CN112763450A - Method for simultaneously determining concentrations of aluminum nitrate and nitric acid in aqueous solution - Google Patents
Method for simultaneously determining concentrations of aluminum nitrate and nitric acid in aqueous solution Download PDFInfo
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- CN112763450A CN112763450A CN202011463707.8A CN202011463707A CN112763450A CN 112763450 A CN112763450 A CN 112763450A CN 202011463707 A CN202011463707 A CN 202011463707A CN 112763450 A CN112763450 A CN 112763450A
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 55
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 30
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 18
- 238000002835 absorbance Methods 0.000 claims abstract description 13
- 238000012937 correction Methods 0.000 claims abstract description 9
- 239000002915 spent fuel radioactive waste Substances 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 4
- 238000010238 partial least squares regression Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000002901 radioactive waste Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000004497 NIR spectroscopy Methods 0.000 description 1
- PZBHVYWEEVVAKK-UHFFFAOYSA-N [Al+3].O[N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound [Al+3].O[N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PZBHVYWEEVVAKK-UHFFFAOYSA-N 0.000 description 1
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- -1 aluminum ions Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to the technical field of chemical analysis, and relates to a method for simultaneously determining the concentrations of aluminum nitrate and nitric acid in an aqueous solution. The method comprises the following steps: (1) preparing a series of aluminum nitrate solutions and nitric acid solutions with known concentrations; (2) respectively measuring the near infrared absorption spectra of the aluminum nitrate solution and the nitric acid solution with known concentrations; (3) selecting a proper wavelength, and establishing a quantitative correction relation between the aluminum nitrate concentration and the corresponding absorbance of aluminum nitrate solutions with different known concentrations under the wavelength by applying chemometrics software; (4) selecting proper wavelength, and establishing a quantitative correction relation between the nitric acid concentration and the corresponding absorbance of nitric acid solutions with different known concentrations under the wavelength; (5) measuring the near infrared absorption spectrum of the sample; (6) and calculating the concentration of the sample. The method for simultaneously measuring the concentrations of the aluminum nitrate and the nitric acid in the aqueous solution can be used for quickly, accurately and efficiently measuring the concentrations of the aluminum nitrate and the nitric acid in the aqueous solution simultaneously.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and relates to a method for simultaneously determining the concentrations of aluminum nitrate and nitric acid in an aqueous solution.
Background
In some special spent fuel reprocessing process research and plant operations, it is common to perform the corresponding process operations after the aluminum matrix is dissolved by nitric acid. During this entire process, the concentration of nitric acid and the concentration of aluminum nitrate need to be measured. Because the sample coexists actinide and aluminum ions and is easy to hydrolyze, the metal ions need to be masked to prevent the hydrolysis of the metal ions from causing measurement errors when the nitric acid concentration is measured; when the aluminum concentration is analyzed, a color developing agent and a complexing agent are required to be added, and if ICP-AES is adopted for measurement, the influence of other interfering ions is required to be removed in advance; for high concentration samples, a dilution operation is also required. In addition, the addition of masking agents and titrants also increases the type and volume of radioactive waste liquid, and puts pressure on the subsequent waste liquid treatment. These all increase the difficulty of handling. Therefore, there is a real need and a practical significance to develop a method for directly and rapidly measuring the concentrations of aluminum nitrate and nitric acid in an aqueous solution at the same time.
Disclosure of Invention
The invention aims to provide a method for simultaneously measuring the concentrations of aluminum nitrate and nitric acid in an aqueous solution, so that the concentrations of the aluminum nitrate and the nitric acid in the aqueous solution can be rapidly, accurately and efficiently measured simultaneously.
To achieve this object, in a basic embodiment, the present invention provides a method for simultaneously determining the concentrations of aluminum nitrate and nitric acid in an aqueous solution, said method comprising the steps of:
(1) preparing a series of aluminum nitrate solutions and nitric acid solutions with known concentrations;
(2) respectively measuring the near infrared absorption spectra of the aluminum nitrate solution and the nitric acid solution with known concentrations;
(3) selecting a proper wavelength, and establishing a quantitative correction relation (partial least squares regression model) between the aluminum nitrate concentration and the corresponding absorbance of the aluminum nitrate solution with different known concentrations under the wavelength by applying chemometrics software;
(4) selecting proper wavelength, and establishing a quantitative correction relation (partial least squares regression model) between the nitric acid concentration and the corresponding absorbance of the nitric acid solution with different known concentrations under the wavelength by applying chemometrics software;
(5) measuring the near infrared absorption spectrum of the sample;
(6) and (3) calculating the concentration of the sample: and (3) respectively substituting absorbance values of the aluminum nitrate and the nitric acid, which are measured by the near-infrared absorption spectrum of the sample under the same wavelength, into the quantitative correction relationship (partial least squares regression model) obtained in the steps (3) and (4), and respectively calculating the concentrations of the aluminum nitrate and the nitric acid in the sample.
In a preferred embodiment, the present invention provides a method for simultaneously measuring the concentrations of aluminum nitrate and nitric acid in an aqueous solution, wherein in step (1), the concentration of the aluminum nitrate solution of known concentration ranges from 0.2 to 2.7mol/L and the concentration of the nitric acid solution of known concentration ranges from 0.5 to 6 mol/L.
In a preferred embodiment, the present invention provides a method for simultaneously determining the concentrations of aluminum nitrate and nitric acid in an aqueous solution, wherein in step (2), the wavelength range of the near-infrared absorption spectrum is 1000-2500 nm.
In a preferred embodiment, the present invention provides a method for simultaneously determining the concentrations of aluminum nitrate and nitric acid in an aqueous solution, wherein in step (3), the suitable wavelength is 1570-1850 nm.
In a preferred embodiment, the present invention provides a method for simultaneously determining the concentrations of aluminum nitrate and nitric acid in an aqueous solution, wherein in step (4), the suitable wavelength is 1570-1850 nm.
In a preferred embodiment, the present invention provides a method for simultaneously determining the concentrations of aluminum nitrate and nitric acid in an aqueous solution produced during the post-treatment of spent fuel.
The method for simultaneously measuring the concentrations of the aluminum nitrate and the nitric acid in the aqueous solution has the beneficial effects that the method for simultaneously measuring the concentrations of the aluminum nitrate and the nitric acid in the aqueous solution can be used for quickly, accurately and efficiently simultaneously measuring the concentrations of the aluminum nitrate and the nitric acid in the aqueous solution.
The method can realize the simultaneous determination of the concentrations of the aluminum nitrate and the nitric acid in the radioactive sample, solves the problem of mutual interference influence of the aluminum nitrate and the nitric acid in the process of determining the concentrations of the aluminum nitrate and the nitric acid by using a near infrared spectroscopy, can obviously reduce the volume of the radioactive waste liquid, and improves the analysis efficiency.
Drawings
FIG. 1 is a graph showing the near infrared absorption spectra of aluminum nitrate solutions of different concentrations.
FIG. 2 is a graph showing the near infrared absorption spectra of nitric acid solutions of different concentrations.
FIG. 3 is a graph showing the correlation between a reference value of nitric acid concentration and a measured value.
FIG. 4 is a graph showing the correlation between a reference value and a measured value of the aluminum nitrate concentration.
Detailed Description
The following description will further describe embodiments of the present invention with reference to the accompanying drawings.
Example 1: calibration model establishment
A series of samples of mixed aluminum nitrate solution with known concentration and nitric acid solution with known concentration were prepared, and the compositions of the samples are shown in table 1. And the near infrared absorption spectrum (1000-.
TABLE 1 composition of the mixed samples
In the determination of the near infrared absorption spectrum, air is used as reference, the resolution and the accumulated times of the instrument are set, a quartz cuvette is used as a measuring cell, and the following similar principle is adopted. The obtained near-infrared absorption spectra of the aluminum nitrate solutions with different concentrations are shown in fig. 1 (as can be seen from fig. 1, the absorbance gradually increases with the increase of the wavelength within a certain wavelength range and shows a certain correlation and can be used for quantitative analysis) and the obtained near-infrared absorption spectra of the nitric acid solutions with different concentrations are shown in fig. 2 (as can be seen from fig. 2, the absorbance gradually increases with the increase of the wavelength within a certain wavelength range and shows a certain correlation and can be used for quantitative analysis).
Selecting a proper wavelength (1570-1850nm), and applying chemometrics software to establish a quantitative calibration model between the aluminum nitrate concentration and the corresponding absorbance of the prepared aluminum nitrate solutions with different known concentrations at the wavelength.
Selecting a proper wavelength (1570-1850nm), and applying chemometrics software to establish a quantitative calibration model between the nitric acid concentration and the corresponding absorbance of the prepared nitric acid solutions with different known concentrations at the wavelength.
Example 2: sample assay
The near-infrared absorption spectra of a series of aqueous solution samples in which the concentrations of aluminum nitrate and nitric acid are known are measured under the same spectral measurement conditions, and the absorbance values of the aluminum nitrate and the nitric acid measured by the near-infrared absorption spectra of the samples under the same wavelength are respectively substituted into the quantitative correction relationship (partial least squares regression model) obtained in example 1, and the concentrations of the aluminum nitrate and the nitric acid in the aqueous solution samples are respectively calculated. The correlation graphs shown in fig. 3 and 4 are obtained by comprehensively analyzing the measurement values of the calculation results and the known concentration reference values, respectively. As can be seen from FIG. 3, the method of the present invention has a good correlation between the measured nitric acid concentration and the reference value, and the correlation coefficient of the sample in the verification set is 0.9997. As can be seen from FIG. 4, the measured aluminum nitrate concentration values of the samples have good correlation with the reference value by applying the method of the present invention, and the correlation coefficient of the verification set samples is 0.9997.
The established calibration model was used to calibrate the results of the above-described nitric acid-aluminum nitrate aqueous solution samples, and the results are shown in table 2 below.
TABLE 2 sample concentration calibration results
As can be seen from the results of table 2, the established analytical method enables accurate determination of the concentrations of nitric acid and aluminum nitrate in the sample.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations. The foregoing examples or embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.
Claims (6)
1. A method for simultaneously measuring the concentrations of aluminum nitrate and nitric acid in an aqueous solution is characterized by comprising the following steps:
(1) preparing a series of aluminum nitrate solutions and nitric acid solutions with known concentrations;
(2) respectively measuring the near infrared absorption spectra of the aluminum nitrate solution and the nitric acid solution with known concentrations;
(3) selecting a proper wavelength, and establishing a quantitative correction relation between the aluminum nitrate concentration and the corresponding absorbance of aluminum nitrate solutions with different known concentrations under the wavelength by applying chemometrics software;
(4) selecting proper wavelength, and establishing a quantitative correction relation between the nitric acid concentration and the corresponding absorbance of the nitric acid solution with different known concentrations under the wavelength by applying chemometrics software;
(5) measuring the near infrared absorption spectrum of the sample;
(6) and (3) calculating the concentration of the sample: and (4) respectively substituting absorbance values of the aluminum nitrate and the nitric acid, which are measured by the near-infrared absorption spectrum of the sample under the same wavelength, into the quantitative correction relationship obtained in the steps (3) and (4), and respectively calculating the concentrations of the aluminum nitrate and the nitric acid in the sample.
2. The method of claim 1, wherein: in the step (1), the concentration range of the aluminum nitrate solution with the known concentration is 0.2-2.7mol/L, and the concentration range of the nitric acid solution with the known concentration is 0.5-6 mol/L.
3. The method of claim 1, wherein: in the step (2), the wavelength range of the near infrared absorption spectrum is 1000-2500 nm.
4. The method of claim 1, wherein: in the step (3), the suitable wavelength is 1570-1850 nm.
5. The method of claim 1, wherein: in the step (4), the suitable wavelength is 1570-1850 nm.
6. The method according to one of claims 1 to 5, characterized in that: the aqueous solution is an aqueous solution containing aluminum nitrate and nitric acid generated in the post-treatment process of the spent fuel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011463707.8A CN112763450A (en) | 2020-12-14 | 2020-12-14 | Method for simultaneously determining concentrations of aluminum nitrate and nitric acid in aqueous solution |
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| CN202011463707.8A CN112763450A (en) | 2020-12-14 | 2020-12-14 | Method for simultaneously determining concentrations of aluminum nitrate and nitric acid in aqueous solution |
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|---|---|---|---|---|
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2020
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Application publication date: 20210507 |