CN103115911B - Closed type fluorescence analyzer - Google Patents
Closed type fluorescence analyzer Download PDFInfo
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- CN103115911B CN103115911B CN201310069450.1A CN201310069450A CN103115911B CN 103115911 B CN103115911 B CN 103115911B CN 201310069450 A CN201310069450 A CN 201310069450A CN 103115911 B CN103115911 B CN 103115911B
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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, and the feed liquid due to nuclear fuel aftertreatment has the features such as hot, highly acid, toxicity, complicated, trace, and analyze difficulty large, analytical instrument is fragile.Therefore, the equipment being applied to reprocessing analysis must be suitable for the particular surroundings of aftertreatment, just can guarantee precision of analysis, this just proposes requirement to the instrument and equipment of aftertreatment: sample analysis must operate in the sealing system having protective equipment, is easy to protection; Easily worn part is easily changed, for ease of maintenaince; The sensitivity of analytical instrument wants high.
Traditional fluorescence analyser is unsuitable for reprocessing analysis, and mainly because need integral sealing, instrument performance index can decline, be unfavorable for the daily maintenance of instrument simultaneously, and the volume of instrument is comparatively large, takies limited space, hot cell, is not suitable for being directly used in nuclear fuel aftertreatment sample analysis.Therefore, being necessary that development one is applicable to nuclear fuel aftertreatment industry can sealed assay sample, and the qualified special fluorescence analyzer of performance index is to expand the scope of application in reprocessing analysis and the practicality of 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, uses Fiber connection fluorescence detector, can realize the fluorescence analysis of sample.But according to the mechanism that fluorescence occurs, under certain condition fluorescence intensity and incident intensity proportional, and existing optical coupling efficiency lower (5% ~ 10%), the signal intensity that detector is detected reduces 10 ~ 20 times.Therefore, adopt Optical Fiber Transmission incident optical signal and fluorescence signal to reduce the intensity of incident light, affect the fluorescence signal intensity that sample produces, again reduce the fluorescence signal intensity that detector is caught simultaneously, thus affect the sensitivity of instrument.Therefore, be badly in need of one and can meet aftertreatment strong acid, hot environment, instrumental sensitivity, lowering apparatus signal to noise ratio (S/N ratio) can be improved again, 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 by sample chamber and spectrometer isolation, be convenient to protect, for ease of maintenaince, highly sensitive, the fluorescence analyzer that is suitable for measuring aftertreatment sample.
(2) technical scheme
For solving the problem, the present invention is achieved by the following technical solutions:
Closed fluorescence analyser is made up of sample chamber system, light-source control system, spectrometer; Sample chamber system comprises sample chamber, light source, optical filter, condenser lens, and on the sample cell support that wherein light source, optical filter and condenser lens are fixed in sample chamber, sample chamber is positioned at glove box; Light-source control system, spectrometer and computer bit are outside glove box, and spectrometer is connected with sample chamber by optical fiber, and this optical fiber is drawn from glove box blind plate.
its preferred version is:
The material of described glove box is stainless steel, for closed sample chamber and radiation protection.
The material of described sample chamber is stainless steel, inwall blacking.
Described sample cell support material is black aluminium, this support has input path and emitting light path two vertical unthreaded holes; Colorimetric pool settles holes joining place; 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 LED, and mounting means adopts card slot type, and power is 30mW ~ 1W, and this light source is 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 type optical filter, and mounting means adopts plug-in;
Described computing machine is equipped with function software FreeAcid V1.0, for data acquisition and processing (DAP).
(3) beneficial effect
Adopt closed fluorescence analyser provided by the invention, there is following beneficial effect:
(1) this luminoscope is by separated to sample chamber and light-source control system, spectrometer, is conducive to maintenance and the replacing of instrument; Sample chamber is placed in glove box, reduces radiation dose suffered by staff;
(2) adopt great power LED etc. as light source 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 shine directly on sample by this light source after optical filtering, can improve incident intensity (10
2-10
3times), thus improve the fluorescence signal intensity that sample produces, the sensitivity that improve instrument.
(3) adopt low ripple flow-through by optical filter, this filter transmission broadband is narrow, be elemental characteristic absorbing wavelength place ± 5nm to be measured, improve the monochromaticity of exciting light; Passband transmitance is high, selects given wavelength average transmittance to be greater than 90%; Low by band transmitance, average transmittance is lower than 0.5%.This optical filter can make the exciting light of selected wavelength through, also can filter assorted scattered light, avoid assorted scattered light on the impact of fluorescence measurement.
Accompanying drawing explanation
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 as shown in Figure 1, is made up of sample chamber system, light-source control system, spectrometer; Sample chamber system comprises sample chamber, light source, optical filter, condenser lens, and on the sample cell support that wherein light source, optical filter and condenser lens are fixed in sample chamber, sample chamber is positioned at glove box; Light-source control system, spectrometer and computer bit are outside glove box, and spectrometer is connected with sample chamber by optical fiber, and this optical fiber is drawn from glove box blind plate.
The material of described glove box is stainless steel, for closed sample chamber and radiation protection.
The material of described sample chamber is stainless steel, inwall blacking.
Described sample cell support material is black aluminium, this support has input path and emitting light path two vertical unthreaded holes; Colorimetric pool settles holes joining place; 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 LED, 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 type optical filter, and mounting means adopts plug-in;
Described computing machine is equipped with function software FreeAcid V1.0, 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, sample produce fluorescence line focus lens focus laggard enter optical fiber, fluorescence signal is transferred to spectrometer by optical fiber, spectrometer receive containing sample message fluorescence signal and as calculated machine process realize the fluorescence measurement of sample.The intensity of light-source control system adjustable light sources be suitable for variable concentrations sample analysis.
embodiment 1
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.Measure the thorium solution of 6 variable concentrations.The equation of linear regression of working curve is y=87.533x+67.869, r > 0.999.Monitoring lower-cut 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 fluorescent analyser is (1-10) ng/ml, Monitoring lower-cut 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 measures thorium solution, solution concentration and fluorescence intensity have good linear dependence, compared with existing fluorescence analyser, sensitivity and sensing range are all enhanced, the range of linearity improves 2 orders of magnitude, Monitoring lower-cut reduces 10 times, illustrates that this measurement device aftertreatment sample is feasible.
Claims (7)
1. closed fluorescence analyser, this analyser is made up of sample chamber system, light-source control system and spectrometer, it is characterized in that, sample chamber system comprises sample chamber, light source, optical filter, condenser lens, and on the sample cell support that wherein light source, optical filter and condenser lens are fixed in sample chamber, sample chamber is positioned at glove box; Light-source control system, spectrometer and computer bit are outside glove box, and spectrometer is connected with sample chamber by optical fiber, and described sample cell support material is black aluminium, this support have input path and emitting light path two vertical unthreaded holes; Colorimetric pool settles holes joining place; 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.
2. closed fluorescence analyser according to claim 1, is characterized in that, the material of described glove box is stainless steel, for closed 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, inwall blacking.
4. closed fluorescence analyser according to claim 1, is characterized in that, what described light source adopted is LED, and mounting means adopts card slot type, and power is 30mW ~ 1W, and this light source is direct irradiation sample after optical filter filters.
5. 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 controls light source is 2 ~ 4V, and current stabilization is at 320mA.
6. closed fluorescence analyser according to claim 1, is characterized in that, what described optical filter adopted is that low strap is logical by type optical filter, and mounting means adopts plug-in.
7. closed fluorescence analyser according to claim 1, is characterized in that, described computing machine is equipped with function software FreeAcid V1.0, for data acquisition and processing (DAP).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 true CN103115911B (en) | 2015-03-11 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109623881B (en) * | 2018-12-26 | 2021-07-30 | 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 |
| CN113358650B (en) * | 2021-06-01 | 2024-04-16 | 浙江大学 | 96 hole micropore board reader |
| CN117826233A (en) * | 2023-12-14 | 2024-04-05 | 中国核电工程有限公司 | Device for radioactive sample analysis and use method |
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| JP3346095B2 (en) * | 1995-05-17 | 2002-11-18 | ミノルタ株式会社 | Spectrophotometer |
| FI103434B1 (en) * | 1996-04-22 | 1999-06-30 | Wallac Oy | Multi-Seal Device |
| WO2003023379A1 (en) * | 2001-09-12 | 2003-03-20 | Apprise Technologies, Inc. | Multichannel fluorosensor |
| CN1566910A (en) * | 2003-07-10 | 2005-01-19 | 上海复生生物工程研究所有限公司 | Fluorescence detecting instrument |
| CN101806737A (en) * | 2010-04-23 | 2010-08-18 | 上海互帼科学仪器有限公司 | Portable fluorescence detector |
| CN201740737U (en) * | 2010-05-18 | 2011-02-09 | 中国计量学院 | Integrating sphere fluoroscopic detection device based on LED light source |
| CN102253024B (en) * | 2011-06-08 | 2013-03-20 | 中国农业大学 | Optical dissolved oxygen sensor |
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