CN212964628U - High-sensitivity in-situ uranium content determinator based on multiple light sources - Google Patents
High-sensitivity in-situ uranium content determinator based on multiple light sources Download PDFInfo
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- CN212964628U CN212964628U CN202021980381.1U CN202021980381U CN212964628U CN 212964628 U CN212964628 U CN 212964628U CN 202021980381 U CN202021980381 U CN 202021980381U CN 212964628 U CN212964628 U CN 212964628U
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Abstract
The utility model belongs to the technical field of the uranium content detects, concretely relates to high sensitivity uranium content on-site measurement appearance based on many light sources. The device is based on a characteristic fluorescence principle of uranyl ion-fluorescence intensifier complexes, adopts a plurality of UV-LEDs as light sources, takes a miniaturized photomultiplier or a silicon photomultiplier as a photoelectric conversion element, and takes a fluorescence cuvette as a measuring pool. The light intensity of the excitation light source is improved, the detection limit can be reduced by several times, the technical difficulty of the sensitivity of the field uranium detector is solved, and the volume and the power consumption of the device are greatly reduced.
Description
Technical Field
The utility model belongs to the technical field of the uranium content detects, concretely relates to high sensitivity uranium content on-site measurement appearance based on many light sources.
Background
With the rapid development of nuclear power and military industry, the demand of the countries in the world for natural uranium also begins to rise greatly, and larger uranium ore development heat is formed, however, the following problem is that the quantity and the types of radioactive wastewater generated in the uranium ore mining and uranium hydrometallurgy processes are more and more. The radioactive wastewater for uranium mining and metallurgy in China has the characteristics of low concentration, large quantity, wide pollution area and the like, contains natural radioactive elements with long half-life periods such as uranium, thorium and radium, and can pollute surface water if the radioactive wastewater is not directly discharged after treatment, and can slowly permeate into the underground to cause pollution of underground water, so that the radioactive wastewater is expanded to a whole biosphere, and finally causes harm to two aspects of chemical toxicity and radiation to people and animals. Therefore, the method is very important for detecting the content of uranium and other radionuclides in various environmental water bodies, and is concerned with the national ecological environment safety and the health of people. Besides laboratory instrument and method confirmation, the method and tool for field detection are indispensable, the data of field detection can quickly reflect the quality of the environmental water body, effective data are provided for government supervision, environmental management and enterprise pollution discharge, and key data can be provided for research and judgment of emergencies and provision of emergency measures.
The current detection technology aiming at uranium in environmental water bodies comprises a laser fluorescence method, a spectrophotometry method, an inductively coupled plasma photometry method, an inductively coupled plasma mass spectrometry (ICP-MS) and the like. The spectrophotometry requires sample pretreatment of multiple steps, including extraction, back extraction, masking, color development and the like, is relatively complex to operate, has low detection sensitivity although being widely applied, and is difficult to realize field detection. The laser fluorescence method has high sensitivity which can reach 0.02 mu g/L, but the portable detection is difficult to realize due to the large volume of the laser; in addition, ICP-MS can realize multi-element detection, but is only suitable for a laboratory environment and cannot be the preferred method for field portable equipment.
With the development of novel solid light sources such as ultraviolet diodes (UV-LEDs) and laser diodes, the miniaturization of light sources provides new ideas and development directions for the miniaturization and portability of detection equipment. At present, the shortest wavelength of the UV-LED can reach 250nm, the service life of the UV-LED reaches 10000 hours, but the UV-LED is not as good as the laser in the aspects of light source intensity, light source convergence capacity and the like. However, the on-site uranium detection equipment only aims at the uranium content in the discharged sewage, generally requires 0.05mg/L and is far higher than the detection limit of a laser uranium detection instrument, so the detection limit of the on-site uranium detection equipment is not high. Therefore, the UV-LED can be completely used as an excitation light source for the field uranium analyzer. Besides patent reports, no report and application of the UV-LED in the field uranium detector are found.
SUMMERY OF THE UTILITY MODEL
The utility model aims at above-mentioned drawback, provide a high sensitivity uranium content field measurement appearance based on many light sources, based on uranyl ion-fluorescence intensifier complex characteristic fluorescence principle, adopt a plurality of UV-LED to be the light source to miniaturized photomultiplier or silicon photomultiplier are as photoelectric conversion component, use the fluorescence cell as the measuring cell. The light intensity of the excitation light source is improved, the detection limit can be reduced by several times, the technical difficulty of the sensitivity of the field uranium detector is solved, and the volume and the power consumption of the device are greatly reduced.
The technical scheme of the utility model as follows:
a high-sensitivity in-situ uranium content tester based on multiple light sources comprises four UV-LEDs, an LED temperature control module, a square bottom light-transmitting fluorescent cuvette, a photosensitive element, a fluorescent detection optical filter, a circuit system and a light-shading outer cover; the four UV-LEDs are fixed on the bottom plate in the shading outer cover through the frame, the four UV-LEDs are respectively vertical to four vertical surfaces of the square bottom light-transmitting fluorescent cuvette in fixed positions, light main shafts emitted by the UV-LEDs are vertical to the vertical surfaces of the cuvette and are positioned on the same plane, and the cross points of the light main shafts are positioned in the square bottom light-transmitting fluorescent cuvette;
the outer edge of the square bottom light-transmitting fluorescent cuvette is fixed in a wrapping mode through a frame, the frame is in a hollow mode, and optical fibers can reach four surfaces of the square bottom light-transmitting fluorescent cuvette through the frame; the frame is fixed on the photosensitive element, so that a gap is reserved between the bottom of the square bottom light-transmitting fluorescent cuvette and the upper part of the photosensitive element;
the photosensitive element is controlled by a circuit system, the converted fluorescence signals are interpreted according to the frequency of a UV-LED pulse light source and the fluorescence lifetime of uranyl ions, wherein the pulse frequency of the UV-LED and the pulse frequency of the optical signals extracted by the photosensitive element are consistent, and the phase delay of the optical signals extracted by the photosensitive element is 1-100 mu s.
And the distance between each UV-LED and each side surface of the square bottom light-transmitting fluorescent cuvette is 0.1-10 mm.
The photosensitive element is a photomultiplier tube.
The light-sensitive element is a silicon photomultiplier, a sensitive light window of the light-sensitive element is used for collecting fluorescent signals excited by the UV-LED, the light-sensitive element is positioned at the bottom of the square bottom light-transmitting fluorescent cuvette, and the axial direction of the light-sensitive element and the main axis of light of the UV-LED form an angle of 90 degrees.
The photosensitive element is a silicon photocell.
The photosensitive element is a photodiode.
The fluorescence detection optical filter is placed on the photosensitive element, the central wavelength range is 450-560 nm, and the distance between the fluorescence detection optical filter and the bottom of the square bottom light-transmitting fluorescence cuvette is 0.1-10 mm.
The central wavelength of the UV-LED is 240-400nm, the power is 10mW-4W, and the constant current source supplies power.
The UV-LED power supply adopts a pulse modulation mode, the frequency is 10-1000 Hz, and the duty ratio is 1: 2-1: 999.
The temperature of the UV-LED is accurately controlled by the LED temperature control module, and is between room temperature and 70 ℃.
The beneficial effects of the utility model reside in that:
the utility model adopts multiple light sources to excite, has higher sensitivity, and can adjust the intensity of the light source according to the field requirement, so that the detection result is more accurate; meanwhile, the device is small in size and low in power, and can completely realize the field detection of uranium in an environmental sample.
The utility model discloses the UV-LED who adopts is novel solid-state miniaturized light source, and the good spectral bandwidth of the light monochromaticity that it sent is narrower (being less than 10nm), and is small, longe-lived, especially adopts deep ultraviolet regional LED (250) and supple with energy 300nm), just in time falls in the best excitation wavelength of uranyl ion and fluorescence reinforcing agent complex, and the fluorescence of arousing is stronger, and the optical noise that LED arouses is very little with undulant, is particularly suitable for the measurement of the weak signal of fluorescence, effectively improves the SNR, improve sensitivity.
Drawings
FIG. 1 is a top view of a high-sensitivity uranium content on-site measuring instrument based on multiple light sources;
fig. 2 is a partial perspective view of the present invention.
In the figure: 1; a UV-LED; 2. a square bottom light-transmitting cuvette; 3. a photosensitive element; 4. an LED temperature control module; 5. circuitry; 6. a fluorescence detection filter 6.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
A high-sensitivity in-situ uranium content determinator based on multiple light sources comprises four UV-LEDs 1, an LED temperature control module 4, a square bottom light-transmitting fluorescent cuvette 2, a photosensitive element 3, a fluorescent detection optical filter 6, a circuit system 5 and a light-shading outer cover. The four UV-LEDs are fixed on the bottom plate inside the shading outer cover through the frame, the four UV-LEDs are respectively perpendicular to four vertical surfaces of the square bottom light-transmitting fluorescent cuvette 2 in fixed positions, a light main shaft sent by the UV-LED1 is perpendicular to the vertical surfaces of the cuvette and is positioned on the same plane, and the cross point of the light main shaft is positioned in the square bottom light-transmitting fluorescent cuvette 2. The outer edge of the square bottom light-transmitting fluorescent cuvette 2 is fixed in a wrapping mode through a frame, the frame is in a hollow mode, and optical fibers can reach four faces of the square bottom light-transmitting fluorescent cuvette 2 through the frame; the frame is fixed on the photosensitive element 3, so that a gap is reserved between the bottom of the square bottom light-transmitting fluorescent cuvette 2 and the upper part of the photosensitive element 3.
The distance between each UV-LED1 and each side face of the square bottom light-transmitting fluorescent cuvette 2 is 0.1-10 mm.
The photosensitive element 3 can be a photomultiplier tube, a silicon photomultiplier, a silicon photocell, or a photodiode. The sensitive light window of the photosensitive element 3 is used for collecting a fluorescent signal excited by the UV-LED1, the photosensitive element 3 is positioned at the bottom of the square bottom light-transmitting fluorescent cuvette 2, and the axial direction of the photosensitive element 3 forms an angle of 90 degrees with the main axis of the light of the UV-LED 1.
The central wavelength of the UV-LED1 is 240-400nm, the power is 10mW-4W, and the constant current source supplies power. The UV-LED1 power supply adopts a pulse modulation mode, the frequency is 10-1000 Hz, and the duty ratio is 1: 2-1: 999. The lamp turning-on and lamp turning-off time of the UV-LED1 is consistent under the control of the circuit system 5, and any number of the UV-LEDs 1 can be selected to be turned on. The temperature of the UV-LED1 is accurately controlled by the LED temperature control module 4, and is between room temperature and 70 ℃.
The fluorescence detection optical filter 6 is placed on the photosensitive element 3, the central wavelength range is 450-560 nm, and the distance between the fluorescence detection optical filter 6 and the bottom of the square bottom light-transmitting fluorescence cuvette 2 is 0.1-10 mm.
The photosensitive element 3 is controlled by the circuit system 5, the converted fluorescence signals are interpreted according to the frequency of a UV-LED1 pulse light source and the fluorescence lifetime of uranyl ions, wherein the UV-LED1 is consistent with the pulse frequency of the optical signals extracted by the photosensitive element, and the phase delay of the optical signals extracted by the photosensitive element is 1-100 mu s.
The actual operation process does, gets a quantitative sample (like river or lake water) or standard solution, puts into the cell, and the fluorescence reinforcing agent is added to the ration again, and the stirring is even in the fluorescence cell, puts into the fluorescence cell again the utility model discloses a cell fixing device opens ultraviolet emitting diode, detects fluorescence intensity by light sensitive element, surveys the uranium content in the sample through standard curve method or standard joining method.
Example 1
A high-sensitivity in-situ uranium content determinator based on multiple light sources is characterized in that an excitation light source is 4 UV-LEDs 1, the center wavelength of the excitation light source is 360nm, the rated current is 100mA, the divergence angle is 120 degrees, a power supply is 100Hz, and the duty ratio is 1: 49. The UV-LED1 adopts an aluminum heat sink, and the heat productivity is small due to the low duty ratio, so that the heat efficiency can be improved by a common heat sink. The distance between the UV-LED1 and the square bottom light-transmitting fluorescent cuvette 2 was 1 mm. The central wavelength of the fluorescence detection filter 6 is 510nm, the bandwidth is 10nm, and the distance between the fluorescence detection filter 6 and the photomultiplier is 1 mm. Since the fluorescence lifetime of the complex of uranyl ion and fluorescence enhancer is several tens to several hundreds of μ s, 50 μ s is selected as the delay time. And (3) synchronously carrying out delayed pulse acquisition on the fluorescence signal of the uranyl ion according to the pulse characteristic of the light source. The repeatability of the instrument for detecting the uranyl ions is less than 8%, the detection sensitivity reaches 0.2 mu g/L and is less than 50 mu g/L of the wastewater discharge standard.
Example 2
A high-sensitivity in-situ uranium content determinator based on multiple light sources is characterized in that an excitation light source is 2 UV-LEDs 1, the central wavelength of the excitation light source is 320nm, the rated current is 50mA, a power supply of a light emitting diode is 500Hz, and the duty ratio is 1: 19. The UV-LED1 adopts an aluminum heat sink, the heat sink does not need a fan, and the power is low and the temperature is stable. The intensity of ultraviolet light emitted by the UV-LED1 light source can be detected in real time, the detector can be directly used for measuring when the detector is started, and time consumed by starting preheating operation is saved. The distance between the UV-LED1 and the square bottom light-transmitting fluorescent cuvette 2 was 0.5 mm. The central wavelength of the fluorescence detection filter 6 is 510nm, the bandwidth is 10nm, and the distance between the fluorescence detection filter 6 and the photomultiplier is 0.5 mm. The circuit system carries out follow-up light source pulse type collection on the fluorescent signals, and the delay time is 50 mu s. The repeatability of the portable equipment for detecting the uranyl ions is less than 4%, the detection sensitivity reaches 0.5 mu g/L and is less than 50 mu g/L of the wastewater discharge standard.
The embodiments described above are merely illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the invention but rather to conform to the broadest scope consistent with the principles and novel features disclosed herein. Various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention shall fall within the scope of the present invention defined by the claims.
Claims (10)
1. A high-sensitivity in-situ uranium content tester based on multiple light sources comprises four UV-LEDs, an LED temperature control module, a square bottom light-transmitting fluorescent cuvette, a photosensitive element, a fluorescent detection optical filter, a circuit system and a light-shading outer cover; the method is characterized in that:
the four UV-LEDs are fixed on the bottom plate in the light-shading outer cover through the frame, the four UV-LEDs are respectively vertical to four vertical surfaces of the square bottom light-transmitting fluorescent cuvette in fixed positions, light main shafts emitted by the UV-LEDs are vertical to the vertical surfaces of the cuvette and are positioned on the same plane, and the cross points of the light main shafts are positioned in the square bottom light-transmitting fluorescent cuvette;
the outer edge of the square bottom light-transmitting fluorescent cuvette is fixed in a wrapping mode through a frame, the frame is in a hollow mode, and optical fibers can reach four surfaces of the square bottom light-transmitting fluorescent cuvette through the frame; the frame is fixed on the photosensitive element, so that a gap is reserved between the bottom of the square bottom light-transmitting fluorescent cuvette and the upper part of the photosensitive element;
the photosensitive element is controlled by a circuit system, the converted fluorescence signals are interpreted according to the frequency of a UV-LED pulse light source and the fluorescence lifetime of uranyl ions, wherein the pulse frequency of the UV-LED and the pulse frequency of the optical signals extracted by the photosensitive element are consistent, and the phase delay of the optical signals extracted by the photosensitive element is 1-100 mu s.
2. The multi-light-source-based high-sensitivity in-situ uranium content determinator of claim 1, wherein: the distance between each UV-LED and each side face of the square bottom light-transmitting fluorescent cuvette is 0.1-10 mm.
3. The multi-light-source-based high-sensitivity in-situ uranium content determinator of claim 1, wherein: the photosensitive element is a photomultiplier tube.
4. The multi-light-source-based high-sensitivity in-situ uranium content determinator of claim 3, wherein: the light-sensitive element is a silicon photomultiplier, a sensitive light window of the light-sensitive element is used for collecting fluorescent signals excited by the UV-LED, the light-sensitive element is positioned at the bottom of the square bottom light-transmitting fluorescent cuvette, and the axial direction of the light-sensitive element and the main axis of light of the UV-LED form an angle of 90 degrees.
5. The multi-light-source-based high-sensitivity in-situ uranium content determinator of claim 3, wherein: the photosensitive element is a silicon photocell.
6. The multi-light-source-based high-sensitivity in-situ uranium content determinator of claim 3, wherein: the photosensitive element is a photodiode.
7. The multi-light-source-based high-sensitivity in-situ uranium content determinator of claim 1, wherein: the fluorescence detection optical filter is placed on the photosensitive element, the central wavelength range is 450-560 nm, and the distance between the fluorescence detection optical filter and the bottom of the square bottom light-transmitting fluorescence cuvette is 0.1-10 mm.
8. The multi-light-source-based high-sensitivity in-situ uranium content determinator according to any one of claims 1 to 7, wherein: the central wavelength of the UV-LED is 240-400nm, the power is 10mW-4W, and the constant current source supplies power.
9. The multi-light-source-based high-sensitivity in-situ uranium content determinator according to any one of claims 1 to 7, wherein: the UV-LED power supply adopts a pulse modulation mode, the frequency is 10-1000 Hz, and the duty ratio is 1: 2-1: 999.
10. The multi-light-source-based high-sensitivity in-situ uranium content determinator according to any one of claims 1 to 7, wherein: the temperature of the UV-LED is accurately controlled by the LED temperature control module, and is between room temperature and 70 ℃.
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