CN114280025A - Device and method for measuring uranium content in solution - Google Patents

Abstract

The invention relates to a uranium content measurement device and measurement method in a solution. By setting a pulse light source generating module and a time-resolved fluorescence detection module, a time-resolved fluorescence measurement method is used to measure the uranium content in a low-concentration uranium-containing solution to be measured; The light source generation module and the fluorescence wavelength dispersion detection module use the wavelength dispersion measurement method to measure the uranium content of high concentration. Compared with the existing fluorescence uranium measuring instrument, the measuring device of the present invention improves the measurement range of the uranium content, and compared with the existing fluorescence uranium measuring instrument The prior art needs to measure relatively high-concentration uranium-containing solutions, and the solution needs to be diluted. The continuous light source generation module and the fluorescence wavelength dispersion detection module provided in the present invention can directly measure the uranium content of the high-concentration uranium-containing solution, reducing the need for The inconvenience of sample dilution and repeated measurements.

Description

A kind of measuring device and measuring method of uranium content in solution

technical field

The invention relates to the technical field of laboratory analysis and testing, in particular to a device and a method for measuring uranium content in a solution.

Background technique

From the analysis and testing of natural uranium ore to the reprocessing of nuclear fuel, the analysis and testing of uranium is involved. Although the existing measurement methods can basically cover the entire process, the matrix components and uranium content of different feed liquids are quite different, and various methods need to be used for measurement.

Due to the advantages of simple equipment, convenient operation and low detection limit, the fluorescent trace uranium determination method has been used in uranium ore testing and post-processing processes. However, due to its relatively narrow linear range, only low concentrations of uranium in the concentration range of 0-100ppb can be directly measured.

Therefore, there is an urgent need for a measuring device and a measuring method for uranium content in a solution to improve the measuring range.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a measuring device and measuring method of uranium content in solution, so as to improve the measuring range of uranium content.

For achieving the above object, the present invention provides the following scheme:

A device for measuring uranium content in a solution, comprising:

Fluorescence cuvette, used to hold the uranium-containing solution to be tested;

a pulsed light source generating module; the ultraviolet pulse excitation light generated by the pulsed light source generating module is incident on the fluorescent cuvette;

a time-resolved fluorescence detection module, used for collecting the first fluorescence generated after the uranium-containing solution to be tested is excited by the ultraviolet pulse excitation light, and detecting the intensity of the first fluorescence;

The optical path between the pulsed light source generating module and the time-resolved fluorescence detection module is perpendicular to the optical path of the ultraviolet pulse excitation light;

a continuous light source generating module; the continuous excitation light generated by the continuous light source generating module is incident on the fluorescent cuvette;

a fluorescence wavelength dispersion detection module, used for collecting the second fluorescence generated after the uranium-containing solution to be tested is excited by continuous excitation light, and detecting the intensity of the second fluorescence;

The optical path between the continuous light source generating module and the fluorescence wavelength dispersion detection module is perpendicular to the optical path of the continuous excitation light;

A computer, connected in communication with the time-resolved fluorescence detection module and the fluorescence wavelength dispersion detection module, respectively, is used to calculate the uranium content in the first concentration range according to the intensity of the first fluorescence, and calculate the uranium content in the first concentration range according to the intensity of the first fluorescence. The intensity calculates the uranium content for a second concentration range, the first concentration range having a smaller value than the second concentration range.

A method for measuring uranium content in a solution using the uranium content measuring device, comprising:

When the time-resolved fluorescence measurement method is used to measure the uranium content first, the uranium content measured by the time-resolved fluorescence measurement method is used as the first preliminary measurement result;

calculating the first difference between the first preliminary measurement result and the maximum endpoint value of the first concentration range;

If the first difference is greater than the threshold, determining the preliminary measurement result as the final uranium content;

If the first difference is less than the threshold, the wavelength dispersion measurement method is used to measure the uranium content to obtain a second uranium content measurement result;

using the second uranium content measurement result as the final uranium content;

When the uranium content is measured by the wavelength dispersion measurement method first, the uranium content measured by the wavelength dispersion measurement method is used as the second preliminary measurement result;

calculating a second difference between the second preliminary measurement and the minimum endpoint value of the second concentration range;

If the second difference is greater than the threshold, determining the second preliminary measurement result as the final uranium content;

If the second difference is smaller than the threshold, the time-resolved fluorescence measurement method is used to measure the uranium content to obtain a third uranium content measurement result;

The third uranium content measurement is taken as the final uranium content.

According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects:

The invention provides a uranium content measurement device and measurement method in a solution. By setting a pulse light source generating module and a time-resolved fluorescence detection module, the time-resolved fluorescence measurement method is used to measure the uranium content in a low-concentration uranium-containing solution to be measured; The continuous light source generation module and the fluorescence wavelength dispersion detection module use the wavelength dispersion measurement method to measure the high-concentration uranium content. Compared with the existing fluorescence uranium measuring instrument, the measuring device of the present invention improves the measurement range of the uranium content, and compared with the existing fluorescent uranium measuring instrument. Since the prior art needs to measure relatively high-concentration uranium-containing solutions, the solution needs to be diluted, the continuous light source generation module and the fluorescence wavelength dispersion detection module provided in the present invention can directly measure the uranium content of high-concentration uranium-containing solutions, reducing It eliminates the inconvenience caused by sample dilution and repeated measurements.

Description of drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the accompanying drawings required in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some of the present invention. In the embodiments, for those of ordinary skill in the art, other drawings can also be obtained according to these drawings without any creative effort. The following drawings are not intentionally scaled to actual size, and the emphasis is on illustrating the gist of the present invention.

1 shows a schematic structural diagram of a device for measuring uranium content in a solution according to the present invention;

Figure 2 shows a flow chart of a method for measuring uranium content in a solution according to the present invention.

Symbol Description:

1- Fluorescence cuvette, 2- Pulse light source generation module, 3- Time-resolved fluorescence detection module, 4- Continuous light source generation module, 5- Fluorescence wavelength dispersion detection module, 6- Computer, 7- Electronic circuit module, 8- Pulse Excitation light source generator, 9-excitation light filter, 10-first focusing lens, 11-pulse signal generator, 12-second focusing lens, 13-monochromatic grating, 14-optical slit, 15-first Photodetector, 16-third focusing lens, 17-emission filter, 18-second photodetector.

Detailed ways

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.

As used herein and in the claims, unless the context clearly dictates otherwise, the words "a", "an", "an" and/or "the" are not intended to be specific in the singular and may include the plural. Generally speaking, the terms "comprising" and "comprising" only imply that the clearly identified steps and elements are included, and these steps and elements do not constitute an exclusive list, and the method or apparatus may also include other steps or elements.

The purpose of the present invention is to provide a measuring device and measuring method of uranium content in solution, so as to improve the measuring range of uranium content.

In order to make the above objects, features and advantages of the present invention more clearly understood, the present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments.

Example 1:

Referring to FIG. 1, this embodiment provides a device for measuring uranium content in a solution, including:

The fluorescence cuvette 1 is used to hold the uranium-containing solution to be tested, preferably the optical path of the fluorescence cuvette 1 is 10-20 mm;

a pulsed light source generating module 2; the ultraviolet pulse excitation light generated by the pulsed light source generating module 2 is incident on the fluorescent cuvette 1;

The time-resolved fluorescence detection module 3 is used to collect the first fluorescence generated after the uranium-containing solution to be tested is excited by the ultraviolet pulse excitation light, and to detect the intensity of the first fluorescence;

The optical path between the pulsed light source generation module 2 and the time-resolved fluorescence detection module 3 is perpendicular to the optical path of the ultraviolet pulse excitation light;

Continuous light source generation module 4; the continuous excitation light generated by the continuous light source generation module 4 is incident on the fluorescent cuvette 1, and the continuous light source generation module 4 can be a semiconductor laser or a mercury lamp and other lamps with specific output wavelengths, such as As shown in FIG. 1 , the pulsed light source generation module 2 and the continuous light source generation module 4 can be located on both sides of the fluorescent cuvette 1 respectively;

The fluorescence wavelength dispersion detection module 5 is used to collect the second fluorescence generated after the uranium-containing solution to be tested is excited by continuous excitation light, and to detect the intensity of the second fluorescence;

The optical path between the continuous light source generation module 4 and the fluorescence wavelength dispersion detection module 5 is perpendicular to the optical path of the continuous excitation light;

The computer 6 is connected in communication with the time-resolved fluorescence detection module 3 and the fluorescence wavelength dispersion detection module 5 respectively, and is used for calculating the uranium content in the first concentration range according to the intensity of the first fluorescence, and according to the first fluorescence intensity. The uranium content in the second concentration range is calculated from the intensity of the second fluorescence, and the value in the first concentration range is smaller than the value in the second concentration range; the computer can also realize remote control of the device through software;

The electronic circuit module 7 is respectively connected with the time-resolved fluorescence detection module 3 and the fluorescence wavelength dispersion detection module 5 through signal lines, and is connected in communication with the computer 6;

The electronic circuit module 7 further includes a power supply module, a signal acquisition module and a timing module; the signal acquisition module is communicatively connected to the timing module, and is electrically connected to the power supply module respectively; the timing module is used to control The collection signal of the first fluorescence by the signal collection module is synchronized with the emission signal of the ultraviolet pulse excitation light path.

As an optional embodiment, the pulsed light source generating module 2 includes a pulsed excitation light source generator 8, an excitation light filter 9 and a first focusing lens 10;

The pulse excitation light source generator 8 is used to generate a pulsed laser light source with an adjustable luminous frequency, including a power supply and a pulse signal generator 11;

The excitation light filter 9 is used to obtain an ultraviolet pulse excitation light source of a specific wavelength;

The first focusing lens 10 is used to shape the ultraviolet pulse excitation light into approximately parallel light, so as to improve the utilization rate of the ultraviolet pulse excitation light source.

The ultraviolet pulse excitation light generated by the pulse excitation light source generator 8 is incident on the fluorescence cuvette 1 after passing through the excitation light filter 9 and the first focusing lens 10 in sequence.

The time-resolved fluorescence detection module 3 includes a second focusing lens 12, a monochromatic grating 13, an optical slit 14, and a first photodetector 15;

The second focusing lens 12 is used to shape the first fluorescence into approximately parallel light, so as to improve the signal intensity of the fluorescence;

The monochromatic grating 13 is used for screening the first fluorescence of a specific wavelength;

The first fluorescent light enters the first photodetector 15 after passing through the second focusing lens 12 , the monochromatic grating 13 and the optical slit 14 in sequence.

The fluorescence wavelength dispersion detection module 5 includes a third focusing lens 16, an emission filter 17 and a second photodetector 18;

The third focusing lens 16 is used to shape the second fluorescence into approximately parallel light, so as to improve the signal intensity of the fluorescence;

The emission light filter 17 is used to filter light signals of other wavelengths, and to filter the second fluorescence of a specific wavelength;

The second fluorescent light is incident on the second photodetector 18 after passing through the third focusing lens 16 and the emission filter 17 in sequence.

The wavelength of the first fluorescence screened out by the monochromatic grating 13 is smaller than the wavelength of the second fluorescence screened out by the emission filter 17;

Preferably, both the first photodetector 15 and the second photodetector 18 include photosensitive components and amplification circuits, wherein the photosensitive components are used for detection of fluorescence intensity, and photomultiplier tubes, silicon photodiodes, etc. can be selected. Amplifying circuits are used to obtain optical signals of sufficient strength.

The measurement device of this embodiment is simple, reliable, easy to operate, and suitable for on-site rapid measurement of uranium in solution; in design, a time-resolved fluorescence detection module is coupled with a pulsed light source generation module, and a fluorescence wavelength dispersion detection module is coupled with a continuous light source generation module, respectively. Using different detection principles, the determination of low-concentration and high-concentration uranium content can be achieved respectively, which broadens the measurement range of uranium content; at the same time, the two measurement channels are independent of each other and do not interfere with each other; The uranium content of the uranium-containing solution is determined, which reduces the inconvenience caused by sample dilution and repeated measurement.

Example 2:

This embodiment utilizes the uranium content measuring device of Embodiment 1 to provide a method for measuring uranium content in a solution, referring to FIG. 2 , including:

S1: when the time-resolved fluorescence measurement method is used to measure the uranium content first, the uranium content measured by the time-resolved fluorescence measurement method is used as the first preliminary measurement result;

S2: Calculate the first difference between the first preliminary measurement result and the maximum endpoint value of the first concentration range;

S3: if the first difference is greater than the threshold, determine the preliminary measurement result as the final uranium content;

S4: if the first difference is smaller than the threshold, the wavelength dispersion measurement method is used to measure the uranium content to obtain a second uranium content measurement result;

S5: take the second uranium content measurement result as the final uranium content;

S6: when the wavelength dispersion measurement method is used to measure the uranium content first, the uranium content measured by the wavelength dispersion measurement method is used as the second preliminary measurement result;

S7: Calculate the second difference between the second preliminary measurement result and the minimum endpoint value of the second concentration range;

S8: if the second difference is greater than the threshold, determine the second preliminary measurement result as the final uranium content;

S9: if the second difference is less than the threshold, use a time-resolved fluorescence measurement method to measure the uranium content to obtain a third uranium content measurement result;

S10: Use the third uranium content measurement result as the final uranium content.

As an optional implementation manner, S1 specifically includes:

adding the fluorescence enhancement solution of preset concentration and quantitative volume into the fluorescence cuvette to obtain the first solution;

Using a time-resolved fluorescence measurement method to obtain the fluorescence intensity of the first solution;

adding a uranium standard solution with a preset concentration and a quantitative volume to the first solution to obtain a second solution;

Obtain the fluorescence intensity of the second solution by using a time-resolved fluorescence measurement method;

Adding a quantitative volume of the uranium-containing solution to be tested to the second solution to obtain a third solution;

Obtain the fluorescence intensity of the third solution by using a time-resolved fluorescence measurement method;

The first preliminary measurement result is calculated according to the fluorescence intensity of the first solution, the fluorescence intensity of the second solution, the fluorescence intensity of the third solution, and the preset concentration of the uranium standard solution.

The obtaining the fluorescence intensity of the first solution by using a time-resolved fluorescence measurement method specifically includes:

Area integration is performed on the triggering decay time and the fluorescence decay intensity of a single ultraviolet pulse excitation light path to obtain a single pulse fluorescence intensity, and the fluorescence decay intensity is the first corresponding to the single ultraviolet pulse excitation light path trigger decay time. solution fluorescence intensity;

The fluorescence intensity of the first solution is obtained by summing the fluorescence intensities of multiple single pulses obtained within the preset time for collecting the fluorescence intensity of the first solution.

As an optional implementation manner, S6 specifically includes:

adding a fluorescence enhancement solution with a preset concentration and a quantitative volume and a uranium standard solution with a preset concentration and a quantitative volume into the fluorescence cuvette to obtain a fourth solution;

Obtain the fluorescence intensity of the fourth solution by using a wavelength dispersion measurement method;

Adding a uranium standard solution with a preset concentration and a set multiple quantitative volume to the fourth solution to obtain a fifth solution;

Obtain the fluorescence intensity of the fifth solution by using a wavelength dispersion measurement method;

Adding a quantitative volume of the uranium-containing solution to be tested to the fourth solution to obtain the sixth solution;

Obtain the fluorescence intensity of the sixth solution by using a wavelength dispersion measurement method;

The second preliminary measurement result is calculated according to the fluorescence intensity of the fourth solution, the fluorescence intensity of the fifth solution, the fluorescence intensity of the sixth solution, and the quantitative volume of the uranium-containing solution to be measured.

The wavelength dispersion measurement method to obtain the fluorescence intensity of the fourth solution specifically includes:

calculating the average value of the fluorescence intensities of a plurality of the fourth solutions obtained within the preset time for collecting the fluorescence intensities of the fourth solutions;

The average value was taken as the fluorescence intensity of the new fourth solution.

In order to make the above process more clearly understood by those skilled in the art, the following is explained with specific examples.

Example 1:

The parameters of the uranium content measuring device are configured as follows:

The pulse excitation light source generator 8 selects a pulsed xenon lamp light source, and the power of the pulsed xenon lamp is 5w;

The continuous light source generation module 4 selects a semiconductor laser, the power of the semiconductor laser is 5mw, and the wavelength is 405nm;

The wavelength range transmitted by the excitation light filter 9: 230-460nm;

Transmitting wavelength range of emission light filter 17: 480-610nm;

The first photodetector 15 selects a photomultiplier tube;

The second photodetector 18 selects a photomultiplier tube.

Working parameter settings:

Working frequency of pulse excitation light source generator 8: 100Hz, pulse width 2μs;

Time-resolved fluorescence detection module 3: The single-pulse fluorescence signal acquisition sequence starts from 10 μs to 1000 μs after the pulse laser light source is triggered, and performs area integration according to the decay time and the fluorescence decay intensity to obtain the single-pulse fluorescence intensity; The cumulative summation of the single-pulse fluorescence intensities.

Semiconductor laser: 5mw continuous output for 10s;

Fluorescence wavelength dispersion detection module 5: the sampling frequency is 100Hz, and the average value of the signal in the interval of 1-10s is taken.

a) Turn on the time-resolved fluorescence detection module 3, and turn off the fluorescence wavelength dispersion detection module 5.

Set the high voltage of the photomultiplier tube to 1000v to collect the fluorescence signal of uranium.

The content of uranium was calculated by the standard addition method: add 4.5mL of 1% sodium pyrophosphate solution to the 5mL fluorescence cell, and the fluorescence intensity was measured as F0, then accurately add 50μL of 100ppb uranium standard solution to the fluorescence cell, and after stirring evenly, measure The fluorescence intensity was measured as F1, then 50 μL of sample solution was added to the fluorescence cell, stirred evenly, and the fluorescence intensity was measured as F2. The content of uranium in the solution can be obtained by calculating C _U =(F2-F1)/(F1- F0)×100ppb.

The first concentration range is set to be 0.02-500ppb. If the difference between the measured uranium content and 500ppb is less than the threshold, the wavelength dispersion measurement method is used to determine the uranium content, namely:

b) Turn off the time-resolved fluorescence detection module 3, turn on the fluorescence wavelength dispersion detection module 5, and set the high voltage of the photomultiplier tube to 1000v.

The external standard method was used to calculate the uranium content in the solution: add 4.5 mL of 1% sodium pyrophosphate solution to the 5 mL fluorescence cell, and accurately add 10 μL of 10 ppm uranium standard solution. Fluorescence intensities F2, F3, F4 and F5 corresponding to 20μL, 30μL, 40μL and 50μL uranium standard solutions, according to the content of uranium in the fluorescence pool and the corresponding fluorescence intensity to make a content-intensity curve, y=ax+b, where y is the fluorescence Intensity, x is the uranium content, a is the slope of the curve, and b is the intercept of the curve. Add 4.5mL of 1% sodium pyrophosphate solution to the 5mL fluorescence cell, add 10μL of sample solution accurately, measure the fluorescence intensity and record it as Fs, the content of uranium in the sample solution can be obtained by calculation C _U =(Fs-b)/a/ 10 μL.

The second concentration range is set to 10-500 ppm, ie 10 ⁴ -5*10 ⁵ ppb.

Example 2:

The parameters of the uranium content measuring device are configured as follows:

The pulse excitation light source generator 8 selects a pulsed xenon lamp light source, and the power of the pulsed xenon lamp is 15w;

The continuous light source generation module 4 selects a semiconductor laser, the power of the semiconductor laser is 100mW, and the wavelength is 405nm;

Adjust the angle of the monochromatic grating 13 to make the wavelength range through the optical slit 14: 300-350nm;

Semiconductor laser power: 100mW;

Semiconductor laser wavelength: 405nm;

The first photodetector 15 selects a photomultiplier tube;

The second photodetector 18 is a silicon photodiode.

Working parameter settings:

Working frequency of pulse excitation light source generator 8: 10Hz, pulse width 5μs;

Working frequency of pulse excitation light source generator 8: 100Hz, pulse width 2μs;

Time-resolved fluorescence detection module 3: The single-pulse fluorescence signal acquisition sequence starts from 10 μs to 100 μs after the pulse light source is triggered, and performs area integration according to the decay time and the fluorescence decay intensity to obtain the single-pulse fluorescence intensity; Cumulative summation of single-pulse fluorescence intensities.

Semiconductor laser: 5mw continuous output for 10s;

Fluorescence wavelength dispersion detection module 5: The sampling frequency is 10 Hz, and the average value of the signal in the interval of 1 to 10 s is taken.

a) Turn off the time-resolved fluorescence detection module 3 and turn on the fluorescence wavelength dispersion detection module 5 .

The external standard method was used to calculate the uranium content in the solution: add 4.5 mL of 1% sodium dihydrogen phosphate solution to the 5 mL fluorescence cell, and accurately add 10 μL of 10 ppm uranium standard solution. Corresponding to the fluorescence intensities F2, F3, F4 and, F5 corresponding to 20μL, 30μL, 40μL and 50μL uranium standard solutions, the content-intensity curve is made according to the content of uranium in the fluorescence pool and the corresponding fluorescence intensity, y=ax+b, where y is Fluorescence intensity, x is the content of uranium, a is the slope of the curve, and b is the intercept of the curve. Add 4.5mL of 1% sodium dihydrogen phosphate solution to the 5mL fluorescence cell, and add 50μL of sample solution accurately. The measured fluorescence intensity is recorded as Fs. The content of uranium in the sample solution can be obtained by calculating C _U =(Fs-b)/a /50μL.

When the second concentration range is set to 10-500ppm, if the difference between the measured uranium content and 10ppm is less than the threshold, the time-resolved fluorescence measurement method is used to determine the uranium content, namely:

b) Turn on the time-resolved fluorescence detection module 3 and turn off the fluorescence wavelength dispersion detection module 5 .

Set the high voltage of the photomultiplier tube to 500v to collect the fluorescence signal of uranium.

Add 4.5mL of 1% sodium dihydrogen phosphate solution to the 5mL fluorescence cell, and the measured fluorescence background value is calculated as F0, and then accurately add 50μL of 300ppb uranium standard solution to the fluorescence cell, and after stirring evenly, the measured fluorescence value is calculated as F1, then add 50 μL of sample solution into the fluorescence cell, stir evenly, the measured fluorescence value is counted as F2, and the content of uranium in the solution can be obtained by calculation C _U = (F2-F1)/(F1-F0)×300ppb.

The first concentration range is set to 0.02-500 ppb.

In the measurement method of this embodiment, the time-resolved fluorescence measurement method is used to measure the uranium content in the low-concentration uranium-containing solution to be tested, and the wavelength dispersion measurement method is used to measure the high-concentration uranium content, which improves the measurement range of the uranium content, and does not require When diluting the high-concentration uranium-containing solution, the uranium content of the high-concentration uranium-containing solution can be directly determined by the wavelength dispersion measurement method, which reduces the inconvenience caused by sample dilution and repeated measurement.

In addition, since the measurement method of this embodiment adopts the software control mode, functions such as the integration of uranium fluorescence are realized through software algorithms, which reduces the functions that can only be realized by circuits in the past, reduces redundant circuits, and improves the portability of the equipment.

The present invention uses specific terms to describe the embodiments of the present invention. Such as "first/second embodiment", "an embodiment", and/or "some embodiments" means a certain feature, structure or characteristic associated with at least one embodiment of the present invention. Therefore, it should be emphasized and noted that two or more references to "an embodiment" or "one embodiment" or "an alternative embodiment" in different places in this specification are not necessarily referring to the same embodiment . Furthermore, certain features, structures or characteristics of the one or more embodiments of the invention may be combined as appropriate.

Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It should also be understood that terms such as those defined in ordinary dictionaries should be construed as having meanings consistent with their meanings in the context of the related art, and should not be construed in an idealized or highly formalized sense unless explicitly stated herein defined as such.

The above is an illustration of the present invention and should not be construed as limiting it. Although several exemplary embodiments of this invention have been described, those skilled in the art will readily appreciate that many modifications are possible in the exemplary embodiments without departing from the novel teachings and advantages of this invention. Accordingly, all such modifications are intended to be included within the scope of this invention as defined in the claims. It is to be understood that the foregoing descriptions of the invention are not to be considered limited to the particular embodiments disclosed, and that modifications to the disclosed embodiments, as well as other embodiments, are intended to be included within the scope of the appended claims. The invention is defined by the claims and their equivalents.

Claims (10)

1. A uranium content measuring device in solution, characterized by comprising:

the fluorescence cuvette is used for containing a uranium-containing solution to be detected;

a pulse light source generating module; the ultraviolet pulse excitation light generated by the pulse light source generation module is incident into the fluorescence cuvette;

the time-resolved fluorescence detection module is used for collecting first fluorescence generated after the uranium-containing solution to be detected is excited by ultraviolet pulse excitation light and detecting the intensity of the first fluorescence;

the light path between the pulse light source generation module and the time-resolved fluorescence detection module is vertical to the light path of the ultraviolet pulse excitation light;

a continuous light source generation module; continuous exciting light generated by the continuous light source generation module is incident into the fluorescence cuvette;

the fluorescence wavelength dispersion detection module is used for collecting second fluorescence generated after the uranium-containing solution to be detected is excited by continuous exciting light and detecting the intensity of the second fluorescence;

the light path between the continuous light source generation module and the fluorescence wavelength dispersion detection module is vertical to the light path of the continuous exciting light;

and the computer is in communication connection with the time-resolved fluorescence detection module and the fluorescence wavelength dispersion detection module respectively, and is used for calculating the uranium content in a first concentration range according to the intensity of the first fluorescence and calculating the uranium content in a second concentration range according to the intensity of the second fluorescence, wherein the value of the first concentration range is smaller than that of the second concentration range.

2. A uranium content measuring device according to claim 1, wherein the pulsed light source generation module comprises a pulsed excitation light source generator, an excitation light filter and a first focusing lens;

ultraviolet pulse excitation light generated by the pulse excitation light source generator sequentially passes through the excitation light filter and the first focusing lens and then is incident into the fluorescence cuvette.

3. A uranium content measurement device according to claim 1, wherein the time-resolved fluorescence detection module comprises a second focusing lens, a monochromatic grating, an optical slit, a first photodetector;

and the first fluorescence sequentially passes through the second focusing lens, the monochromatic grating and the optical slit and then enters the first photoelectric detector.

4. A uranium content measuring device according to claim 1, wherein the fluorescence wavelength dispersion detection module comprises a third focusing lens, an emission light filter and a second photodetector;

and the second fluorescence sequentially passes through the third focusing lens and the emission light filter and then enters the second photoelectric detector.

5. A uranium content measurement device according to claim 1, further comprising: the electronic circuit module is respectively connected with the time resolution fluorescence detection module and the fluorescence wavelength dispersion detection module through signal wires and is in communication connection with the computer;

the electronic circuit module also comprises a power supply module, a signal acquisition module and a time sequence module; the signal acquisition module is in communication connection with the time sequence module and is respectively and electrically connected with the power supply module; the time sequence module is used for controlling the signal acquisition module to synchronize the acquisition signal of the first fluorescence with the emission signal of the ultraviolet pulse excitation light path.

6. A method of measuring the content of uranium in a solution using the uranium content measuring device according to any one of claims 1 to 5, comprising:

when the uranium content is measured by adopting a time-resolved fluorescence measurement method, taking the uranium content measured by the time-resolved fluorescence measurement method as a first preliminary measurement result;

calculating a first difference between the first preliminary measurement and a maximum endpoint value of the first concentration range;

if the first difference is larger than a threshold value, determining the preliminary measurement result as the final uranium content;

if the first difference value is smaller than the threshold value, determining the uranium content by adopting a wavelength dispersion measurement method to obtain a second uranium content measurement result;

taking the second uranium content measurement result as a final uranium content;

when the uranium content is measured by adopting a wavelength dispersion measurement method, taking the uranium content measured by the wavelength dispersion measurement method as a second primary measurement result;

calculating a second difference between the second preliminary measurement and a minimum endpoint value of the second concentration range;

if the second difference is greater than the threshold, determining the second preliminary measurement result as a final uranium content;

if the second difference is smaller than the threshold value, determining the uranium content by adopting a time-resolved fluorescence measurement method to obtain a third uranium content measurement result;

taking the third uranium content measurement as the final uranium content.

7. The method according to claim 6, wherein the uranium content is measured by a time-resolved fluorescence measurement method, and the uranium content measured by the time-resolved fluorescence measurement method is used as a first preliminary measurement result, and the method specifically comprises:

adding a fluorescence enhancement solution with a preset concentration and a quantitative volume into a fluorescence cuvette to obtain a first solution;

obtaining the fluorescence intensity of the first solution by adopting a time-resolved fluorescence measurement method;

adding a uranium standard solution with a preset concentration and a quantitative volume into the first solution to obtain a second solution;

obtaining the fluorescence intensity of the second solution by adopting a time-resolved fluorescence measurement method;

adding a quantitative volume of the uranium-containing solution to be detected into the second solution to obtain a third solution;

obtaining the fluorescence intensity of the third solution by adopting a time-resolved fluorescence measurement method;

and calculating to obtain the first preliminary measurement result according to the fluorescence intensity of the first solution, the fluorescence intensity of the second solution, the fluorescence intensity of the third solution and the preset concentration of the uranium standard solution.

8. The method for measuring the uranium content according to claim 7, wherein the obtaining of the fluorescence intensity of the first solution by using a time-resolved fluorescence measurement method specifically comprises:

performing area integration on the single ultraviolet pulse excitation light path trigger attenuation time and the fluorescence attenuation intensity to obtain a single pulse fluorescence intensity, wherein the fluorescence attenuation intensity is the first solution fluorescence intensity corresponding to the single ultraviolet pulse excitation light path trigger attenuation time;

and summing the fluorescence intensities of the plurality of single pulses obtained within the preset time for acquiring the fluorescence intensity of the first solution to obtain the fluorescence intensity of the first solution.

9. The method according to claim 6, wherein when the uranium content is measured by using the wavelength dispersion measurement method, taking the uranium content measured by using the wavelength dispersion measurement method as a second preliminary measurement result specifically comprises:

adding a fluorescence enhancement solution with a preset concentration and a quantitative volume and a uranium standard solution with a preset concentration and a quantitative volume into a fluorescence cuvette to obtain a fourth solution;

obtaining the fluorescence intensity of the fourth solution by adopting a wavelength dispersion measurement method;

adding a uranium standard solution with preset concentration and a set multiple quantitative volume into the fourth solution to obtain a fifth solution;

obtaining the fluorescence intensity of the fifth solution by adopting a wavelength dispersion measurement method;

adding a quantitative volume of uranium-containing solution to be detected into the fourth solution to obtain a sixth solution;

obtaining the fluorescence intensity of the sixth solution by adopting a wavelength dispersion measurement method;

and calculating to obtain the second preliminary measurement result according to the fluorescence intensity of the fourth solution, the fluorescence intensity of the fifth solution, the fluorescence intensity of the sixth solution and the quantitative volume of the uranium-containing solution to be measured.

10. A method according to claim 9 for measuring the uranium content, wherein the obtaining of the fluorescence intensity of the fourth solution by a wavelength dispersion measurement method specifically comprises:

calculating the average value of the fluorescence intensities of a plurality of fourth solutions obtained within the preset time for collecting the fluorescence intensity of the fourth solution;

the mean value is taken as the fluorescence intensity of the new fourth solution.

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