate or sodium nitrate with determined abundance¹⁵N₂O gas, can be prepared in specific abundance according to needs¹⁵N₂And (4) O gas. Prepared by the method¹⁵N₂The O gas can be used for the research of nitrogen circulation, the quantitative and qualitative detection is carried out, and the result accuracy and precision are high.

Drawings

FIG. 1 is a schematic diagram of¹⁵N abundance KNO₃Generation of N₂Of O¹⁵Standard curve of N abundance.

Detailed Description

Reagent preparation

1.K¹⁵NO₃Solution (20mg N L^-1): weighing 136mgK¹⁵NO₃Adding into distilled water, and diluting to 1L.

2. Titanium trichloride solution (20%): 10g of titanium trichloride is weighed into distilled water, and the volume is adjusted to 50 ml.

3. 2-4 potassium hydroxide particles.

Example 1

20ml of 20mg of N L^-1K of¹⁵NO₃The solution was mixed with 1ml of 20% TiCl by mass₃Mixing the solution with 120ml glass bottle with butyl plug, sealing, shaking, standing for more than 5 hr, pumping 20ml gas from its upper part, transferring into another sealed vacuum glass bottle with KOH particles added at bottom, and standing for more than 24 hr to obtain the final product¹⁵N₂And (4) O gas. The abundance of which is substantially the same as that of the selected K¹⁵NO₃The abundance is consistent, but the concentration sum is measured on a computer after dilution¹⁵The N abundance. The test results are as follows:

table 1: is different¹⁵N abundance KNO₃Generation of N₂Of O¹⁵N abundance and N₂Concentration of O

K¹⁵NO₃Is/are as follows¹⁵Abundance of N	N₂Of O¹⁵Abundance of N	N₂O concentration (ppm)
			0	0.36％	615
10	10.08％	596
			50	50.03％	622
90	90.01％	668

Example 2

20ml of 20mg of N L^-1Na of (2)¹⁵NO₃The solution was mixed with 1ml of 20% TiCl₃Mixing the solution with 120ml glass bottle with butyl plug, sealing, shaking, standing for more than 5 hr, pumping 20ml gas from its upper part, transferring to another sealed vacuum bottle with N added at bottomPlacing the aOH particles in a 20ml glass bottle, and standing for more than 24h to obtain the product¹⁵N₂And (4) O gas. The abundance of which is substantially equal to that of the selected Na¹⁵NO₃The abundance is consistent, but the concentration sum is measured on a computer after dilution¹⁵The N abundance.

Example 3

20ml of 20mg of N L^-1K of¹⁵NO₃The solution was mixed with 1ml of 20% Ti₂(SO₄)₃Mixing the solution with 120ml glass bottle with butyl plug, sealing, shaking, standing for more than 5 hr, pumping 20ml gas from its upper part, transferring into another sealed vacuum glass bottle with KOH particles added at bottom, and standing for more than 24 hr to obtain the final product¹⁵N₂And (4) O gas. The abundance of which is substantially the same as that of the selected K¹⁵NO₃The abundance is consistent, but the concentration sum is measured on a computer after dilution¹⁵The N abundance.

Example 4

40ml of 20mg of N L^-1Na of (2)¹⁵NO₃The solution was mixed with 2ml of 20% Ti₂(SO₄)₃Mixing the solution with 120ml glass bottle with butyl plug, sealing, shaking, standing for more than 5 hr, pumping 20ml gas from its upper part, transferring into another sealed vacuum glass bottle with NaOH granules added at bottom, and standing for more than 24 hr to obtain the final product¹⁵N₂And (4) O gas. The abundance of which is substantially equal to that of the selected Na¹⁵NO₃The abundance is consistent, but the concentration sum is measured on a computer after dilution¹⁵The N abundance.

Prepared by the method of measuring on a machine¹⁵N₂O gas concentration and abundance, it was found that when the 15N abundance of the selected reagent was higher, the produced¹⁵N₂O gas¹⁵The higher the N abundance goodness of fit, and¹⁵N₂the concentration of O gas is basically 500-700ppm, the concentration range is enough to meet most of experimental requirements, and the O gas can be diluted as required to prepare the O gas with proper concentration¹⁵N₂And (4) O gas.

Claims

1. A method for preparing a composition with certain properties¹⁵N abundance N₂O method, characterized in thatIn that,

20mg of N L^-1K of¹⁵NO₃Or Na¹⁵NO₃The solution is mixed with TiCl with the mass solubility of 20%₃Or Ti₂(SO₄)₃Mixing the two solutions, placing in a glass bottle, covering tightly, shaking lightly, standing at room temperature for 5-12 hr, pumping gas from its upper part, transferring into another sealed vacuum glass bottle with KOH or NaOH granules added at bottom, and standing at room temperature for 24-48 hr to obtain the final product¹⁵N₂O gas; said K¹⁵NO₃Or Na¹⁵NO₃Is/are as follows¹⁵The N abundance is 50-90.

2. Method according to claim 1, characterized in that it comprises the following steps:

1) measuring 20-60ml 20mg N L^-1 K¹⁵NO₃Or Na¹⁵NO₃Putting the solution in a glass bottle;

2) preparing a butyl plug and a sealing aluminum ring;

5) slightly shaking to mix;

6) standing for 5-12 hours to allow the reaction to be complete;

9) vacuumizing the glass bottle in the step 8);

10) extracting 20ml of upper gas from the glass bottle in the step 6), and transferring the upper gas into the glass bottle in the step 9);

3. According toThe method of claim 1, wherein the prepared solution has a defined concentration¹⁵N₂The O gas can be diluted and put on a machine to measure the specific concentration, and is used for qualitative and quantitative research of the nitrogen circulation process.

4. The method of claim 1,

2-4 particles of KOH or NaOH are added.