CN103115911A - Closed type fluorescence analyzer - Google Patents
Closed type fluorescence analyzer Download PDFInfo
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- CN103115911A CN103115911A CN2013100694501A CN201310069450A CN103115911A CN 103115911 A CN103115911 A CN 103115911A CN 2013100694501 A CN2013100694501 A CN 2013100694501A CN 201310069450 A CN201310069450 A CN 201310069450A CN 103115911 A CN103115911 A CN 103115911A
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Abstract
The invention belongs to the technical field of analytical chemistry, and particularly relates to a closed type fluorescence analyzer consists of a sample chamber system, a light source control system and a spectrograph, and is characterized is that the sample chamber system comprises a sample chamber, a light source, a light filter and a focusing lens, wherein the light source, the light filter and the focusing lens are fixed on a sample cell bracket in the sample chamber; the sample chamber is arranged in a glove box; the light source control system, the spectrograph and a computer are arranged outside the glove box; and the spectrograph is connected with the sample chamber by an optical fiber. The closed type fluorescence analyzer has the characteristics of being convenient in protection, easy to maintain, high in sensitivity and suitable for analyzing the measured aftertreatment sample.
Description
Technical field
The invention belongs to technical field of analytical chemistry, be specifically related to a kind of closed fluorescence analyser.
Background technology
Fluorescence analyser can be used for the analysis of Simultaneous Determination of Trace Elements, because the feed liquid of nuclear fuel aftertreatment has the characteristics such as hot, highly acid, toxicity, complicated, trace, analyzes difficulty large, and analytical instrument is fragile.Therefore, the equipment that is applied to reprocessing analysis must be suitable for the particular surroundings of aftertreatment, just can guarantee precision of analysis, this has just proposed requirement to the instrument and equipment of aftertreatment: sample analysis must operate in the sealing system of protective equipment is arranged, and is easy to protection; Easily worn part is easily changed, for ease of maintenaince; It is high that the sensitivity of analytical instrument is wanted.
Traditional fluorescence analyser is unsuitable for reprocessing analysis, is mainly that the instrument performance index can descend because need integral sealing, the daily maintenance that is unfavorable for simultaneously instrument, and the volume of instrument is larger, takies limited space, hot cell, is not suitable for being directly used in nuclear fuel aftertreatment sample analysis.Therefore, be necessary to develop one be applicable to nuclear fuel aftertreatment industry can airtight analytic sample, the qualified special-purpose fluorescence analyzer of performance index is with the scope of application in reprocessing analysis and the practicality of expansion fluorescence analysis.
The concrete principle of existing fluorescence analyser is: light source enters optical fiber through coupling fiber and shines on sample, and the fluorescence that sample produces enters optical fiber through coupling fiber again, connects fluorescence detector with optical fiber, can realize the fluorescence analysis of sample.But according to the mechanism that fluorescence occurs, fluorescence intensity and incident intensity are proportional under certain condition, and existing optical coupling efficiency lower (5%～10%) makes the signal intensity that detector detects reduce by 10～20 times.Therefore, adopt Optical Fiber Transmission incident optical signal and fluorescence signal to reduce the incident light intensity, affect the fluorescence signal intensity that sample produces, reduced again the fluorescence signal intensity that detector is caught simultaneously, thereby affected the sensitivity of instrument.Therefore, be badly in need of a kind ofly can satisfying aftertreatment strong acid, hot environment, can improve again instrumental sensitivity, lowering apparatus signal to noise ratio (S/N ratio), realize the fluorescence analysis spectrometer of the analysis of trace element.
Summary of the invention
(1) goal of the invention
The invention provides a kind of with the isolation of sample chamber and spectrometer, be convenient to protect, for ease of maintenaince, highly sensitive, the fluorescence analyzer that is suitable for measuring the aftertreatment sample.
(2) technical scheme
For addressing the above problem, the present invention is achieved by the following technical solutions:
Closed fluorescence analyser is comprised of sample chamber system, light-source control system, spectrometer; The sample chamber system comprises sample chamber, light source, optical filter, condenser lens, and wherein light source, optical filter and condenser lens are fixed on sample cell support in the sample chamber, the sample chamber is positioned at glove box; Light-source control system, spectrometer and computer bit are outside glove box, and spectrometer is connected with the sample chamber by optical fiber, and this optical fiber is drawn from the glove box blind plate.
Its preferred version is:
The material of described glove box is stainless steel, is used for sealing sample chamber and radiation protection.
The material of described sample chamber is stainless steel, the inwall blacking.
Described sample cell support material has two vertical unthreaded holes of input path and emitting light path for black aluminium on this support; Colorimetric pool is settled two joining places, hole; Light source, optical filter, colorimetric pool are positioned at same axis in input path; Colorimetric pool, condenser lens are positioned at same axis at emitting light path.
What described light source adopted is the LED lamp, and mounting means adopts card slot type, and power is 30mW～1W, and this light source is the direct irradiation sample after optical filter filters;
Described light-source control system is constant current source, is arranged in spectrometer, and control reference voltage is 2～4V, and current stabilization is at 320mA;
What described optical filter adopted is that low strap is logical by the type optical filter, and mounting means adopts plug-in;
Described computing machine is equipped with the FreeAcid V1.0 of function software, is used for data acquisition and processing (DAP).
(3) beneficial effect
Adopt closed fluorescence analyser provided by the invention, have following beneficial effect:
(1) this luminoscope is separated with sample chamber and light-source control system, spectrometer, is conducive to maintenance and the replacing of instrument; The sample chamber is placed in glove box, has reduced the suffered radiation dose of staff;
(2) adopt great power LED etc. as light source and unconventional xenon lamp, mercury lamp, the monochromaticity of this light source is good, energy is strong, volume is little, the life-span is long and this light source is shone directly on sample after optical filtering, can improve incident intensity (10
2-10
3Times), thereby improve the fluorescence signal intensity of sample generation, the sensitivity that has improved instrument.
(3) adopt low ripple flow-through by optical filter, this optical filter transmission broadband is narrow, be elemental characteristic absorbing wavelength place ± 5nm to be measured, improved the monochromaticity of exciting light; The passband transmitance is high, and selected wavelength place average transmittance is greater than 90%; Low by the band transmitance, average transmittance is lower than 0.5%.This optical filter can make the exciting light of selected wavelength see through, and also can filter assorted scattered light, avoids assorted scattered light on the impact of fluorescence measurement.
Description of drawings
Fig. 1: closed fluorescence analyser sketch:
1. light source; 2. optical filter; 3. sample cell support; 4. colorimetric pool jack; 5. condenser lens; 6. sample chamber; 7. optical fiber; 8. spectrometer; 9. glove box;
Fig. 2: instrument light path schematic diagram.
Embodiment
Below in conjunction with specification drawings and specific embodiments, the present invention is further elaborated.
Closed fluorescence analyser is comprised of sample chamber system, light-source control system, spectrometer as shown in Figure 1; The sample chamber system comprises sample chamber, light source, optical filter, condenser lens, and wherein light source, optical filter and condenser lens are fixed on sample cell support in the sample chamber, the sample chamber is positioned at glove box; Light-source control system, spectrometer and computer bit are outside glove box, and spectrometer is connected with the sample chamber by optical fiber, and this optical fiber is drawn from the glove box blind plate.
The material of described glove box is stainless steel, is used for sealing sample chamber and radiation protection.
The material of described sample chamber is stainless steel, the inwall blacking.
Described sample cell support material has two vertical unthreaded holes of input path and emitting light path for black aluminium on this support; Colorimetric pool is settled two joining places, hole; Light source, optical filter, colorimetric pool are positioned at same axis in input path; Colorimetric pool, condenser lens are positioned at same axis at emitting light path.
What described light source adopted is the LED lamp, and mounting means adopts card slot type, and power is 30mW～1W;
Described light-source control system is constant current source, is arranged in spectrometer, and control reference voltage is 2～4V, and current stabilization is at 320mA;
What described optical filter adopted is that low strap is logical by the type optical filter, and mounting means adopts plug-in;
Described computing machine is equipped with the FreeAcid V1.0 of function software, is used for data acquisition and processing (DAP).
The index path of this analyser as shown in Figure 2, light source shines directly on sample after filtering, the fluorescence line focus lens focus that sample produces is laggard enters optical fiber, optical fiber is transferred to spectrometer with fluorescence signal, spectrometer receive the fluorescence signal contain sample message and as calculated machine process the fluorescence measurement of realizing sample.The intensity of light-source control system adjustable light sources be suitable for variable concentrations sample analysis.
Utilize closed fluorescence analyser provided by the invention to measure the thorium solution of variable concentrations, investigate the relation of sample concentration and fluorescence intensity.Measured the thorium solution of 6 variable concentrations.The equation of linear regression of working curve is y=87.533x+67.869, r＞0.999.Detect lower limit 0.1 ng/ml, the range of linearity of working curve is (0.1-100) ng/ml.According to document, the range of linearity of common fluorescence analyser is (1-10) ng/ml, detects lower limit 1 ng/ml.
The relation of table 1 thorium concentration and fluorescence intensity
| Thorium concentration ng/ml | Fluorescence intensity F |
| 0.1 | 120 |
| 0.5 | 320 |
| 1 | 153 |
| 5 | 480 |
| 10 | 750 |
| 50 | 4480 |
| 100 | 8823 |
| Equation of linear regression | ?y = 87.533x + 67.869 |
Result shows: closed fluorescence analyser is measured thorium solution, solution concentration and fluorescence intensity have good linear dependence, compare with existing fluorescence analyser, sensitivity and sensing range all are enhanced, the range of linearity improves 2 orders of magnitude, detect lower limit and reduced by 10 times, illustrate that this measurement device aftertreatment sample is feasible.
Claims (8)
1. closed fluorescence analyser, this analyser is comprised of sample chamber system, light-source control system and spectrometer, it is characterized in that, the sample chamber system comprises sample chamber, light source, optical filter, condenser lens, and wherein light source, optical filter and condenser lens are fixed on sample cell support in the sample chamber, the sample chamber is positioned at glove box; Light-source control system, spectrometer and computer bit are outside glove box, and spectrometer is connected with the sample chamber by optical fiber.
2. closed fluorescence analyser according to claim 1, is characterized in that, the material of described glove box is stainless steel, is used for sealing sample chamber and radiation protection.
3. closed fluorescence analyser according to claim 1, is characterized in that, the material of described sample chamber is stainless steel, the inwall blacking.
4. closed fluorescence analyser according to claim 1, is characterized in that, described sample cell support material has two vertical unthreaded holes of input path and emitting light path for black aluminium on this support; Colorimetric pool is settled two joining places, hole; Light source, optical filter, colorimetric pool are positioned at same axis in input path; Colorimetric pool, condenser lens are positioned at same axis at emitting light path.
5. closed fluorescence analyser according to claim 1, is characterized in that, what described light source adopted is the LED lamp, and mounting means adopts card slot type, and power is 30mW～1W, and this light source is the direct irradiation sample after optical filter filters.
6. closed fluorescence analyser according to claim 1, is characterized in that, described light-source control system is constant current source, is arranged in spectrometer, and the voltage range that this control system is controlled light source is 2～4V, and current stabilization is at 320mA.
7. closed fluorescence analyser according to claim 1, is characterized in that, what described optical filter adopted is that low strap is logical by the type optical filter, and mounting means adopts plug-in.
8. closed fluorescence analyser according to claim 1, is characterized in that, described computing machine is equipped with the FreeAcid V1.0 of function software, is used for data acquisition and processing (DAP).
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| CN201310069450.1A CN103115911B (en) | 2013-03-05 | 2013-03-05 | Closed type fluorescence analyzer |
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| CN201310069450.1A CN103115911B (en) | 2013-03-05 | 2013-03-05 | Closed type fluorescence analyzer |
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| CN103115911B CN103115911B (en) | 2015-03-11 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109623881A (en) * | 2018-12-26 | 2019-04-16 | 中国原子能科学研究院 | Lighting device for glove box |
| CN111175236A (en) * | 2020-01-09 | 2020-05-19 | 中国原子能科学研究院 | Light path correction method and device for baseline drift in glove box type online spectral analysis |
| CN113358650A (en) * | 2021-06-01 | 2021-09-07 | 浙江大学 | 96-hole microporous plate reader |
| CN113358650B (en) * | 2021-06-01 | 2024-04-16 | 浙江大学 | 96 hole micropore board reader |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109623881A (en) * | 2018-12-26 | 2019-04-16 | 中国原子能科学研究院 | Lighting device for glove box |
| CN111175236A (en) * | 2020-01-09 | 2020-05-19 | 中国原子能科学研究院 | Light path correction method and device for baseline drift in glove box type online spectral analysis |
| CN113358650A (en) * | 2021-06-01 | 2021-09-07 | 浙江大学 | 96-hole microporous plate reader |
| CN113358650B (en) * | 2021-06-01 | 2024-04-16 | 浙江大学 | 96 hole micropore board reader |
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