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Method for detecting content of nitrate radicals in high-level liquid waste

A measurement method and high-level waste liquid technology, applied in the field of analytical chemistry, can solve problems such as increasing operational complexity, and achieve the effect of fast measurement speed and high selectivity

Inactive Publication Date: 2018-09-07
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, additional admixtures will increase the complexity of the operation, especially for high-radioactive samples, so it is best to choose the signal of the solution itself as the internal standard signal

Method used

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  • Method for detecting content of nitrate radicals in high-level liquid waste
  • Method for detecting content of nitrate radicals in high-level liquid waste
  • Method for detecting content of nitrate radicals in high-level liquid waste

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: the Raman spectrum measurement of different concentration nitric acid and sodium nitrate solution

[0025] Nitrate and nitric acid solutions are the main components of high-level radioactive waste, so a series of different concentrations of nitric acid solutions and sodium nitrate solutions were prepared as standard solutions, and the Raman spectra were measured respectively. The results are as follows figure 1 and figure 2 shown.

[0026] From figure 1 and figure 2 It can be seen that the nitrate is at 1047cm -1 has a characteristic signal; but with figure 2 compared to, figure 1 Medium H + When the concentration increases from 0.10mol / L to 1.50mol / L, the peak shape of water changes, and the change of its intensity is determined by H + The peak shape of nitrate is sharp due to the change of concentration, and its intensity increases with the increase of concentration.

[0027] Based on this result, it is necessary to select the best preprocessi...

Embodiment 2

[0028] Embodiment 2: water combination peak area normalization processing and working curve drawing (water combination peak area normalization method)

[0029] Use the normalization function in the built-in software of the Renishaw confocal Raman spectrometer-Integratedsignal, with water at 2800-3800cm -1 The combined peak area of ​​the range is the normalization standard, and the Raman spectrum data of different concentrations of nitric acid are processed to obtain the normalized NO 3 - Peak area values, plotted for the NO 3 - The working curve between the peak area value and its concentration is shown in image 3 .

[0030] Depend on image 3 Visible, when the solution H + When the concentration is in the range of 0.10-1.80mol / L, the combined peak area of ​​water can be used as the normalization standard for NO 3 - For quantitative analysis, NO 3 - There is a good linear relationship between the peak area value and its concentration, that is, within this concentrat...

Embodiment 3

[0031] Embodiment 3: the normalization processing of the highest point of the water combination peak and the drawing of the working curve (normalization method of the highest point of the water combination peak)

[0032] After subtracting the baseline from the Raman spectrum of the nitric acid aqueous solution, read the value of the highest point of the combined peak of water, and the NO 3 - The peak height is compared with this value, obtains the peak height ratio, draws the peak height ratio with the nitric acid concentration change relation curve, is shown in Figure 4 . From Figure 4 It can be seen that when the solution H + When the concentration is in the range of 0.10-1.80mol / L, it is feasible to use the highest point of the water combination peak as the internal standard, and the established working curve R 2 = 0.999.

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Abstract

The invention belongs to the technical field of analytical chemistry, and relates to a method for detecting the content of nitrate radicals in high-level liquid waste. The detection method comprises the following steps: (1) detecting the Raman spectra of standard solutions containing different concentrations of nitrate radicals, and drawing a working curve of the peak area or the peak height and concentration relationship of the nitrate radicals at 1047 cm<-1>; (2) detecting the Raman spectrum diagram of the high-level liquid waste to obtain the peak area or the peak height at 1047 cm<-1>; (3)calculating the content of the nitrate radicals in the high-level liquid waste according to the peak area or the peak height of the sample at 1047 cm<-1> and the working curve. The detection method can be used to accurately detect the content of the nitrate radicals simply and rapidly without the interference of interfering substances in the high-level liquid waste.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry and relates to a method for determining the content of nitrate in high-level radioactive waste liquid. Background technique [0002] With the development of the nuclear industry, more and more high-level waste liquids are produced in reprocessing plants, and their radioactive specific activities are high (greater than 10 12 Bq / L), high toxicity and high corrosiveness, it is not suitable for long-term storage, and needs to be solidified in time and disposed of in deep geological conditions. The prerequisite for carrying out research on the solidification treatment of high-level radioactive liquid waste is to conduct a full analysis of the chemical composition and radionuclides of high-level radioactive waste liquid, and to obtain complete and accurate source term data. Nitrate is the main chemical component in high-level waste liquid, and its content affects the curing process; and wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/65
Inventor 张倩慈朱海巧柳倩田国新
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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