CN109734063A - A kind of prepare has determination15N abundance N2The method of O - Google Patents

Abstract

The invention belongs to technical field of chemistry, a kind of specifically easily prepare has determination¹⁵N abundance N₂The method of O.Operation of the present invention is simple, cost economy, can carry out in laboratory, proposes using with determination¹⁵The potassium nitrate or sodium nitrate of N abundance are substrate, and obtaining has determining abundance¹⁵N₂O gas can prepare specific abundance as needed¹⁵N₂O gas.Using made from the method¹⁵N₂O gas can be used for the research of nitrogen cycle, carry out detection qualitatively and quantitatively, and result precision and accuracy are high.

Description

A kind of prepare has determination15N abundance N2The method of O

Technical field

The invention belongs to technical field of chemistry, a kind of specifically easily prepare has determination¹⁵N abundance N₂The side of O Method.

Background technique

N isotope tracer technique is to study one of the effective ways of Nitrogen Cycling, and by tracer technique, we can be more preferable The rate and flux of each process of nitrogen cycle turnover are distinguished in ground, and then can qualitatively and quantitatively observe the turnover of nitrogen cycle. N at present₂The preparation method of O gas mainly has the thermal decomposition method of ammonium nitrate, the contact oxidation method of ammonia and penicillium janthinellum method, above Method all has certain limitation, such as security risk, the problems such as synthesis purity is inadequate, raw material are unstable, complicated for operation.

And it how quickly, safely, conveniently to prepare to have in laboratory and determine¹⁵N abundance N₂O gas, this is also to be engaged in The staff in field practical problem urgently to be solved.Through studying, titanous can generate N with nitrate reaction₂O gas, after Person removes impurity (NO and NO under the action of highly basic substance₂), finally obtain N₂O gas.And nitrate¹⁵N abundance determines N₂O gas¹⁵N abundance can select difference on demand¹⁵It is prepared by the nitrate of N abundance.

Summary of the invention

The purpose of the present invention is to provide a kind of prepare to have determination¹⁵N abundance N₂The method of O, to promote to pass through¹⁵The same position N Plain trace method measures nitrogen cycle.Operation of the present invention is simple, cost economy, can carry out in laboratory, proposes using with determination¹⁵For the nitrate of N abundance under the action of titanous, being made has determination¹⁵N abundance N₂The method of O.

To achieve the above object, the technical solution adopted by the present invention are as follows:

The invention reside in provide the simple and efficient preparation of one kind to have determining abundance¹⁵N₂O method, the method includes following Step:

By 20mg N L^-1K¹⁵NO₃Or Na¹⁵NO₃The TiCl that solution and quality solubility are 20%₃Or Ti₂(SO₄)₃Two molten Liquid mixes in vial, covers tightly compression jog, be stored at room temperature 5-12h, extracts gas transfer in another sealing from upper part Vacuum bottoms have added in the vial of KOH or NaOH particle (2-4), stand at room temperature for 24 hours -48h to get¹⁵N₂O gas.

1) 20-60ml 20mg N L is measured^-1K¹⁵NO₃Or Na¹⁵NO₃Solution is in the 120ml vial with butyl plug；

2) butyl plug and sealing aluminium circle are got out；

3) Xiang Shengyou K¹⁵NO₃The titanium trichloride or Ti of 1-3ml are added in the vial of solution₂(SO₄)₃Reagent；

4) butyl plug is covered at once, and it is sealed with capping machine；

5) gentle agitation makes its mixing；

6) 5-12 hours are stood, allows its fully reacting；

7) prepare the 20ml vial with butyl plug, potassium hydroxide or NaOH particle 2-4 is added in bottom；

8) butyl plug on the glass cap of step 7) and press aluminium circle is covered tightly；

9) vial of step 8) is vacuumized；

10) upper gas (mainly N is extracted from the vial of step 6)₂O, there are also a small amount of NO and NO₂) 20ml, turn It moves into the vial in step 9)；

11) vial of step 10) stands -48h for 24 hours at room temperature, obtains¹⁵N₂O。

It 12) can be to made from step 11¹⁵N₂O is diluted, and upper machine measure its concentration and¹⁵N abundance.Prepared has Determine concentration¹⁵N₂O gas can dilute machine and determine specific concentration, the qualitative and quantitative study for nitrogen cycle process.

The principle of the invention are as follows: nitrate ion is reduced to NO under the action of titanous₂, NO and N₂O, the latter is in hydroxide Purification is N under the action of potassium₂O.And it is made¹⁵N₂O's¹⁵In N abundance and selected nitrate¹⁵N abundance is almost unanimously (in air Have a little¹⁵N)。

Innovation of the invention mainly and existing preparation¹⁵N₂The method of O is compared, safer (ammonium nitrate pyrolysismethod, The ammonium nitrate excessively high explosive of temperature during heating), convenient (comparing Penicillium notatum denitrification method of formation, more simple operations), warp It helps (selected reagent is relatively inexpensive, and required test equipment is conventional equipment, without strain and high equipment), to have It determines¹⁵The potassium nitrate or sodium nitrate of N abundance are substrate, and obtaining has determining abundance¹⁵N₂O gas can prepare tool as needed Body abundance¹⁵N₂O gas.Using made from the method¹⁵N₂O gas can be used for the research of nitrogen cycle, carry out inspection qualitatively and quantitatively It surveys, result precision and accuracy are high.

Detailed description of the invention

Fig. 1 is difference¹⁵N abundance KNO₃The N of generation₂O's¹⁵The standard curve of N abundance.

Specific embodiment

Preparation of reagents

1.K¹⁵NO₃Solution (20mg N L^-1): weigh 136mgK¹⁵NO₃In distilled water, it is settled to 1L.

2. titanium trichloride solution (20%): weighing 10g titanium trichloride in distilled water, be settled to 50ml.

3. potassium hydroxide pellet, 2-4.

Embodiment 1

By 20ml 20mg N L^-1K¹⁵NO₃The TiCl that the mass concentration of solution and 1ml are 20%₃Solution, mix in In the vial with butyl plug of 120ml, cover tightly compression jog, stand 5h or more, from upper part extract the transfer of 20ml gas in Another sealing Vacuum bottoms has added in the 20ml vial of KOH particle, stand it is above for 24 hours to get¹⁵N₂O gas.Its abundance base Sheet and selected K¹⁵NO₃Abundance is consistent, but after need to diluting upper machine measure its concentration and¹⁵N abundance.Test result is as follows:

Table 1: different¹⁵N abundance KNO₃The N of generation₂O's¹⁵N abundance and N₂O concentration

K15NO3's15N abundance	N2O's15N abundance	N2O concentration (ppm)
			0	0.36%	615
10	10.08%	596
			50	50.03%	622
90	90.01%	668

Embodiment 2

By 20ml 20mg N L^-1Na¹⁵NO₃The TiCl of solution and 1ml 20%₃Solution mixes the band butyl in 120ml In the vial of plug, compression jog is covered tightly, stands 5h or more, the transfer of 20ml gas is extracted from upper part and seals vacuum in another Bottom has added in the 20ml vial of NaOH particle, stand it is above for 24 hours to get¹⁵N₂O gas.Its abundance substantially with it is selected Na¹⁵NO₃Abundance is consistent, but after need to diluting upper machine measure its concentration and¹⁵N abundance.

Embodiment 3

By 20ml 20mg N L^-1K¹⁵NO₃The Ti of solution and 1ml 20%₂(SO₄)₃Solution is mixed in the band fourth of 120ml In the vial of base plug, compression jog is covered tightly, stands 5h or more, it is true in another sealing to extract the transfer of 20ml gas from upper part Empty bottom has added in the 20ml vial of KOH particle, stand it is above for 24 hours to get¹⁵N₂O gas.Its abundance substantially with it is selected K¹⁵NO₃Abundance is consistent, but after need to diluting upper machine measure its concentration and¹⁵N abundance.

Embodiment 4

By 40ml 20mg N L^-1Na¹⁵NO₃The Ti of solution and 2ml 20%₂(SO₄)₃Solution is mixed in the band of 120ml In the vial of butyl plug, compression jog is covered tightly, stands 5h or more, extracts the transfer of 20ml gas in another sealing from upper part Vacuum bottoms have added in the 20ml vial of NaOH particle, stand it is above for 24 hours to get¹⁵N₂O gas.Its abundance substantially with it is selected Na¹⁵NO₃Abundance is consistent, but after need to diluting upper machine measure its concentration and¹⁵N abundance.

It is measured made from this law as upper machine¹⁵N₂O gas concentration and abundance, discovery is higher when the 15N abundance of selected reagent, Made¹⁵N₂O gas¹⁵The N abundance goodness of fit is higher, and¹⁵N₂O gas concentration is substantially in 500-700ppm, this concentration range foot To meet most of test needs, can be diluted on demand, and then suitable concentration is made¹⁵N₂O gas.

Claims (3)

1. a kind of prepare has determination¹⁵N abundance N₂The method of O, which is characterized in that

By 20mg N L^-1K¹⁵NO₃Or Na¹⁵NO₃The TiCl that solution and quality solubility are 20%₃Or Ti₂(SO₄)₃Two solution, It mixes in vial, covers tightly compression jog, be stored at room temperature 5-12h, it is true in another sealing to extract gas transfer from upper part Empty bottom has added in the vial of KOH or NaOH particle (2-4), stand at room temperature for 24 hours -48h to get¹⁵N₂O gas.

2. the method according to claim 1, wherein described method includes following steps:

1) 20-60ml 20mg N L is measured^-1K¹⁵NO₃Or Na¹⁵NO₃Solution is in vial；

2) butyl plug and sealing aluminium circle are got out；

3) Xiang Shengyou K¹⁵NO₃The titanium trichloride or Ti of 1-3ml are added in the vial of solution₂(SO₄)₃Reagent；

4) butyl plug is covered at once, and it is sealed with capping machine；

5) gentle agitation makes its mixing；

6) 5-12 hours are stood, allows its fully reacting；

7) prepare the 20ml vial with butyl plug, potassium hydroxide or NaOH particle 2-4 is added in bottom；

8) butyl plug on the glass cap of step 7) and press aluminium circle is covered tightly；

9) vial of step 8) is vacuumized；

10) upper gas (mainly N is extracted from the vial of step 6)₂O, there are also a small amount of NO and NO₂) 20ml, it is transferred to In vial in step 9)；

11) vial of step 10) stands -48h for 24 hours at room temperature, obtains¹⁵N₂O。

3. the method according to claim 1, wherein prepared having determines concentration¹⁵N₂O gas can be dilute The machine of releasing determines specific concentration, the qualitative and quantitative study for nitrogen cycle process.