CN109632979B - Hydroxylamine analysis method in the coexistence of aminohydroxyurea - Google Patents
Hydroxylamine analysis method in the coexistence of aminohydroxyurea Download PDFInfo
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Abstract
The invention discloses a hydroxylamine analysis method when aminohydroxyurea coexists, which comprises the steps of neutralizing and diluting an aminohydroxyurea coexisting sample to be detected, putting the sample into a volumetric flask, adding a nitrobenzaldehyde solution, fixing the volume by using an acetic acid solution, shaking up, and standing at room temperature; and then, analyzing the sample to be detected by using a method of combining a high performance liquid chromatography column and an ultraviolet detector to obtain the peak area of hydroxylamine in the sample to be detected, and calculating to obtain the concentration of hydroxylamine in the sample to be detected by using a standard working curve of hydroxylamine. The minimum detection concentration of hydroxylamine can reach 2 x 10‑7mol/L, the relative standard deviation of the analytical method of this example is 0.8%. The method for analyzing hydroxylamine by establishing the chemical derivatization-liquid chromatography has the advantages that the hydroxylamine analysis is not influenced by the amino hydroxyurea, the operation is simple, the sensitivity is high, and the repeatability is good.
Description
Technical Field
The invention relates to a hydroxylamine analysis method, in particular to a hydroxylamine analysis method by liquid chromatography, which is applied to the technical field of analytical chemistry.
Background
China is vigorously developing nuclear power, and the rapid development of the nuclear power inevitably generates a large amount of spent fuel, namely used nuclear fuel. These nuclear fuels are very radioactive and pose a significant environmental and ecological threat if left untreated. If the spent fuel is subjected to post-treatment, not only can the unused nuclear fuel uranium-235 and newly generated nuclear fuel plutonium-239 be recycled, but also the volume of the radioactive nuclear waste can be greatly reduced, thereby being beneficial to the final disposal of the radioactive waste. The aminohydroxyurea is a novel salt-free reducing agent for separating uranium from plutonium and in spent fuel reprocessing, the uranium is separated from the plutonium and in a nitric acid solution, the radiation of a feed liquid is strong, under the condition, the aminohydroxyurea can be decomposed to generate hydroxylamine, the hydroxylamine can influence the normal operation of the spent fuel reprocessing process, so that the concentration of the hydroxylamine generated by decomposing the aminohydroxyurea must be researched, and the concentration analysis of the hydroxylamine is involved. The hydroxylamine analysis method reported in the literature mainly utilizes the reducibility of hydroxylamine to react with an oxidizing agent to generate a colored substance, and then uses a spectrophotometric method for analysis. Since aminohydroxyurea is also a reducing agent and also reacts with the oxidizing agent, it interferes with the accurate analysis of hydroxylamine. To date, no literature has reported methods for hydroxylamine analysis in the presence of aminohydroxyureas.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects of the prior art and provide a hydroxylamine analysis method in the coexistence of amino hydroxyurea, wherein a chemical derivatization method and a liquid chromatography method are adopted to analyze hydroxylamine, so that the analysis of hydroxylamine is not influenced by amino hydroxyurea, and the method has the advantages of simple operation, high sensitivity and good repeatability.
In order to achieve the purpose, the invention adopts the following technical scheme:
a hydroxylamine analysis method in the coexistence of amino hydroxyurea adopts a chemical derivation method and a liquid chromatography method to analyze hydroxylamine, and comprises the following steps:
a. drawing a standard working curve of hydroxylamine:
taking a series of volumetric flasks with the same volume, respectively adding 1.0ml of aminohydroxyurea solution with known concentration according to the solvent addition calculated according to the volume ratio, respectively and correspondingly adding hydroxylamine standard solutions with different volumes, and shaking up; then respectively adding 1.0ml of color-developing agent nitrobenzaldehyde solution with known concentration, using acetic acid solution with known concentration to make constant volume, uniformly shaking so as to obtain the hydroxylamine containing amino hydroxyurea whose concentration is (0.4-200.0) × 10-6A series of hydroxylamine standard solutions in mol/L; then standing at room temperature for at least 100min to obtain standardA sample; then, analyzing the series of hydroxylamine standard solutions by using a liquid chromatography method to obtain the hydroxylamine peak area in each standard sample, and drawing by using the hydroxylamine concentration as a horizontal coordinate and the hydroxylamine peak area as a vertical coordinate to obtain a standard working curve of hydroxylamine;
b. taking a sample to be tested for analysis, thereby obtaining the concentration of hydroxylamine in the sample:
neutralizing and diluting the aminohydroxyurea coexistence solution to be detected to obtain a sample to be detected, putting 1.0ml of the sample to be detected into a volumetric flask, adding 1.0ml of a color reagent nitrobenzaldehyde solution with the same concentration as that used in the step a, and carrying out constant volume and shaking up by using an acetic acid solution with the same concentration as that used in the step a; then standing at room temperature for at least 100min to obtain a target detection sample; analyzing the target detection sample by using a liquid chromatography to obtain the peak area of hydroxylamine in the target detection sample; and (c) calculating to obtain the concentration of hydroxylamine in the sample to be detected by using the standard working curve of hydroxylamine drawn in the step (a).
In the step b, the conditions of the liquid chromatography are preferably:
a chromatographic column: ZORBAX-eclipse XDB-C18;
mobile phase: 40% acetonitrile in water;
flow rate: 1.0 mL/min;
column temperature: room temperature;
sample introduction amount: 20 mu L of the solution;
detection wavelength: 305 nm.
In the step a and the step b, the liquid chromatography is used for analytical test under the same condition.
In the step b, the sample to be tested is preferably analyzed and tested by a method of combining a high performance liquid chromatography column ZORBAX-eclipses XDB-C18 and an ultraviolet detector.
In the step b, preferably, the aminohydroxyurea coexistence solution to be detected is an aminohydroxyurea-nitric acid solution, and preferably, the concentration of nitric acid is 0.2-1.0 mol/L; preferably, the absorption dose of the aminohydroxyurea coexistence solution to be detected is 5-25 kGy.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method establishes chemical derivatization-liquid chromatography for analyzing hydroxylamine, and the aminohydroxyurea does not influence the analysis of hydroxylamine, and the method has the advantages of simple operation, high sensitivity and good repeatability;
2. the minimum detection concentration of hydroxylamine by the method of the invention can reach 2 multiplied by 10-7mol/L, the relative standard deviation of the analysis method can reach 0.8%;
3. under the condition of the method, the peak of the amino-hydroxyurea is about 2.0min, the retention time of the hydroxylamine peak is about 4.4min, so the analysis of hydroxylamine is not interfered by the amino-hydroxyurea, and in addition, the peak of the developer nitrobenzaldehyde is about 5.3min, and the separation of three peaks is good.
Drawings
FIG. 1 is a liquid chromatogram of a standard solution of hydroxylamine in the presence of aminohydroxyurea according to a preferred embodiment of the present invention.
FIG. 2 is a graph of a standard working curve of hydroxylamine plotted according to a preferred embodiment of the present invention.
FIG. 3 is a graph of hydroxylamine concentration versus dose in 0.2M HSC-nitric acid irradiated samples according to a preferred embodiment of the present invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the main experimental apparatus:
an Agilent 1100 model high performance liquid chromatograph comprises an online degasser, a quaternary pump, a column incubator, an ultraviolet detector and a chemical workstation.
In this example, a method for analyzing hydroxylamine in the presence of aminohydroxyurea, which employs a chemical derivatization method and a liquid chromatography method, includes the following steps:
1) preparing a hydroxylamine standard solution:
according to the solvent addition calculated by volume ratio, the standard substance hydroxylamine is accurately prepared into 2.0 multiplied by 10-3A mol/L hydroxylamine standard solution; taking 7 10mL volumetric flasks, adding 1.0mL of the solution2×10-3mol/L aminohydroxyurea, then adding into different volume concentration of 2.0X 10-3mol/L hydroxylamine standard solution, 1.0ml of 6X 10-3Shaking the solution of developer nitrobenzaldehyde in mol/L, and finally using the solution with the concentration of 2.0X 10-3The solution of acetic acid of mol/L is added to constant volume and shaken up to obtain the amino hydroxyurea-containing solution with the hydroxylamine concentration of 0.4, 0.8, 2.0, 6.0, 20.0, 60.0 and 200.0 multiplied by 10-6Standing the hydroxylamine standard solution at the mol/L for 100min at room temperature to obtain a standard sample;
2) drawing a standard working curve of hydroxylamine:
analyzing the standard sample obtained in the step 1) by using a liquid chromatography so as to obtain peak areas of hydroxylamine with different concentrations, and drawing a graph by using the hydroxylamine concentration as a horizontal coordinate and the hydroxylamine peak area as a vertical coordinate, and drawing the graph by using the hydroxylamine peak area to the hydroxylamine concentration so as to obtain a standard working curve of the hydroxylamine;
as shown in FIG. 2, FIG. 2 is a graph of the standard work curve of hydroxylamine, with hydroxylamine concentration on the abscissa, 10-6mol/L, the ordinate is hydroxylamine peak area, mAU s; the concentration of hydroxylamine is 0.4 to 200.0 times 10-6In the mol/L range, the hydroxylamine concentration is proportional to the peak area, the standard work curve equation of hydroxylamine is that y is 0.8984x-0.7732, and the correlation coefficient is as follows: r20.9995; wherein, hydroxylamine standard working curve data is shown in table 1:
TABLE 1 hydroxylamine Standard working Curve data sheet
| Concentration (10)-6mol/L) | 0.4 | 0.8 | 2.0 | 6.0 | 20.0 | 60.0 | 200.0 |
| Peak area (mAU s) | 1.07 | 1.12 | 2.08 | 3.96 | 15.12 | 51.42 | 179.62 |
The conditions of the liquid chromatography were:
a chromatographic column: ZORBAX-eclipse XDB-C18;
mobile phase: 40% acetonitrile in water;
flow rate: 1.0 mL/min;
column temperature: room temperature;
sample introduction amount: 20 mu L of the solution;
detection wavelength: 305 nm;
3) taking a sample to be tested for analysis, thereby obtaining the concentration of hydroxylamine in the sample:
taking the analysis of hydroxylamine concentration in the sample irradiated by 0.2mol/L aminohydroxyurea-nitric acid solution as an example,
the concentration of nitric acid is 0.2mol/L, 0.6mol/L and 1.0 mol/L; the absorbed doses of the samples were 5kGy, 10kGy, 15kGy, 20kGy and 25 kGy. Respectively putting 1.0mL of sample into a 10mL volumetric flask, adding KOH solution with corresponding concentration for neutralization, then using ultrapure water for constant volume and shaking up to obtain 18 samples with different nitric acid concentrations and different absorption doses; taking 18 10mL volumetric flasks, adding 0.1mL of the sample respectively, and then adding the samples respectively1.0mL of 6X 10-3The mol/L developer nitrobenzaldehyde is used with 2X 10-3Fixing the volume of the mol/L acetic acid, and standing for 100min at room temperature; these irradiated samples were analyzed under the same liquid chromatography analysis conditions as in said step 2) to obtain peak areas of the hydroxylamines they contained, as shown in Table 2, in which the dilution factor was (10/1) × (10/0.1);
TABLE 2.0.2M area of peak of hydroxylamine (mAU. s) in HSC-nitric acid irradiated samples
| Dosage (kGy) | 0 | 5 | 10 | 15 | 20 | 25 |
| 0.2M |
0 | 1.68 | 2.63 | 3.23 | 4.29 | 4.92 |
| 0.6M HNO3 | 1.01 | 1.05 | 1.16 | 1.27 | 1.48 | 1.84 |
| 1.0M HNO3 | 1.03 | 1.35 | 1.37 | 1.49 | 1.57 | 1.90 |
The standard working curve of hydroxylamine is obtained as y which is 0.6294x +0.8363, and the concentration range of hydroxylamine is (0.2-4.63) × 10-6mol/L，R20.9949. The concentration of hydroxylamine in the irradiated sample can be calculated according to the peak area of hydroxylamine in the irradiated sample, the standard working curve of hydroxylamine and the dilution factor of the sample, and the result is shown in table 3:
TABLE 3.0.2M concentration of hydroxylamine in HSC-nitric acid irradiated samples (10)-3mol/L)
| Dosage (kGy) | 0 | 5 | 10 | 15 | 20 | 25 |
| 0.2M HNO3 | 0.00 | 1.34 | 2.85 | 3.80 | 5.48 | 6.48 |
| 0.6M HNO3 | 0.27 | 0.34 | 0.51 | 0.69 | 1.02 | 1.59 |
| 1.0M HNO3 | 0.30 | 0.81 | 0.84 | 1.03 | 1.16 | 1.69 |
Plotting the absorbed dose of the sample as abscissa and the hydroxylamine concentration as ordinate to obtain a relationship graph of hydroxylamine concentration and dose generated by the radiolysis of the aminohydroxyurea nitric acid solution, such as FIG. 3, FIG. 3 is a relationship graph of hydroxylamine concentration and dose in a 0.2M HSC-nitric acid irradiated sample, the abscissa is the absorbed dose of the sample, kGy, the ordinate is the hydroxylamine concentration, 10-3mol/L。
In this example, the liquid chromatogram of a hydroxylamine standard solution in the presence of aminohydroxyurea is shown in FIG. 1, with retention time, min, on the abscissa. Wherein: 1: aminohydroxyurea peak 2: hydroxylamine peak 3: nitrobenzaldehyde peak. Under the conditions of this example, the retention time of the aminohydroxyurea peak was 2.0min and the retention time of the hydroxylamine peak was 4.4min, so that the aminohydroxyurea did not interfere with the analysis of hydroxylamine. The developer nitrobenzaldehyde peak retention time was about 5.3min, and the three peaks were well separated, as shown in FIG. 1.
In the new method for analyzing hydroxylamine in the coexistence of aminohydroxyurea in the embodiment, after a sample to be tested is neutralized and diluted, 1.0mL of the sample is put into a 10mL volumetric flask, 1.0mL of nitrobenzaldehyde solution is added, the volume is determined by using acetic acid solution, the mixture is shaken up, and the mixture is kept standing for 100min at room temperature; and then, analyzing the sample to be detected under the optimal condition by using a method of combining a high performance liquid chromatography column ZORBAX-eclipss XDB-C18 and an ultraviolet detector to obtain the peak area of hydroxylamine in the sample to be detected, and calculating to obtain the concentration of hydroxylamine in the sample to be detected by using a standard working curve of hydroxylamine. The minimum detection concentration of hydroxylamine can reach 2 x 10-7mol/L, the relative standard deviation of the analytical method of this example is 0.8%. The method for analyzing hydroxylamine by establishing the chemical derivatization-liquid chromatography has the advantages that the hydroxylamine analysis is not influenced by the amino hydroxyurea, the operation is simple, the sensitivity is high, and the repeatability is good.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes may be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitution patterns, so long as the technical principle and the inventive concept of the hydroxylamine analysis method in the coexistence of aminohydroxyurea of the present invention are met, and the present invention shall fall within the protection scope of the present invention.
Claims (5)
1. A method for analyzing hydroxylamine in the coexistence of aminohydroxyurea is characterized in that the method for analyzing hydroxylamine by adopting a chemical derivatization method and a liquid chromatography method comprises the following steps:
a. drawing a standard working curve of hydroxylamine:
taking a series of volumetric flasks with the same volume, respectively adding 1.0ml of aminohydroxyurea solution with known concentration according to the solvent addition calculated according to the volume ratio, respectively and correspondingly adding hydroxylamine standard solutions with different volumes, and shaking up; then respectively adding 1.0ml of color-developing agent nitrobenzaldehyde solution with known concentration, using acetic acid solution with known concentration to make constant volume, uniformly shaking so as to obtain the hydroxylamine containing amino hydroxyurea whose concentration is (0.4-200.0) × 10-6A series of hydroxylamine standard solutions in mol/L; then standing at room temperature for at least 100min to obtain a standard sample; then, analyzing the series of hydroxylamine standard solutions by using a liquid chromatography method to obtain the hydroxylamine peak area in each standard sample, and drawing by using the hydroxylamine concentration as a horizontal coordinate and the hydroxylamine peak area as a vertical coordinate to obtain a standard working curve of hydroxylamine;
b. taking a sample to be tested for analysis, thereby obtaining the concentration of hydroxylamine in the sample:
neutralizing and diluting the aminohydroxyurea coexistence solution to be detected to obtain a sample to be detected, putting 1.0ml of the sample to be detected into a volumetric flask, adding 1.0ml of a color reagent nitrobenzaldehyde solution with the same concentration as that used in the step a, and carrying out constant volume and shaking up by using an acetic acid solution with the same concentration as that used in the step a; then standing at room temperature for at least 100min to obtain a target detection sample; analyzing the target detection sample by using a liquid chromatography to obtain the peak area of hydroxylamine in the target detection sample; then, calculating to obtain the concentration of hydroxylamine in the sample to be detected by using the standard working curve of hydroxylamine drawn in the step a;
in the step b, the conditions of the liquid chromatography are as follows:
a chromatographic column: ZORBAX-eclipse XDB-C18;
mobile phase: 40% acetonitrile in water;
flow rate: 1.0 mL/min;
column temperature: room temperature;
sample introduction amount: 20 mu L of the solution;
detection wavelength: 305 nm.
2. The method of analyzing hydroxylamine in the coexistence of aminohydroxyurea according to claim 1, characterized in that: in said steps a and b, the liquid chromatography is used for analytical tests with the same conditions.
3. The method of analyzing hydroxylamine in the coexistence of aminohydroxyurea according to claim 1, characterized in that: in the step b, a high performance liquid chromatography column ZORBAX-eclipss XDB-C18 and an ultraviolet detector are used together to carry out analysis test on the sample to be tested.
4. The method of analyzing hydroxylamine in the coexistence of aminohydroxyurea according to claim 1, characterized in that: in the step b, the aminohydroxyurea coexistence solution to be detected is an aminohydroxyurea-nitric acid solution.
5. The method of analyzing hydroxylamine in the coexistence of aminohydroxyurea according to claim 4, characterized in that: in the step b, the aminohydroxyurea coexistence solution to be detected is an aminohydroxyurea-nitric acid solution, and the concentration of the nitric acid is 0.2-1.0 mol/L; the absorption dose of the aminohydroxyurea coexistence solution to be detected is 5-25 kGy.
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| CN111812249A (en) * | 2020-07-24 | 2020-10-23 | 济南同路医药科技发展有限公司 | Detection method of trace hydroxylamine hydrochloride |
| CN111855881B (en) * | 2020-08-24 | 2022-08-16 | 珠海润都制药股份有限公司 | Method for detecting hydroxylamine hydrochloride in azilsartan |
| CN114994212A (en) * | 2022-06-21 | 2022-09-02 | 常州合全药业有限公司 | High performance liquid chromatography detection method for hydroxylamine residue in medicine |
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