CN110715922A - Br-PADAP-uranyl ion spectrophotometry - Google Patents

Br-PADAP-uranyl ion spectrophotometry Download PDF

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CN110715922A
CN110715922A CN201911137842.0A CN201911137842A CN110715922A CN 110715922 A CN110715922 A CN 110715922A CN 201911137842 A CN201911137842 A CN 201911137842A CN 110715922 A CN110715922 A CN 110715922A
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padap
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胡晖
蒋磊
汪湉
张佳源
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Fuzhou University
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Abstract

The invention discloses a Br-PADAP-uranyl ion spectrophotometry, which mainly solves the problem that the existing Br-PADAP-uranyl ion spectrophotometry needs a highly toxic substance sodium fluoride as a stabilizer. The technical scheme is as follows: adding a nitric acid solution, an ascorbic acid solution and an organic extractant into a solution containing uranyl ions, oscillating, standing and layering; transferring part of the organic extract phase into a volumetric flask, adding a masking agent, a buffering agent, a stabilizing agent and a color developing agent, fixing the volume with absolute ethyl alcohol, shaking up, and measuring the content of uranyl ions in the solution by using an ultraviolet-visible spectrophotometer. Compared with the existing detection method, the method has the advantages of simple and convenient operation, strong anti-interference capability, environmental protection, no need of pretreatment of the detection sample liquid and the like.

Description

Br-PADAP-uranyl ion spectrophotometry
Technical Field
The invention belongs to the field of analysis and detection, and particularly relates to a Br-PADAP-uranyl ion spectrophotometry.
Background
Uranium is a rare and noble metal, and three kinds of isotopes exist in nature234U、235U and238u, all carry radioactivity. The current world energy crisis is aggravated continuously, the nuclear power industry taking uranium as fuel receives attention of various countries gradually, and with the great development of the nuclear power industry, the risk of uranium polluting water bodies is greatly increased due to the fact that a large amount of uranium-containing nuclear waste liquid is generated in the exploitation of uranium ores and the nuclear industry, abnormal leakage of nuclear power plants and the like. The pollution of uranium, usually in the form of uranyl ions (UO), by the sources mentioned above presents a great potential threat to the environment and humans2 2+) The method is in an aqueous solution, so that the development of a simple detection method for in-situ monitoring of the content of uranyl ions in nuclear waste storage areas and water environments near uranium ores is of great significance.
The detection method of uranyl ions in the aqueous solution mainly comprises the following steps: laser induced fluorescence, inductively coupled plasma emission spectroscopy, atomic absorption spectroscopy, spectrophotometry, and the like. The laser-induced fluorescence method, the inductively coupled plasma emission spectrometry method and the atomic absorption spectrometry method have the advantages of high sensitivity and strong anti-interference capability, but have the defects of expensive instrument and equipment, complex sample pretreatment procedure, complex operation and the like, and are not suitable for in-situ monitoring of uranyl ions in a water environment. The spectrophotometry has the advantages of low instrument and equipment, simplicity and convenience in operation, low requirement on working environment and the like, and is suitable for in-situ monitoring of uranyl ions in water environment. The spectrophotometry method for detecting uranyl ions in aqueous solution mainly comprises the following steps: azoarsine I spectrophotometry, azoarsine III spectrophotometry, thiocyanate spectrophotometry and Br-PADAP spectrophotometry. Arsenazo I and Arsenazo III spectrophotometry are susceptible to interference from coexisting ions. The thiocyanate spectrophotometry is insensitive to color reaction and the formed color-developing complex has poor stability. The Br-PADAP spectrophotometry takes Br-PADAP [2- (5-bromine-2-pyridine azo) -5-diethylamino phenol ] as a color developing agent, the color developing reaction is sensitive, the stability of the formed color developing complex is good, and the interference of coexisting ions is not easy. However, the Br-PADAP spectrophotometry needs to use a highly toxic substance sodium fluoride as a stabilizer, and the defects of fluoride poisoning of testers and difficulty in treatment of generated test waste liquid containing the highly toxic substance sodium fluoride exist in the test process. SDS (sodium dodecyl sulfate) is an anionic surfactant, and is often used to make low toxicity, harmless detergents and emulsifiers due to its low toxicity and good foaming properties. Aiming at the defect that highly toxic sodium fluoride is required to be used as a stabilizer in the Br-PADAP spectrophotometry, the low-toxicity SDS is used as the stabilizer, so that the green environmental protection performance of the Br-PADAP spectrophotometry is improved.
Disclosure of Invention
The invention provides a uranyl ion analysis method which is free of sodium fluoride, green, environment-friendly, simple and convenient to test and strong in anti-interference capacity, and has important significance for detecting uranyl ions.
The technical scheme adopted by the invention is as follows: adding a proper amount of nitric acid solution, ascorbic acid solution and organic extractant into 0.1-5mL of solution containing uranyl ions, oscillating, standing and layering; transferring the organic extract phase into a volumetric flask, adding a masking agent, a buffering agent, a stabilizing agent and a color developing agent, fixing the volume with absolute ethyl alcohol, shaking up, and measuring the content of uranyl ions in the solution by using an ultraviolet-visible spectrophotometer.
The concentration of the nitric acid solution is 0.5 ~ 2 mol/L, and the dosage of the nitric acid solution is 20-100 mL.
The concentration of the ascorbic acid solution is 5 ~ 10 wt%, and the dosage of the ascorbic acid solution is 2-10 mL.
The organic extractant is TOPO (tri-n-octylphosphine oxide) -cyclohexane solution, the concentration is 0.05 ~ 0.2.2M, and the dosage of the TOPO-cyclohexane solution is 2-5 mL.
The rotation speed of the oscillation is 60-180 rpm, the oscillation time is 10-15 min, the standing is at room temperature, and the standing time is 30 ~ 60 min.
The masking agent is a mixed solution of CyDTA (cyclohexanediamine tetraacetic acid) and sulfosalicylic acid, the concentration of the CyDTA (cyclohexanediamine tetraacetic acid) is 2 ~ 4 wt%, the concentration of the sulfosalicylic acid is 2 ~ 4 wt%, and the dosage of the mixed solution is 0.5-4 mL.
The buffer is TEA (triethanolamine) solution with the concentration of 10 ~ 30 vol%, and the dosage of the triethanolamine solution is 0.5-4 mL.
The stabilizer is SDS (sodium dodecyl sulfate) solution, the concentration is 0.5 ~ 5 wt%, and the dosage of the sodium dodecyl sulfate solution is 0.5-4 mL.
The color developing agent is Br-PADAP [2- (5-bromine-2-pyridine azo) -5-diethylaminophenol ] solution, the concentration is 0.05 ~ 0.1.1 wt%, and the using amount of the Br-PADAP solution is 1-4 mL.
In the preparation process of the Br-PADAP solution, absolute ethyl alcohol is used as a solvent to dissolve Br-PADAP, the Br-PADAP solution is transferred into a volumetric flask, and the absolute ethyl alcohol is used for constant volume.
The testing wavelength of the ultraviolet-visible spectrophotometer is 576 nm.
The invention has the beneficial effects and outstanding advantages that:
1. the test principle of the invention is that the U (VI), the sodium dodecyl sulfate and the Br-PADAP generate a peach color developing complex with the coordination ratio of 1:1:1, the maximum absorption wavelength is 576nm, the method is simple, convenient and quick, large-scale equipment is not required to be put into, and the cost is saved.
2. The invention adopts the mixed solution of CyDTA (cyclohexanediaminetetraacetic acid) and sulfosalicylic acid as a masking agent and adopts the low-toxicity anionic surfactant SDS (sodium dodecyl sulfate) as a stabilizing agent to successfully replace the high-toxicity substance sodium fluoride which can cause diseases, is lethal and is difficult to treat, thereby reducing the hazard of the analysis and detection process.
3. The invention has the advantages of strong anti-interference capability and environmental protection.
Drawings
FIG. 1 is a wavelength scan of the present invention;
FIG. 2 is a standard operating curve of the present invention;
FIG. 3 shows the stability test results of the U (VI) -Br-PADAP complex.
Detailed Description
The present invention will be further described with reference to examples, which will help to better understand the present invention, but the present invention is not limited to only the following examples.
Example 1 maximum wavelength establishment;
firstly, 1M HNO is prepared3Solution, 5% [ w (g)/v (mL) ]]Ascorbic acidThe solution, 0.05M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 1% SDS solution, 20% TEA solution and a mixed solution containing 2% CyDTA and 4% sulfosalicylic acid. 0, 0.5, 1, 1.5, 2 and 2.5 mL of 100 mg/L uranyl ion standard solution are respectively put into a 50 mL conical flask, and 30 mL1 MHNO is added3The solution, 2mL ascorbic acid solution and 5mL extracting agent are vibrated for 15 min, the mixture is kept still for reaction for 30 min, 2mL upper layer organic phase is taken and put into a 25 mL volumetric flask, 2mL masking agent, 2mL buffer solution, 2mL SDS solution, 2mL color developing agent and 12 mL absolute ethyl alcohol are accurately added in sequence, the volume is determined by the absolute ethyl alcohol, the mixture is shaken up and kept still for 30 min to be completely developed, blank samples without uranyl ions are taken as reference, wavelength scanning is carried out by an ultraviolet visible spectrophotometer within the wavelength range of 350 ~ 700 nm and 700 nm, a scanning spectrogram is shown in figure 1, and the maximum absorption wavelength can be seen as 576 nm.
Example 2 standard working curve establishment;
firstly, 1M HNO is prepared3Solution, 5% [ w (g)/v (mL) ]]Ascorbic acid solution, 0.05M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 1% SDS solution, 20% TEA solution and mixed solution containing 2% CyDTA and 4% sulfosalicylic acid. 0 mL, 0.5 mL, 1.5 mL, 2mL and 2.5 mL of 100 mg/L uranyl ion standard solution are respectively put into a 50 mL conical flask, and 30 mL of 1 MHNO is added3Vibrating the solution, 2mL ascorbic acid solution and 5mL extractant for 15 min, and standing for reaction for 30 min. Taking 2mL of the upper organic phase, transferring the upper organic phase into a 25 mL volumetric flask, accurately adding 4 mL of masking agent, 2mL of buffer solution, 2mL of SDS solution, 1mL of color developing agent and 10 mL of absolute ethyl alcohol in sequence, fixing the volume with the absolute ethyl alcohol, shaking up, and standing for 30 minutes to completely develop the color; a blank sample without uranyl ions is used as a reference, an ultraviolet-visible spectrophotometer is used for measurement, the test result is shown in table 1, and the standard working curve is shown in fig. 2.
TABLE 1 Standard working Curve test results
Figure DEST_PATH_IMAGE002
Standard working curve equation: y =0.1796x +0.0031, linear correlation coefficient R2= 0.9991。
Example 3 stability determination experiment;
firstly, 1M HNO is prepared3Solution, 5% [ w (g)/v (mL) ]]Ascorbic acid solution, 0.05M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 2% SDS solution, 10% TEA solution and mixed solution containing 2% CyDTA and 4% sulfosalicylic acid. 0, 0.5, 1, 1.5, 2 and 2.5 mL of 100 mg/L uranyl ion standard solution are respectively put into a 50 mL conical flask, and 30 mL1 MHNO is added3Vibrating the solution, 2mL ascorbic acid solution and 5mL extractant for 15 min, and standing for reaction for 30 min. Taking 2mL of the upper organic phase, transferring the upper organic phase into a 25 mL volumetric flask, accurately adding 2mL of a masking agent, 4 mL of a buffer solution, 3 mL of an SDS solution, 2mL of a color developing agent and 8 mL of absolute ethyl alcohol in sequence, fixing the volume with the absolute ethyl alcohol, shaking up, and standing for 30 minutes to completely develop the color; a blank sample without uranyl ions is used as a reference, 0 h, 1 h, 2 h, 3 h and 4 h are used as time intervals, an ultraviolet visible spectrophotometer is used for measurement, the test result is shown in table 2, and the stability measurement is shown in fig. 3.
Table 2 stability determination experimental results
Figure DEST_PATH_IMAGE004
Example 4 normalized recovery test;
firstly, 1M HNO is prepared3Solution, 5% [ w (g)/v (mL) ]]Ascorbic acid solution, 0.05M TOPO-cyclohexane solution, 0.05% Br-PADAP solution, 1% SDS solution, 20% TEA solution, and a mixed solution containing 2% CyDTA and 2% sulfosalicylic acid. Respectively taking 1mL of 2 mg/L and 1mL of 4 mg/L uranyl ion standard solution to a numbered 50 mL conical flask, and adding 30 mL of 1M HNO3Vibrating the solution, 2mL ascorbic acid solution and 3 mL extracting agent for 15 min, and standing for reaction for 30 min. Transferring 1mL of the upper organic phase into a 25 mL volumetric flask, accurately adding 4 mL of masking agent, 4 mL of buffer solution, 4 mL of SDS solution, 2mL of color developing agent and 8 mL of absolute ethyl alcohol in sequence, fixing the volume with the absolute ethyl alcohol, shaking up, and standing for 30 minutes to completely develop the color; a blank sample without uranyl ions is used as a reference, and an ultraviolet-visible spectrophotometer is used for measurement, and the test results are shown in table 3.
TABLE 3 results of recovery calculations with addition of standard
Figure DEST_PATH_IMAGE006
Example 5 Ca resistance2+Measuring the capacity;
firstly, 1M HNO is prepared3Solution, 5% [ w (g)/v (mL) ]]Ascorbic acid solution, 0.05M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 2% SDS solution, 20% TEA solution and mixed solution containing 2% CyDTA and 4% sulfosalicylic acid. Respectively taking 1.5 mL of uranyl ion-containing solution, adding Ca-containing solution with different concentrations into a conical flask with the volume of 50 mL and the number of the conical flask being numbered in advance2+Solution, 30 mL 1M HNO3Vibrating the solution, 2mL ascorbic acid solution and 5mL extractant for 15 min, and standing for reaction for 30 min. Transferring 1mL of the upper organic phase into a 25 mL volumetric flask, accurately adding 3 mL of masking agent, 2mL of buffer solution, 3 mL of SDS solution, 2mL of color developing agent and 10 mL of absolute ethyl alcohol in sequence, fixing the volume with the absolute ethyl alcohol, shaking up, and standing for 30 minutes to completely develop the color; a blank sample containing no uranyl ions was used as a reference, and the measurement was performed by an ultraviolet-visible spectrophotometer, and the results are shown in Table 4.
TABLE 4 Ca resistance2+Results of Capacity measurement
Figure DEST_PATH_IMAGE008
Under the experimental conditions of the present invention, Ca was present in the solution2+(1000 mg/L) the error of the absorbance result is not more than +/-5 percent, and the absorbance result belongs to the normal error range.
Example 6 anti-Mg2+Measuring the capacity;
firstly, 1M HNO is prepared3Solution, 5% [ w (g)/v (mL) ]]Ascorbic acid solution, 0.05M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 1% SDS solution, 20% TEA solution and mixed solution containing 3% CyDTA and 3% sulfosalicylic acid. Respectively taking 1.5 mL of uranyl ion-containing solution, adding Mg-containing solution with different concentrations into a conical flask with the volume of 50 mL numbered in advance2+Solution, 30 mL 1M HNO3Vibrating the solution, 2mL ascorbic acid solution and 4 mL extractant for 15 min, and standing for reaction for 30 min. Take 2mL of the upper organic phase and phase into 25 mL volumeA bottle, which is sequentially and accurately added with 3 mL of masking agent, 2mL of buffer solution, 2mL of SDS solution, 2mL of color developing agent and 10 mL of absolute ethyl alcohol, the volume is determined by the absolute ethyl alcohol, the mixture is shaken up and is kept still for 30 minutes to completely develop color; a blank sample containing no uranyl ions was used as a reference, and the measurement was performed by an ultraviolet-visible spectrophotometer, and the results are shown in Table 5.
TABLE 5 anti-Mg2+Results of Capacity measurement
Figure DEST_PATH_IMAGE010
In the experimental conditions of the present invention, Mg is present in the solution2+(1000 mg/L) the error of the absorbance result is not more than +/-5%, and the error falls within the normal error range.
Example 7
Firstly, 1M HNO is prepared3Solution, 5% [ w (g)/v (mL) ]]Ascorbic acid solution and 0.05M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 1% SDS solution, 20% TEA solution and a mixed solution containing 2% CyDTA and 4% sulfosalicylic acid. 1.5 mL of an ionic solution containing the following contents was taken: UO2 2+(2 mg/L)、Mg2+(1 g/L)、Fe3+(500 mg/L)、Ca2+(500mg/L)、Al3+(100 mg/L)、Mn2+(50 mg/L)、Zn2+(50 mg/L)、SO4 2-(2 g/L)、Cl-(1 g/L), 30 mL 1M HNO was added to a 50 mL Erlenmeyer flask3Vibrating the solution, 2mL ascorbic acid solution and 4 mL extractant for 15 min, and standing for reaction for 30 min. Taking 2mL of the upper organic phase, transferring the upper organic phase into a 25 mL volumetric flask, accurately adding 3 mL of masking agent, 2mL of buffer solution, 2mL of SDS solution, 2mL of color developing agent and 10 mL of absolute ethyl alcohol in sequence, fixing the volume with the absolute ethyl alcohol, shaking up, and standing for 30 minutes to completely develop the color; and taking a blank sample which does not contain uranyl ions as a reference, and measuring the content of the uranyl ions in the solution to be 2.02 mg/L by using an ultraviolet-visible spectrophotometer.
Example 8
The uranyl ion-containing test sample liquid is nuclear waste liquid which mainly contains U (VI), Zn (II), Mn (II) and SO4 2-And NO3 -。
Firstly, 2M HNO is prepared3Solution, 10% [ w (g)/v (mL) ]]Ascorbic acid solution and 0.15M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 1% SDS solution, 20% TEA solution and a mixed solution containing 2% CyDTA and 4% sulfosalicylic acid. Taking 1mL of nuclear waste liquid sample into a 50 mL conical flask, and adding 30 mL of 2M HNO3Vibrating the solution, 2mL ascorbic acid solution and 5mL extractant for 15 min, and standing for reaction for 30 min. Transferring 1mL of the upper organic phase into a 25 mL volumetric flask, accurately adding 4 mL of masking agent, 4 mL of buffer solution, 1mL of SDS solution, 4 mL of color developing agent and 10 mL of absolute ethyl alcohol in sequence, fixing the volume with the absolute ethyl alcohol, shaking up, and standing for 30 minutes to completely develop the color; and measuring the content of uranyl ions in the waste liquid to be 3.82 mg/L by using an ultraviolet-visible spectrophotometer.
Example 9
The test sample liquid containing uranyl ions is nuclear waste liquid which mainly contains U (VI), Mg (II), Mn (II), Th (IV) and Cl-、SO4 2-And NO3 -。
Firstly, 2M HNO is prepared3Solution, 10% [ w (g)/v (mL) ]]Ascorbic acid solution and 0.15M TOPO-cyclohexane solution, 0.1% Br-PADAP solution, 1% SDS solution, 20% TEA solution and a mixed solution containing 2% CyDTA and 4% sulfosalicylic acid. Taking 1mL of nuclear waste liquid sample into a 50 mL conical flask, and adding 30 mL of 2M HNO3Vibrating the solution, 2mL ascorbic acid solution and 5mL extractant for 15 min, and standing for reaction for 30 min. Transferring 1mL of the upper organic phase into a 25 mL volumetric flask, accurately adding 4 mL of masking agent, 4 mL of buffer solution, 1mL of SDS solution, 4 mL of color developing agent and 10 mL of absolute ethyl alcohol in sequence, fixing the volume with the absolute ethyl alcohol, shaking up, and standing for 30 minutes to completely develop the color; and measuring the content of uranyl ions in the waste liquid to be 1.93 mg/L by using an ultraviolet-visible spectrophotometer.
The method can accurately measure the uranyl ions under the condition of a large amount of coexisting interference ions, and the method is high in anti-interference capability, and high in precision and accuracy due to the fact that the Relative Standard Deviation (RSD) of the method is 0.5% ~ 2%.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention. The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (10)

1. A Br-PADAP-uranyl ion spectrophotometry method is characterized in that: adding a proper amount of nitric acid solution, ascorbic acid and an organic extractant into 0.1-5mL of solution containing uranyl ions, oscillating and standing; transferring the organic extract phase into a volumetric flask, adding a masking agent, a buffering agent, a stabilizing agent and a color developing agent, fixing the volume with absolute ethyl alcohol, shaking up, and measuring the content of uranyl ions in the solution by using an ultraviolet-visible spectrophotometer.
2. The Br-PADAP-uranyl ion spectrophotometric method of claim 1, wherein the concentration of the nitric acid solution is 0.5 ~ 2 mol/L, and the dosage of the nitric acid solution is 20-100 mL.
3. The Br-PADAP-uranyl ion spectrophotometric method of claim 1, wherein the concentration of the ascorbic acid solution is 5 ~ 10 wt%, and the dosage of the ascorbic acid solution is 2-10 mL.
4. The Br-PADAP-uranyl ion spectrophotometric method of claim 1, wherein the organic extractant is TOPO-cyclohexane solution with a concentration of 0.05 ~ 0.2.2 mol/L and a dosage of 2-5 mL.
5. The Br-PADAP-uranyl ion spectrophotometry method according to claim 1, wherein the oscillating speed is 60-180 rpm, the oscillating time is 10-15 min, and the standing time is 30 ~ 60min at room temperature.
6. The Br-PADAP-uranyl ion spectrophotometry method of claim 1, wherein the masking agent is a mixed solution of cyclohexanediaminetetraacetic acid and sulfosalicylic acid, the concentration of the cyclohexanediaminetetraacetic acid is 2 ~ 4 wt%, the concentration of the sulfosalicylic acid is 2 ~ 4 wt%, and the dosage of the mixed solution is 0.5-4 mL.
7. The Br-PADAP-uranyl ion spectrophotometric method of claim 1, wherein the buffering agent is triethanolamine solution with a concentration of 10 ~ 30 vol% and a dosage of 0.5-4 mL.
8. The Br-PADAP-uranyl ion spectrophotometric method of claim 1, wherein the stabilizer is sodium dodecyl sulfate solution with a concentration of 0.5 ~ 5 wt%, and the dosage of the sodium dodecyl sulfate solution is 0.5-4 mL.
9. The Br-PADAP-uranyl ion spectrophotometric method according to claim 1, wherein the color developing agent is a Br-PADAP solution, the concentration of the Br-PADAP solution is 0.05 ~ 0.1.1 wt%, the dosage of the Br-PADAP solution is 1-4 mL, and the solvent of the Br-PADAP solution is absolute ethyl alcohol.
10. The Br-papap-uranyl ion spectrophotometry of claim 1, wherein: the testing wavelength of the ultraviolet-visible spectrophotometer is 576 nm.
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CN111303193A (en) * 2020-03-31 2020-06-19 南华大学 PADAP derivative, preparation method and application thereof
CN111303193B (en) * 2020-03-31 2022-12-27 南华大学 PADAP derivative, preparation method and application thereof

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