CN103115911B - Closed type fluorescence analyzer - Google Patents
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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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- 230000003287 optical effect Effects 0.000 claims abstract description 15
- 239000013307 optical fiber Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 230000005855 radiation Effects 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims 1
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 13
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 238000012423 maintenance Methods 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 6
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 5
- 229910052776 Thorium Inorganic materials 0.000 description 5
- 238000012921 fluorescence analysis Methods 0.000 description 5
- 238000012805 post-processing Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 238000012958 reprocessing Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000003758 nuclear fuel Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013480 data collection Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
本发明属于分析化学技术领域，具体涉及一种封闭式荧光分析仪。该分析仪由样品室系统、光源控制系统及光谱仪组成，其特征在于，样品室系统包括样品室、光源、滤光片、聚焦透镜，其中光源、滤光片及聚焦透镜固定在样品室内的样品池支架上、样品室位于手套箱内；光源控制系统、光谱仪和计算机位于手套箱外，光谱仪通过光纤与样品室相连。该分析仪具有便于防护、易于维修、灵敏度高、适合于测量后处理样品分析的特点。
The invention belongs to the technical field of analytical chemistry, and in particular relates to a closed fluorescence analyzer. The analyzer is composed of a sample chamber system, a light source control system and a spectrometer. It is characterized in that the sample chamber system includes a sample chamber, a light source, an optical filter, and a focusing lens, wherein the light source, optical filter, and focusing lens are fixed on the sample in the sample chamber. On the cell support, the sample chamber is located in the glove box; the light source control system, the spectrometer and the computer are located outside the glove box, and the spectrometer is connected to the sample chamber through an optical fiber. The analyzer has the characteristics of convenient protection, easy maintenance, high sensitivity, and is suitable for analysis of post-measurement samples.
Description
技术领域 technical field
本发明属于分析化学技术领域，具体涉及一种封闭式荧光分析仪。 The invention belongs to the technical field of analytical chemistry, and in particular relates to a closed fluorescence analyzer.
背景技术 Background technique
荧光分析仪可用于多种痕量元素的分析，由于核燃料后处理的料液具有强放射性、强酸性、毒性、成份复杂、痕量等特点，分析难度大，分析仪器易损坏。因此，应用于后处理分析的设备必须适合于后处理的特殊环境，才能确保分析结果的准确性，这就对后处理的仪器设备提出了要求：样品分析必须在有防护设施的密封体系中操作，易于防护；易损部件容易更换，易于维修；分析仪器的灵敏度要高。 Fluorescence analyzers can be used for the analysis of various trace elements. Due to the characteristics of strong radioactivity, strong acidity, toxicity, complex components, and trace amounts of the feed liquid after nuclear fuel reprocessing, the analysis is difficult and the analysis equipment is easily damaged. Therefore, the equipment used in post-processing analysis must be suitable for the special environment of post-processing in order to ensure the accuracy of the analysis results, which puts forward requirements for post-processing equipment: sample analysis must be operated in a sealed system with protective facilities , easy to protect; easy to replace vulnerable parts, easy to maintain; the sensitivity of the analytical instrument should be high.
传统的荧光分析仪不适于后处理分析，主要是因为需要整体密封，仪器性能指标会下降，同时不利于仪器的日常维护保养，而且仪器的体积较大，占用有限的热室空间，不适合直接用于核燃料后处理样品分析。因此，有必要研制一台适用于核燃料后处理行业能够密闭分析样品，性能指标合格的专用荧光分析仪器以扩展荧光分析的在后处理分析中的适用范围和实用性。 The traditional fluorescence analyzer is not suitable for post-processing analysis, mainly because the overall sealing is required, the performance index of the instrument will drop, and it is not conducive to the daily maintenance of the instrument, and the instrument is large in size and occupies limited space in the hot chamber, so it is not suitable for direct For nuclear fuel reprocessing sample analysis. Therefore, it is necessary to develop a special fluorescence analysis instrument suitable for the nuclear fuel reprocessing industry, capable of airtight analysis of samples, and with qualified performance indicators, so as to expand the scope and practicability of fluorescence analysis in reprocessing analysis.
现有的荧光分析仪的具体原理为：光源经光纤耦合进入光纤照到样品上，样品产生的荧光再经光纤耦合进入光纤，用光纤连接荧光检测器，可实现样品的荧光分析。但是根据荧光发生的机理，在一定条件下荧光强度与入射光强度成正比关系，而现有的光纤耦合效率较低（5%～10%），使探测器检测到的信号强度降低了10～20倍。因此，采用光纤传输入射光信号和荧光信号降低了入射光的强度，影响样品产生的荧光信号强度，同时又降低了探测器捕获的荧光信号强度，从而影响仪器的灵敏度。因此，急需一种既能满足后处理强酸、强放射性环境，又能提高仪器灵敏度、降低仪器信噪比，实现痕量元素的分析的荧光分析谱仪。 The specific principle of the existing fluorescence analyzer is: the light source is coupled into the optical fiber through the optical fiber to illuminate the sample, the fluorescence generated by the sample is coupled into the optical fiber through the optical fiber, and the optical fiber is connected to the fluorescence detector to realize the fluorescence analysis of the sample. However, according to the mechanism of fluorescence, the fluorescence intensity is proportional to the incident light intensity under certain conditions, and the existing optical fiber coupling efficiency is low (5%-10%), which reduces the signal intensity detected by the detector by 10-10%. 20 times. Therefore, the use of optical fiber to transmit the incident light signal and the fluorescence signal reduces the intensity of the incident light, which affects the intensity of the fluorescence signal generated by the sample, and at the same time reduces the intensity of the fluorescence signal captured by the detector, thereby affecting the sensitivity of the instrument. Therefore, there is an urgent need for a fluorescence analysis spectrometer that can not only meet the post-treatment of strong acid and strong radioactive environments, but also improve the sensitivity of the instrument, reduce the signal-to-noise ratio of the instrument, and realize the analysis of trace elements.
发明内容 Contents of the invention
（一）发明目的(1) Purpose of the invention
本发明提供了一种将样品室和光谱仪隔离、便于防护、易于维修、灵敏度高、适合于测量后处理样品的荧光分析仪器。 The invention provides a fluorescence analysis instrument which isolates a sample chamber from a spectrometer, is convenient for protection, easy for maintenance, high in sensitivity and is suitable for measuring post-processing samples.
（二）技术方案(2) Technical solution
为解决上述问题，本发明是通过以下技术方案实现的： In order to solve the above problems, the present invention is achieved through the following technical solutions:
封闭式荧光分析仪由样品室系统、光源控制系统、光谱仪组成；样品室系统包括样品室、光源、滤光片、聚焦透镜，其中光源、滤光片及聚焦透镜固定在样品室内的样品池支架上、样品室位于手套箱内；光源控制系统、光谱仪和计算机位于手套箱外，光谱仪通过光纤与样品室相连，该光纤从手套箱盲板引出。 The closed fluorescence analyzer consists of a sample chamber system, a light source control system, and a spectrometer; the sample chamber system includes a sample chamber, a light source, a filter, and a focusing lens, where the light source, filter, and focusing lens are fixed on the sample cell bracket in the sample chamber The upper and sample chambers are located in the glove box; the light source control system, spectrometer and computer are located outside the glove box, and the spectrometer is connected to the sample chamber through an optical fiber, which is led out from the blind plate of the glove box.
其优选方案为：Its preferred scheme is:
所述的手套箱的材质为不锈钢，用于封闭样品室和辐射防护。 The material of the glove box is stainless steel, which is used for sealing the sample room and radiation protection.
所述的样品室的材料为不锈钢，内壁涂黑。 The material of the sample chamber is stainless steel, and the inner wall is painted black.
所述的样品池支架材质为黑铝，该支架上有入射光路和出射光路两个垂直光孔；比色池安置两孔相交点处；光源、滤光片、比色池在入射光路位于同一轴线；比色池、聚焦透镜在出射光路位于同一轴线。 The material of the sample cell support is black aluminum, and there are two vertical light holes on the support, the incident light path and the exit light path; the colorimetric cell is placed at the intersection of the two holes; The same axis; the colorimetric cell and focusing lens are located on the same axis in the exit light path.
所述的光源采用的是LED灯，安装方式采用卡槽式，功率为30mW～1W，该光源经滤光片滤光后直接照射样品； The light source used is an LED light, the installation method is a slot type, and the power is 30mW-1W. The light source directly illuminates the sample after being filtered by an optical filter;
所述的光源控制系统为恒流源，安装在光谱仪内，电压控制范围为2～4V，电流稳定在320mA； The light source control system is a constant current source installed in the spectrometer, the voltage control range is 2-4V, and the current is stable at 320mA;
所述的滤光片采用的是低带通截至型滤光片，安装方式采用插拔式； The filter used is a low-bandpass cut-off filter, and the installation method is plug-in;
所述的计算机装有操作软件FreeAcid V1.0，用于数据采集和处理。 The computer is equipped with operating software FreeAcid V1.0 for data collection and processing.
（三）有益效果(3) Beneficial effects
采用本发明提供的封闭式荧光分析仪，具有以下有益效果： The closed fluorescence analyzer provided by the invention has the following beneficial effects:
（1）该荧光仪将样品室与光源控制系统、光谱仪分割开来，有利于仪器的维修和更换；将样品室置于手套箱内，降低了工作人员所受辐射剂量； (1) The fluorometer separates the sample room from the light source control system and the spectrometer, which is conducive to the maintenance and replacement of the instrument; the sample room is placed in the glove box, which reduces the radiation dose of the staff;
（2）采用大功率LED等作为光源而非传统的氙灯、汞灯，该光源的单色性好、能量强、体积小、寿命长并且将该光源经滤光后直接照射到样品上，可提高入射光强度（102-103倍），从而提高样品产生的荧光信号强度、提高了仪器的灵敏度。 (2) High-power LEDs are used as light sources instead of traditional xenon lamps and mercury lamps. The light source has good monochromaticity, strong energy, small size, and long life, and the light source is directly irradiated on the sample after filtering. Increase the incident light intensity (10 2 -10 3 times), thereby increasing the fluorescence signal intensity generated by the sample and improving the sensitivity of the instrument.
（3）采用低波通型截至滤光片，此滤光片透射宽带窄、为待测元素特征吸收波长处±5nm，提高了激发光的单色性；通带透过率高，选定波长处平均透射率大于90%；截至带透过率低，平均透射率低于0.5%。此滤光片可使选定波长的激发光透过，还可滤掉杂散射光，避免杂散射光对荧光测量的影响。 (3) Low-wave pass type cut-off filter is adopted. This filter has a narrow transmission bandwidth and is ±5nm at the characteristic absorption wavelength of the element to be measured, which improves the monochromaticity of the excitation light; the passband transmittance is high, and the selected The average transmittance at the wavelength is greater than 90%; the cut-off band transmittance is low, and the average transmittance is less than 0.5%. This optical filter can transmit excitation light of selected wavelength, and can also filter out stray scattered light, so as to avoid the influence of stray scattered light on fluorescence measurement.
附图说明 Description of drawings
图1：封闭式荧光分析仪简图： Figure 1: A schematic diagram of a closed fluorescence analyzer:
1. 光源；2.滤光片；3.样品池支架；4.比色池插孔；5.聚焦透镜；6.样品室；7.光纤；8.光谱仪；9.手套箱； 1. Light source; 2. Optical filter; 3. Sample cell bracket; 4. Colorimetric cell jack; 5. Focusing lens; 6. Sample chamber; 7. Optical fiber; 8. Spectrometer; 9. Glove box;
图2：仪器光路示意图。 Figure 2: Schematic diagram of the optical path of the instrument.
具体实施方式 Detailed ways
下面结合说明书附图和具体实施方式对本发明做进一步阐述。 The present invention will be further elaborated below in conjunction with the accompanying drawings and specific embodiments.
封闭式荧光分析仪如图1所示，由样品室系统、光源控制系统、光谱仪组成；样品室系统包括样品室、光源、滤光片、聚焦透镜，其中光源、滤光片及聚焦透镜固定在样品室内的样品池支架上、样品室位于手套箱内；光源控制系统、光谱仪和计算机位于手套箱外，光谱仪通过光纤与样品室相连，该光纤从手套箱盲板引出。 The enclosed fluorescence analyzer is shown in Figure 1. It consists of a sample chamber system, a light source control system, and a spectrometer; the sample chamber system includes a sample chamber, a light source, an optical filter, and a focusing lens. The light source, optical filter, and focusing lens are fixed on The sample chamber is on the sample cell bracket in the sample chamber, and the sample chamber is located in the glove box; the light source control system, spectrometer and computer are located outside the glove box, and the spectrometer is connected to the sample chamber through an optical fiber, which is led out from the blind plate of the glove box.
所述的手套箱的材质为不锈钢，用于封闭样品室和辐射防护。 The material of the glove box is stainless steel, which is used for sealing the sample room and radiation protection.
所述的样品室的材料为不锈钢，内壁涂黑。 The material of the sample chamber is stainless steel, and the inner wall is painted black.
所述的样品池支架材质为黑铝，该支架上有入射光路和出射光路两个垂直光孔；比色池安置两孔相交点处；光源、滤光片、比色池在入射光路位于同一轴线；比色池、聚焦透镜在出射光路位于同一轴线。 The material of the sample cell support is black aluminum, and there are two vertical light holes on the support, the incident light path and the exit light path; the colorimetric cell is placed at the intersection of the two holes; The same axis; the colorimetric cell and focusing lens are located on the same axis in the exit light path.
所述的光源采用的是LED灯，安装方式采用卡槽式，功率为30mW～1W； The light source mentioned is an LED lamp, and the installation method is a card slot type, and the power is 30mW～1W;
所述的光源控制系统为恒流源，安装在光谱仪内，电压控制范围为2～4V，电流稳定在320mA； The light source control system is a constant current source installed in the spectrometer, the voltage control range is 2-4V, and the current is stable at 320mA;
所述的滤光片采用的是低带通截至型滤光片，安装方式采用插拔式； The filter used is a low-bandpass cut-off filter, and the installation method is plug-in;
所述的计算机装有操作软件FreeAcid V1.0，用于数据采集和处理。 The computer is equipped with operating software FreeAcid V1.0 for data collection and processing.
该分析仪的光路图如图2所示，光源经滤光后直接照射到样品上，样品产生的荧光经聚焦透镜聚焦后进入光纤，光纤将荧光信号传输到光谱仪，光谱仪接收含有样品信息的荧光信号并经计算机处理实现样品的荧光测量。光源控制系统可调节光源的强度适合于不同浓度的的样品分析。 The optical path diagram of the analyzer is shown in Figure 2. The light source is filtered and irradiated directly on the sample. The fluorescence generated by the sample is focused by the focusing lens and then enters the optical fiber. The optical fiber transmits the fluorescent signal to the spectrometer, and the spectrometer receives the fluorescent light containing the sample information. The signal is processed by computer to realize the fluorescence measurement of the sample. The light source control system can adjust the intensity of the light source to be suitable for the analysis of samples with different concentrations.
实施例1Example 1
利用本发明提供的封闭式荧光分析仪测量不同浓度的钍溶液，考察样品浓度与荧光强度的关系。测量了6个不同浓度的钍溶液。工作曲线的线性回归方程为y = 87.533x + 67.869，r ＞0.999。检测下限0.1 ng/ml，工作曲线的线性范围为(0.1-100) ng/ml。根据文献，普通荧光分析仪的线性范围为(1-10) ng/ml，检测下限1 ng/ml。 The closed-type fluorescence analyzer provided by the invention is used to measure thorium solutions with different concentrations, and the relationship between sample concentration and fluorescence intensity is investigated. Six different concentrations of thorium solutions were measured. The linear regression equation of the working curve is y = 87.533x + 67.869, r > 0.999. The lower limit of detection is 0.1 ng/ml, and the linear range of the working curve is (0.1-100) ng/ml. According to the literature, the linear range of ordinary fluorescence analyzers is (1-10) ng/ml, and the detection limit is 1 ng/ml.
表1钍浓度与荧光强度的关系 Table 1 Relationship between thorium concentration and fluorescence intensity
结果表明：封闭式荧光分析仪测量钍溶液，溶液浓度与荧光强度具有很好的线性相关性，与现有荧光分析仪相比，灵敏度和检测范围都有了较大的提高，线性范围提高2个数量级，检测下限降低了10倍，说明本装置测量后处理样品是完全可行的。 The results show that: the closed fluorescence analyzer measures the thorium solution, and the solution concentration has a good linear correlation with the fluorescence intensity. Compared with the existing fluorescence analyzer, the sensitivity and detection range have been greatly improved, and the linear range has increased by 2 An order of magnitude, the detection limit is reduced by 10 times, indicating that the device is completely feasible to process samples after measurement.
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| 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 |
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| 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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2013
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