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Pre-treatment method of nitrate nitrogen oxygen isotope sample analysis

An oxygen isotope and sample analysis technology, which is applied in the preparation of test samples, analysis materials, material separation, etc., can solve the problems of complex operation process, low conversion efficiency, unstable reaction, etc., and achieve low price and complete solid-liquid separation , the effect of saving operation time

Active Publication Date: 2018-11-30
成都栢晖生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The purpose of the present invention is to provide a pretreatment method for the analysis of nitrate nitrogen and oxygen isotope samples, which solves the problem that the existing pretreatment methods for the analysis of nitrate nitrogen and oxygen isotope samples have relatively complicated operation process, low conversion efficiency and narrow application range. Unstable reaction, complicated mechanism, etc.

Method used

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Examples

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Comparison scheme
Effect test

Embodiment 1

[0040] A kind of pretreatment method of nitrate nitrogen oxygen isotope sample analysis described in the present embodiment comprises the following steps:

[0041] Step 1. Sample dilution: Dilute batches of samples separately, each batch includes at least 40 samples, including 3 standards, 2 quality controls, 1 blank and at least 34 actual samples. Specifically, first use 0.2 ~0.7mol / L sodium chloride solution to dilute each sample separately, so that the NO in the sample 3 - -N decreased to 15-25μmol / L, and ensured that the diluted volume of each sample was above 40ml;

[0042] Step 2, pH value adjustment: adjust the pH value of the diluted sample solution to 6.0-8.0, specifically, add a few drops of 0.5-1.0mol / L HCl to reduce the pH value of the solution to 2-3.0, and then add 1.0 ~2.0mol / L imidazole can increase the pH value to 6.0~8.0;

[0043] Step 3, metal reduction: Add reducing metal to the sample solution that has completed the pH value adjustment in step 2. The re...

Embodiment 2

[0048]The traditional method of dilution and pH value adjustment is to first test the initial concentration of the solution, then add the diluent (usually water), then measure the diluted concentration, and then add the diluent, and repeat this many times until the required pH value is obtained. Dilution concentration, or close to the required dilution concentration; in the same way, first measure the initial pH value of the solution, then add the adjustment solution, measure the pH value at this time, then add the adjustment solution, repeat several times, until the desired pH is obtained In the process of diluting and adjusting the pH value, constant oscillation and testing are required. Such artificial efficiency is very low, which seriously affects the progress of the experiment, and even the timeliness of the experiment and the accuracy and reliability of the experimental results. For this reason, on the basis of Example 1, in order to improve the pretreatment efficiency o...

Embodiment 3

[0051] On the basis of Example 2, this embodiment creatively changes the reducing metal in step 3 from copper-plated cadmium grains to iron sheets, and curls the iron sheets into a cylindrical shape. The outer surface of the cylindrical iron sheet The diameter is smaller than the inner diameter of the test tube containing the sample. When the traditional method uses copper-plated cadmium grains as the reduction metal, because the copper-plated cadmium grains are expensive, generally only a few grains (5-10 grains) are used, resulting in a limited contact surface between the copper-plated cadmium grains and the solution, and the reduction reaction is slow and ineffective. However, compared with the traditional copper-plated cadmium particles, the iron sheet of this embodiment has a much larger contact surface with the solution, and the reaction is more sufficient, which can make the NO 3 - more fully reduced to NO 2 - , and the reaction of the iron sheet is more stable than ...

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Abstract

The invention discloses a pre-treatment method of nitrate nitrogen oxygen isotope sample analysis. The pre-treatment method comprises following steps: 1, sample dilution, wherein samples from one batch are diluted respectively, and the volume of the samples after dilution is maintained to be 40ml or more; 2, pH adjusting, wherein the pH values of the diluted sample solutions are adjusted to 6.0 to8.0; 3, metal reduction, wherein a reductive metal is introduced into the diluted sample solutions after pH adjusting in step 2 so as to obtain solution A, the solution A is introduced into headspacebottles, and the headspace bottles are sealed with covers; and 4, chemical conversion, wherein an acetic acid solution and a NaN3 solution are mixed so as to obtain a solution B, the solution B is introduced into the headspace bottles containing the solution A, full vibration of the headspace bottles is carried out, and N2O gas obtained in the headspace bottles is introduced into a gas mass spectrometer for nitrogen oxygen isotope ratio measuring. The pre-treatment method is capable of simplifying operation process, increasing conversion rate, enlarging suitable range, and stabilizing reaction.

Description

technical field [0001] The invention belongs to the field of stable isotope determination, and in particular relates to a pretreatment method for analyzing nitrate nitrogen and oxygen isotope samples. Background technique [0002] Nitrogen is an essential element for life on earth and one of the core elements for life metabolism. In agriculture, nitrogen is both a yield-enhancing factor and a major limiting factor of soil productivity. The development and agricultural application of nitrogen fertilizer industry in the 19th century increased crop yields and played an extremely important role in ensuring food supply and world population growth. However, at the same time, excessive agricultural nitrogen fertilizer input also led to a large amount of active nitrogen entering The environment strongly interferes with the biogeochemical cycle of nitrogen. It is estimated that the amount of reactive nitrogen entering the biosphere due to human activities increased from 15Tg in 186...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/88G01N1/38
CPCG01N1/38G01N30/02G01N30/7206G01N30/88G01N2030/025G01N2030/8868
Inventor 李娜周星梅王曦陈建中
Owner 成都栢晖生物科技有限公司
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