WO2021179592A1 - Liquid absorption coefficient measurement device and measurement method - Google Patents
Liquid absorption coefficient measurement device and measurement method Download PDFInfo
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- WO2021179592A1 WO2021179592A1 PCT/CN2020/119927 CN2020119927W WO2021179592A1 WO 2021179592 A1 WO2021179592 A1 WO 2021179592A1 CN 2020119927 W CN2020119927 W CN 2020119927W WO 2021179592 A1 WO2021179592 A1 WO 2021179592A1
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
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- the instrument of the present invention is to solve this problem conveniently.
- ⁇ is the light absorption coefficient of the medium
- x is the propagation distance of light in the medium
- ⁇ I is the light intensity lost by factors such as interface reflection
- I 0 is the incident light intensity of the sample cell.
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Abstract
A liquid absorption coefficient measurement device and a measurement method. The measurement device comprises a light source unit (1), a sample cell unit (2), a measurement unit (5), a position control unit (4), a signal synchronization and data collection unit (6), and an instrument shell (7); the left side of the sample cell unit (2) is fixedly connected to the light source unit (1); the right side of the sample cell unit (2) is fixedly connected to the measurement unit (5); the sample cell unit (2), the light source unit (1), and the measurement unit (5) are placed in the instrument shell (7); the signal synchronization and data collection unit (6) is separately and electrically connected to the light source unit (1) and the measurement unit (5), and is located outside the instrument shell (7); the sample cell unit (2) is of a rectangular shell-shaped structure; the position control unit (4) is located in the sample cell unit (2) and slidably connected to the sample cell unit (2); a first through hole (203) is formed on the left side of the sample cell unit (2); a second through hole (401) and a third through hole (402) are formed on the position control unit (4); and the signal synchronization and data collection unit (6) is used for adjusting the wavelength of light outputted by the light source unit (1), and collecting an electrical signal obtained by the measurement unit (5).
Description
本发明涉及水体指标测定技术领域,具体涉及一种液体吸收系数测量装置及测量方法。The invention relates to the technical field of water body index determination, in particular to a liquid absorption coefficient measuring device and a measuring method.
紫外可见吸收光谱,属原子或分子吸收光谱,是由于物质中分子(或离子)吸收紫外或可见光的能量,发生电子能级跃迁而产生的。除了电子能级外,分子(或离子)吸收能量将伴随着分子(或离子)的振动和转动,同时将发生振动能级和转动能级的跃迁。The ultraviolet-visible absorption spectrum, which belongs to the atomic or molecular absorption spectrum, is produced by the energy level transition of the molecules (or ions) in the substance absorbing the energy of ultraviolet or visible light. In addition to the electronic energy level, the energy absorbed by the molecule (or ion) will be accompanied by the vibration and rotation of the molecule (or ion), and a transition between the vibrational energy level and the rotational energy level will occur at the same time.
紫外可见吸收光谱适用范围广,它既可以定量分析,也可以定性分析和结构分析,常用于无机物和有机物的分析等。由于测量操作简单、快捷,且灵敏度、准确度比较高的特点,因此在众多领域得到广泛的应用。例如,在食品生产中为了保证有颜色的饮料(如可乐、果汁及茶饮料)产品的颜色一致,可以在可见光区用紫外-可见分光光度计来测定其吸光度值,使色差符合产品要求;紫外-可见分光光度法是近年来应用于多糖含量测定最为广泛的方法;在水质研究中,常通过建立紫外-可见吸收光谱数据与水中某些特殊物质之间的相关关系和数学模型,在此基础上根据被测水样的紫外-可见吸收光谱数据分析结果定量地得到水中某些特殊物质的含量。Ultraviolet-visible absorption spectroscopy has a wide range of applications. It can be used for quantitative analysis, qualitative analysis and structural analysis. It is often used for the analysis of inorganic and organic substances. Because of the simple and fast measurement operation, and the characteristics of high sensitivity and accuracy, it has been widely used in many fields. For example, in order to ensure the consistent color of colored beverages (such as cola, juice and tea beverages) in food production, an ultraviolet-visible spectrophotometer can be used in the visible light region to measure the absorbance value, so that the color difference meets the product requirements; UV -Visible spectrophotometry is the most widely used method for the determination of polysaccharide content in recent years; in water quality research, correlations and mathematical models between UV-visible absorption spectrum data and some special substances in water are often established. The above quantitatively obtains the content of some special substances in the water based on the analysis results of the ultraviolet-visible absorption spectrum data of the measured water sample.
双光束紫外可见吸收光谱仪是很常用的测量吸收光谱的仪器。物质对光的吸收是选择性的,利用被测物质对某波长的光的吸收来了解物质的特性。由于各种物质具有各自不同的分子、原子和不同的分子 空间结构,其吸收光能量的情况也就不会相同,因此,每种物质就有其特有的、固定的吸收光谱曲线,可根据吸收光谱上的某些特征波长处的吸光度的高低判别或测定该物质的含量。经常使用双光束紫外可见吸收光谱仪的技术人员都知道这样一个有悖常识的现象:在测量某些高透率液体样品时,吸光度可能出现负值。显然这样的测量结果是需要修正的。The dual-beam ultraviolet-visible absorption spectrometer is a very commonly used instrument for measuring absorption spectra. The absorption of light by a substance is selective, and the absorption of a certain wavelength of light by the measured substance is used to understand the characteristics of the substance. Since various substances have their own different molecules, atoms and different molecular spatial structures, their absorption of light energy will not be the same. Therefore, each substance has its own unique and fixed absorption spectrum curve, which can be based on absorption Determine the absorbance of certain characteristic wavelengths on the spectrum or determine the content of the substance. Technicians who often use dual-beam UV-Vis absorption spectrometers are aware of such a phenomenon that is contrary to common sense: when measuring some high-transmittance liquid samples, the absorbance may appear negative. Obviously, such measurement results need to be corrected.
目前现有技术的主要缺陷是,双光束紫外可见吸收光谱仪的部分光路图如图2所示,其中,PMT是光电倍增管,Ref是参比室比色皿,Sam是样品室比色皿,W是光阑,SEC、CH是组合半反镜,M7、M10是平面镜,M6、M9是凹面镜。基线扫描时,参考室和样品室的比色皿都是空白的,设光路经过样品室和参考室的光强相同,最后两束光到光电倍增管的强度都相同。设透过参比池的光为I
0,透过样品池的光为I。基线扫描时,两样品池内容物相同,此时基线扫描值恒为0,可认为此时透过样品池的光与参比池的光相同。
The main defect of the current prior art is that the partial light path diagram of the dual-beam UV-Vis absorption spectrometer is shown in Figure 2, where PMT is a photomultiplier tube, Ref is a reference chamber cuvette, and Sam is a sample chamber cuvette. W is diaphragm, SEC and CH are combined half mirrors, M7 and M10 are flat mirrors, and M6 and M9 are concave mirrors. During the baseline scan, the cuvettes in the reference chamber and the sample chamber are blank. The light intensity of the light path through the sample chamber and the reference chamber is the same, and the intensity of the last two beams to the photomultiplier tube is the same. Suppose the light passing through the reference cell is I 0 , and the light passing through the sample cell is I. During the baseline scan, the contents of the two sample cells are the same. At this time, the baseline scan value is always 0. It can be considered that the light passing through the sample cell is the same as the light of the reference cell at this time.
当样品池中放入高透过率液体后,吸光度可用下式表示:When the high transmittance liquid is put in the sample cell, the absorbance can be expressed by the following formula:
其中A为吸光度,T为透光率(也叫透过率,即I/I
0),在传统的双光束分光光度计中,通常以经过参比池后的光强代替入射到样品池的光强,如果经过样品池后的光强大于经过参比池的光强,则吸光度的测量值就显示为负值;
Among them, A is the absorbance and T is the light transmittance (also called transmittance, that is, I/I 0 ). In a traditional dual-beam spectrophotometer, the light intensity after passing through the reference cell is usually used instead of the light intensity incident on the sample cell. Light intensity, if the light intensity after passing through the sample cell is stronger than the light intensity passing through the reference cell, the measured value of absorbance will be displayed as a negative value;
以目前较新的岛津仪器公司的UV-2600仪器为例,进入波长扫描界面,设置扫描范围为200nm-900nm,扫描步长为2nm;将两个洁净 的石英比色皿放入样品室内和参比室中,进行基线扫描,所得基线是一条在200nm-900nm范围内吸光度均为0的直线;将样品池中比色皿装入去离子纯水后,再将此装有纯水的比色皿放入样品池,参比室的空白比色皿保持不变,然后进行波长扫描检测,所得的结果如图3所示。图3中横坐标为波长,纵坐标为吸光度。由图3的结果可以发现,纯水在绝大部分波长的吸光度都出现了负值。由我们的常识可知,光在水下的衰减是异常严重的,即便是经过过滤的最纯净的水,它对光的衰减也是不可忽视的。空气的透光率显然应该比水高,即使是纯净的去离子水,其吸光度也应该比水高,水的吸光度测量结果应该是正值。在实验步骤都正确,且仪器、配套工具都是正常工作的前提下,测量的去离子纯净水样品的吸光度依然出现负值。Take the current UV-2600 instrument of Shimadzu Instruments as an example, enter the wavelength scanning interface, set the scanning range to 200nm-900nm, and the scanning step length to 2nm; put two clean quartz cuvettes into the sample chamber and In the reference chamber, the baseline scan is performed, and the baseline obtained is a straight line with an absorbance of 0 in the range of 200nm-900nm; after filling the cuvette in the sample cell with deionized pure water, it is filled with pure water. The cuvette is put into the sample cell, the blank cuvette in the reference room remains unchanged, and then the wavelength scanning detection is performed. The result obtained is shown in Figure 3. In Figure 3, the abscissa is the wavelength, and the ordinate is the absorbance. From the results in Figure 3, it can be found that the absorbance of pure water at most wavelengths has a negative value. From our common sense, the attenuation of light underwater is extremely serious, even the purest filtered water, the attenuation of light cannot be ignored. The light transmittance of air should obviously be higher than that of water. Even pure deionized water should have a higher absorbance than water, and the absorbance measurement result of water should be a positive value. Under the premise that the experimental steps are correct and the instrument and supporting tools are working normally, the measured absorbance of the deionized pure water sample still shows a negative value.
样品池的比色皿内装的纯净水,参考池的比色皿内装的是空气,洁净空气的透光率大于纯净水的透光率,经过样品池后的光强又怎可能会大于经过参考池后的光强呢?如果考虑比色皿的界面反射之后,就会发现事实果真如此。The pure water in the cuvette of the sample cell, the cuvette of the reference cell is filled with air, the light transmittance of clean air is greater than that of pure water, how can the light intensity after passing through the sample cell be greater than the reference How about the light intensity behind the pool? If you consider the reflection of the cuvette's interface, you will find that this is the case.
光线穿过样品池或参比池的比色皿时,都需要经过四个界面,如图4所示。样品池的比色皿与参比池的比色皿外侧两个界面(①和④)是一致的,因此光线在界面上的反射也是一样的。比色皿内侧两个界面(②和③)由于内容物的折射率有较大的差别,导致样品池的比色皿与参比池的比色皿在这两界面的反射率差别很大。当样品池比色皿的内容物的吸光度较大时,比色皿内侧两界面反射率的差别通常可以忽略不计;当样品池比色皿内容物的透光率较大与参比池比色皿内容 物的透光率差别较小时,比色皿内侧两界面反射率的差别就不可忽略不计了。When light passes through the cuvette of the sample cell or reference cell, it needs to pass through four interfaces, as shown in Figure 4. The two interfaces (① and ④) outside the cuvette of the sample cell and the cuvette of the reference cell are the same, so the reflection of light on the interface is also the same. The two interfaces (② and ③) inside the cuvette have a large difference in the refractive index of the contents, resulting in a large difference in reflectivity between the cuvette of the sample cell and the cuvette of the reference cell at these two interfaces. When the absorbance of the content of the sample cell cuvette is large, the difference in reflectance of the two interfaces inside the cuvette is usually negligible; when the light transmittance of the content of the sample cell cuvette is larger than that of the reference cell When the difference in light transmittance of the contents of the cuvette is small, the difference in reflectance of the two interfaces inside the cuvette cannot be ignored.
测量时参比池比色皿的内容物为空气,空气的折射率约为1,样品池比色皿的内容物为纯净水,水的折射率比空气的折射率大,与石英的折射率更接近,因此样品池比色皿内侧两界面对光线的反射率小于参比池比色皿内侧两界面对光线的反射率,两界面反射率的差别甚至大于纯水和空气的透射率的差别,因此导致纯水的吸光度测量出现负值。要得到正确的测量结果,必须考虑样品池内侧两界面反射率的差别。也就是说,在测量透射率较高的液体例如纯净水的吸光度时,必须考虑比色皿内侧两界面反射率差别的影响,对测量结果进行修正。修正的方法通常比较繁琐,且准确度也存在一定偏差。When measuring, the content of the cuvette of the reference cell is air, and the refractive index of air is about 1. The content of the cuvette of the sample cell is pure water. The refractive index of water is larger than that of air and the refractive index of quartz. It is closer, so the reflectivity of the two interfaces inside the sample cell cuvette to light is less than the reflectivity of the two interfaces inside the reference cell cuvette, and the difference in reflectivity between the two interfaces is even greater than the difference in transmittance between pure water and air. , Which leads to negative values in the absorbance measurement of pure water. To obtain correct measurement results, the difference in reflectivity between the two interfaces inside the sample cell must be considered. That is to say, when measuring the absorbance of liquids with higher transmittance, such as pure water, the difference in reflectivity between the two interfaces inside the cuvette must be considered, and the measurement results must be corrected. The correction method is usually cumbersome, and the accuracy also has a certain deviation.
本发明所述仪器就是为了便捷解决此问题。The instrument of the present invention is to solve this problem conveniently.
发明内容Summary of the invention
本发明的目的是提供一种液体吸收系数测量装置及测量方法以解决现有技术中存在的问题。本发明的装置及测量方法可以避免在测量透射率较高的液体的吸光度时,因比色皿内侧两界面反射率差别的影响造成测量结果误差大的问题,本发明的测量装置及测量方法简单实用,测量结果精准。The purpose of the present invention is to provide a liquid absorption coefficient measuring device and measuring method to solve the problems existing in the prior art. The device and measurement method of the present invention can avoid the problem of large error in the measurement result caused by the difference in reflectance of the two interfaces inside the cuvette when measuring the absorbance of liquids with higher transmittance. The measurement device and measurement method of the present invention are simple Practical, accurate measurement results.
为实现上述目的,本发明提供了如下方案:本发明提供一种液体吸收系数测量装置,包括光源单元、样品池单元、探测单元、位置控制单元、信号同步及数据采集单元和仪器外壳;所述样品池单元左侧固接所述光源单元,所述样品池单元右侧固接所述探测单元,所述样 品池单元、光源单元和探测单元放置在仪器外壳内,所述信号同步及数据采集单元分别电性连接所述光源单元和探测单元且处于所述仪器外壳外侧;In order to achieve the above objectives, the present invention provides the following solutions: the present invention provides a liquid absorption coefficient measurement device, including a light source unit, a sample cell unit, a detection unit, a position control unit, a signal synchronization and data acquisition unit, and an instrument housing; The left side of the sample cell unit is fixedly connected to the light source unit, the right side of the sample cell unit is fixedly connected to the detection unit, the sample cell unit, the light source unit and the detection unit are placed in the instrument housing, the signal synchronization and data acquisition The units are respectively electrically connected to the light source unit and the detection unit and are located outside the instrument housing;
所述样品池单元为矩形壳体状结构,所述位置控制单元处于所述样品池单元内且与所述样品池单元滑动连接,所述样品池左侧开设有第一通孔,所述位置控制单元开设有第二通孔、第三通孔;The sample cell unit has a rectangular shell-like structure, the position control unit is located in the sample cell unit and is slidably connected to the sample cell unit, a first through hole is opened on the left side of the sample cell, and the position The control unit is provided with a second through hole and a third through hole;
所述信号同步及数据采集单元用于调控光源单元输出光的波长并采集探测单元所得的电信号,由此可知被液体吸收后入射到探测器的光强。The signal synchronization and data acquisition unit is used to adjust the wavelength of the light output by the light source unit and collect the electrical signal obtained by the detection unit, so that the intensity of the light incident on the detector after being absorbed by the liquid can be known.
优选的,所述样品池前板、样品池后板上均设置有刻度主尺,所述样品池上方搭接有刻度标尺,所述刻度标尺处于所述位置控制单元上方。Preferably, the front plate of the sample cell and the rear plate of the sample cell are both provided with a main scale ruler, a scale ruler is overlapped above the sample cell, and the scale ruler is above the position control unit.
优选的,所述第一通孔内安装有石英透光准直窗口,所述第二通孔内安装有聚光透镜窗口,所述第三通孔处于所述第二通孔下方。Preferably, a quartz light-transmitting collimating window is installed in the first through hole, a condenser lens window is installed in the second through hole, and the third through hole is under the second through hole.
优选的,所述探测单元包括光纤,所述光纤伸入所述样品池单元内并连接所述聚光透镜窗口。Preferably, the detection unit includes an optical fiber, which extends into the sample cell unit and is connected to the condenser lens window.
优选的,所述位置控制单元下板、前侧板、后侧板均精密抛光且分别与所述样品池底板、样品池前板、样品池后板精密嵌合。Preferably, the lower plate, the front side plate, and the rear side plate of the position control unit are all precisely polished and are respectively precisely fitted with the bottom plate of the sample cell, the front plate of the sample cell, and the rear plate of the sample cell.
优选的,所述光源单元灯泡采用氙灯和钨丝灯组合,分光部分采用棱镜分光或光栅分光。Preferably, the light source unit bulb adopts a combination of a xenon lamp and a tungsten filament lamp, and the light splitting part adopts prism light splitting or grating light splitting.
一种液体吸收系数测量装置的测量方法,包括以下步骤,A measuring method of a liquid absorption coefficient measuring device includes the following steps,
1)、介质吸收光的一般规律可用式(2)表示:1) The general law of light absorption by the medium can be expressed by formula (2):
I=I
0·e
-αx (2)
I=I 0 ·e -αx (2)
式中I
0表示入射光的光强,I表示入射光在介质传播x距离后的光强,在双光束紫外可见吸收光谱仪中,用参比室后测量的光强代替入射到样品池的光强,所以有:
In the formula, I 0 represents the light intensity of the incident light, I represents the light intensity of the incident light after x distance travels through the medium. In a dual-beam UV-visible absorption spectrometer, the light intensity measured after the reference chamber is used to replace the light incident on the sample cell. Strong, so there are:
与式(1)一致,A为吸光度,α为吸收系数;Consistent with formula (1), A is the absorbance and α is the absorption coefficient;
2)、光强为I
0的热射光通过样品池后,探测器探测到的光强可用下式描述:
2) After the thermal light with light intensity I 0 passes through the sample cell, the light intensity detected by the detector can be described by the following formula:
I=(I
0-ΔI)·e
-ax (4)
I = (I 0 -ΔI) · e -ax (4)
式中α为介质的光吸收系数,x为光在介质中的传播距离,ΔI为界面反射等因素损失的光强,I
0为样品池的入射光强,通过测量样品池不同长度x位置的光强I
x,就可以计算出样品的光吸收系数α;
Where α is the light absorption coefficient of the medium, x is the propagation distance of light in the medium, ΔI is the light intensity lost by factors such as interface reflection, and I 0 is the incident light intensity of the sample cell. With light intensity I x , the light absorption coefficient α of the sample can be calculated;
3)、选取某确定波长的光照入样品池,将位置控制单元及光纤探头靠近样品池设有石英透光准直窗口的第一通孔,测得入射光的强度为I
0;在样品池中注入待测液体,将位置控制单元及光纤探头移至位置x处,测得光强为I
x,记录多组位置x和光强Ix值,用式(4)计算出待测液体某波长的光吸收系数。
3) Select a certain wavelength of light into the sample cell, place the position control unit and the optical fiber probe close to the first through hole of the sample cell with a quartz transparent collimating window, and measure the intensity of the incident light as I 0 ; in the sample cell Inject the liquid to be measured into the liquid, move the position control unit and the optical fiber probe to position x, the measured light intensity is I x , record multiple sets of position x and light intensity Ix values, and calculate a certain wavelength of the liquid to be measured using formula (4) The light absorption coefficient.
本发明公开了以下技术效果:The present invention discloses the following technical effects:
1、本发明通过设置光源单元、样品池单元、位置控制单元、探测单元、信号同步及数据采集单元,在样品池单元上开设第一通孔并安装石英透光准直窗口,位置控制单元上开设第二通孔并安装聚光透镜窗口,通过测量不同位置的透射光强(即透过不同厚度液体的光强) 计算液体的光吸收系数,可以避免在测量透射率较高的液体的吸光度时,因比色皿内侧两界面反射率差别的影响造成测量结果误差大的问题;1. In the present invention, the light source unit, the sample cell unit, the position control unit, the detection unit, the signal synchronization and the data acquisition unit are set, the first through hole is opened in the sample cell unit and the quartz transparent collimating window is installed, and the position control unit is Open a second through hole and install a condenser lens window, and calculate the light absorption coefficient of the liquid by measuring the transmitted light intensity at different positions (that is, the light intensity through liquids of different thicknesses), which can avoid measuring the absorbance of liquids with higher transmittance. When, due to the influence of the difference in reflectivity between the two interfaces inside the cuvette, the measurement result has a large error;
2、通过在样品池前板、样品池后板上均设置有刻度主尺,样品池上方搭接有刻度标尺,刻度标尺处于位置控制单元上方,刻度主尺与刻度标尺组成游标尺,可精密读出位置控制单元板的位置;2. The main scale of the scale is set on the front plate of the sample cell and the back plate of the sample cell. The scale ruler is overlapped above the sample cell. The scale ruler is located above the position control unit. The scale main ruler and the scale ruler form a vernier ruler, which can be precise Read the position of the position control unit board;
3、通过在位置控制单元上设置第三通孔且处于第二通孔下方,第三通孔为液体流动窗口,液体流动窗口可使位置控制单元移动前后,样品液面保持不变。3. A third through hole is provided on the position control unit and is located below the second through hole. The third through hole is a liquid flow window. The liquid flow window can make the position control unit move before and after the sample liquid level remains unchanged.
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the following will briefly introduce the drawings that need to be used in the embodiments. Obviously, the drawings in the following description are only some of the present invention. Embodiments, for those of ordinary skill in the art, without creative labor, other drawings can be obtained based on these drawings.
图1为本发明液体吸收系数测量装置结构示意图;Figure 1 is a schematic diagram of the structure of the liquid absorption coefficient measuring device of the present invention;
图2为紫外可见光谱仪UV-2600光路图;Figure 2 is the optical path diagram of the UV-Vis spectrometer UV-2600;
图3为纯水的吸收曲线;Figure 3 shows the absorption curve of pure water;
图4为光线穿过比色皿的示意图;Figure 4 is a schematic diagram of light passing through a cuvette;
图5为样品池单元和位置控制单元的结构示意图。Figure 5 is a schematic diagram of the structure of the sample cell unit and the position control unit.
其中,1为光源单元,2为样品池单元,3为刻度标尺,4为位置控制单元,5为探测单元,6为信号同步及数据采集单元,7为仪器 外壳,8为光纤,201为样品池前板,202为样品池后板,203为第一通孔,401为第二通孔,402为第三通孔。Among them, 1 is the light source unit, 2 is the sample cell unit, 3 is the scale ruler, 4 is the position control unit, 5 is the detection unit, 6 is the signal synchronization and data acquisition unit, 7 is the instrument housing, 8 is the optical fiber, and 201 is the sample The cell front plate, 202 is the sample cell back plate, 203 is the first through hole, 401 is the second through hole, and 402 is the third through hole.
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with 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, rather than all 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 shall fall within the protection scope of the present invention.
为使本发明的上述目的、特征和优点能够更加明显易懂,下面结合附图和具体实施方式对本发明作进一步详细的说明。In order to make the above-mentioned objects, features and advantages of the present invention more obvious and understandable, the present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.
参照图1-5,本发明提供一种液体吸收系数测量装置,包括光源单元1、样品池单元2、探测单元5、位置控制单元4、信号同步及数据采集单元6和仪器外壳7;样品池单元2左侧固接光源单元1,样品池单元2右侧固接探测单元5,样品池单元2、光源单元1和探测单元5放置在仪器外壳7内,信号同步及数据采集单元6分别电性连接光源单元1和探测单元5且处于仪器外壳7外侧;Referring to Figures 1-5, the present invention provides a liquid absorption coefficient measuring device, which includes a light source unit 1, a sample cell unit 2, a detection unit 5, a position control unit 4, a signal synchronization and data acquisition unit 6 and an instrument housing 7; a sample cell The left side of the unit 2 is fixedly connected to the light source unit 1, and the right side of the sample cell unit 2 is fixedly connected to the detection unit 5. The sample cell unit 2, the light source unit 1 and the detection unit 5 are placed in the instrument housing 7, and the signal synchronization and data acquisition unit 6 are separately electrically connected. The light source unit 1 and the detection unit 5 are sexually connected and are located outside the instrument housing 7;
样品池单元2为矩形壳体状结构,位置控制单元4处于样品池单元2内且与样品池单元2滑动连接,样品池左侧开设有第一通孔203,第一通孔允许光源单元的光直线入射进入样品池,位置控制单元4开设有第二通孔401、第三通孔402,第二通孔可安装光纤探头,第三通孔可使位置控制单元左右侧液体保持平衡;The sample cell unit 2 is a rectangular shell structure, the position control unit 4 is located in the sample cell unit 2 and is slidably connected to the sample cell unit 2. A first through hole 203 is opened on the left side of the sample cell, and the first through hole allows the light source unit to The light is incident straight into the sample cell, the position control unit 4 is provided with a second through hole 401 and a third through hole 402, the second through hole can be installed with an optical fiber probe, and the third through hole can keep the liquid on the left and right sides of the position control unit in balance;
信号同步及数据采集单元6用于调控光源单元1输出光的波长并 采集探测单元5所得的电信号,由此可知被液体吸收后入射到探测器的光强,信号同步及数据采集单元6的结构及原理均为现有技术,为本领域技术人员的公知常识,在此不再赘述。The signal synchronization and data acquisition unit 6 is used to adjust the wavelength of the light output from the light source unit 1 and collect the electrical signal obtained by the detection unit 5. From this it can be known the intensity of the light incident on the detector after being absorbed by the liquid, and the signal synchronization and data acquisition unit 6 The structure and principle are the prior art, which are common knowledge of those skilled in the art, and will not be repeated here.
进一步优选方案,样品池前板201、样品池后板202上均设置有刻度主尺,样品池上方搭接有刻度标尺3,刻度标尺3处于位置控制单元4上方,刻度主尺与刻度标尺3组成游标尺,可精密读出位置控制单元4板的位置。In a further preferred solution, the sample cell front plate 201 and the sample cell rear plate 202 are both provided with a scale main ruler, a scale ruler 3 is overlapped above the sample cell, and the scale ruler 3 is above the position control unit 4, and the scale main ruler and the scale ruler 3 It is composed of a vernier scale, which can accurately read the position of the 4 plates of the position control unit.
进一步优选方案,第一通孔203内安装有石英透光准直窗口,第二通孔401内安装有聚光透镜窗口,第三通孔402处于第二通孔401下方,第三通孔402为液体流动窗口,液体流动窗口可使位置控制单元4移动前后,样品液面保持不变。In a further preferred solution, a quartz light-transmitting collimating window is installed in the first through hole 203, a condenser lens window is installed in the second through hole 401, the third through hole 402 is under the second through hole 401, and the third through hole 402 is It is a liquid flow window, which can make the position control unit 4 move before and after the sample liquid level remains unchanged.
进一步优选方案,探测单元5包括光纤8,光纤8伸入样品池单元2内并连接聚光透镜窗口,探测单元5与其他光探测单元相似,包括光探测器如光电倍增管和雪崩光电二极管以及其他伺服电路,其内部结构及使用原理为现有技术,为本领域技术人员的公知常识,在此不再赘述。In a further preferred solution, the detection unit 5 includes an optical fiber 8, which extends into the sample cell unit 2 and is connected to a condenser lens window. The detection unit 5 is similar to other light detection units, including photodetectors such as photomultiplier tubes and avalanche photodiodes, and For other servo circuits, their internal structure and operating principles are in the prior art and are common knowledge of those skilled in the art, and will not be repeated here.
进一步优选方案,位置控制单元4下板、前侧板、后侧板均精密抛光且分别与样品池底板、样品池前板201、样品池后板202精密嵌合。In a further preferred solution, the lower plate, the front side plate, and the rear side plate of the position control unit 4 are all precisely polished and are precisely fitted with the sample cell bottom plate, the sample cell front plate 201, and the sample cell rear plate 202, respectively.
进一步优选方案,光源单元1灯泡采用氙灯和钨丝灯组合,分光部分采用棱镜分光或光栅分光。In a further preferred solution, the bulb of the light source unit 1 adopts a combination of a xenon lamp and a tungsten filament lamp, and the light splitting part adopts prism light splitting or grating light splitting.
本发明一种液体吸收系数测量装置的测量方法,包括以下步骤,The measuring method of a liquid absorption coefficient measuring device of the present invention includes the following steps:
1)、介质吸收光的一般规律可用式(2)表示:1) The general law of light absorption by the medium can be expressed by formula (2):
I=I
0·e
-αx (2)
I=I 0 ·e -αx (2)
式中I
0表示入射光的光强,I表示入射光在介质传播x距离后的光强,在双光束紫外可见吸收光谱仪中,用参比室后测量的光强代替入射到样品池的光强,所以有:
In the formula, I 0 represents the light intensity of the incident light, I represents the light intensity of the incident light after x distance travels through the medium. In a dual-beam UV-visible absorption spectrometer, the light intensity measured after the reference chamber is used to replace the light incident on the sample cell. Strong, so there are:
与式(1)一致,A为吸光度,α为吸收系数;Consistent with formula (1), A is the absorbance and α is the absorption coefficient;
2)、光强为I
0的热射光通过样品池后,探测器探测到的光强可用下式描述:
2) After the thermal light with light intensity I 0 passes through the sample cell, the light intensity detected by the detector can be described by the following formula:
I=(I
0-ΔI)·e
-ax (4)
I = (I 0 -ΔI) · e -ax (4)
式中α为介质的光吸收系数,x为光在介质中的传播距离,ΔI为界面反射等因素损失的光强,I
0为样品池的入射光强,通过测量样品池不同长度x位置的光强I
x,就可以计算出样品的光吸收系数α;
Where α is the light absorption coefficient of the medium, x is the propagation distance of light in the medium, ΔI is the light intensity lost by factors such as interface reflection, and I 0 is the incident light intensity of the sample cell. With light intensity I x , the light absorption coefficient α of the sample can be calculated;
3)、选取某确定波长的光照入样品池,将位置控制单元4及光纤8探头靠近样品池设石英透光准直孔的一端,测得入射光的强度为I
0;在样品池中注入去离子蒸馏水,将位置控制单元4及光纤8探头移至位置x处,测得光强为I
x,以上表用式(4)计算出不同波长液体的光吸收系数。
3) Select a certain wavelength of light into the sample cell, place the position control unit 4 and the optical fiber 8 probe close to the end of the sample cell where the quartz transparent collimating hole is set, and measure the intensity of the incident light as I 0 ; inject into the sample cell With deionized distilled water, move the position control unit 4 and the optical fiber 8 probe to position x, and the measured light intensity is I x . The above table uses formula (4) to calculate the light absorption coefficient of liquids with different wavelengths.
选取某确定波长的光照入样品池,将位置控制单元4及光纤8探头靠近样品池设有石英透光准直窗口的第一通孔203,测得入射光的强度为I
0;在样品池中注入去离子蒸馏水,将位置控制单元4及光纤8探头移至位置x处,测得光强为I
x,x分别为1.0cm、2.0cm、5cm 和10cm。所测的数据如下表1:
Select a certain wavelength of light into the sample cell, place the position control unit 4 and the optical fiber 8 probe close to the first through hole 203 of the sample cell with a quartz transparent collimating window, and measure the intensity of the incident light as I 0 ; in the sample cell Inject deionized distilled water into the medium, move the position control unit 4 and the optical fiber 8 probe to the position x, and the measured light intensity is I x , and x is 1.0 cm, 2.0 cm, 5 cm and 10 cm, respectively. The measured data are as follows in Table 1:
表1.位置控制单元在不同位置时探测光光强Table 1. The position control unit detects the light intensity at different positions
以上表用式(4)计算出不同波长液体的光吸收系数如下表2:The above table uses formula (4) to calculate the light absorption coefficient of liquids with different wavelengths as shown in Table 2:
表2.水的吸收系数测量值Table 2. Measured values of water absorption coefficient
在本发明的描述中,需要理解的是,术语“纵向”、“横向”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位 或位置关系,仅是为了便于描述本发明,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。In the description of the present invention, it should be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", The orientation or positional relationship indicated by "horizontal", "top", "bottom", "inner", "outer", etc. are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention, rather than indicating or It is implied that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation to the present invention.
以上所述的实施例仅是对本发明的优选方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。The above-mentioned embodiments only describe the preferred mode of the present invention, and do not limit the scope of the present invention. Without departing from the design spirit of the present invention, those of ordinary skill in the art have made various contributions to the technical solutions of the present invention. Variations and improvements should fall within the protection scope determined by the claims of the present invention.
Claims (7)
- 一种液体吸收系数测量装置,其特征在于,包括光源单元(1)、样品池单元(2)、探测单元(5)、位置控制单元(4)、信号同步及数据采集单元(6)和仪器外壳(7);所述样品池单元(2)左侧固接所述光源单元(1),所述样品池单元(2)右侧固接所述探测单元(5),所述样品池单元(2)、光源单元(1)和探测单元(5)放置在仪器外壳(7)内,所述信号同步及数据采集单元(6)分别电性连接所述光源单元(1)和探测单元(5)且处于所述仪器外壳(7)外侧;A liquid absorption coefficient measuring device, which is characterized by comprising a light source unit (1), a sample cell unit (2), a detection unit (5), a position control unit (4), a signal synchronization and data acquisition unit (6) and an instrument Housing (7); the left side of the sample cell unit (2) is fixedly connected to the light source unit (1), the right side of the sample cell unit (2) is fixedly connected to the detection unit (5), the sample cell unit (2) The light source unit (1) and the detection unit (5) are placed in the instrument housing (7), and the signal synchronization and data acquisition unit (6) is electrically connected to the light source unit (1) and the detection unit ( 5) It is located outside the instrument housing (7);所述样品池单元(2)为矩形壳体状结构,所述位置控制单元(4)处于所述样品池单元(2)内且与所述样品池单元(2)滑动连接,所述样品池单元左侧开设有第一通孔(203);所述位置控制单元(4)开设有第二通孔(401)、第三通孔(402);The sample cell unit (2) is a rectangular shell-shaped structure, the position control unit (4) is located in the sample cell unit (2) and is slidably connected to the sample cell unit (2), and the sample cell The left side of the unit is provided with a first through hole (203); the position control unit (4) is provided with a second through hole (401) and a third through hole (402);所述信号同步及数据采集单元(6)用于调控光源单元(1)输出光的波长并采集探测单元(5)所得的电信号,由此可知被液体吸收后入射到探测器的光强。The signal synchronization and data acquisition unit (6) is used to control the wavelength of the light output by the light source unit (1) and collect the electrical signal obtained by the detection unit (5), so that the intensity of the light incident on the detector after being absorbed by the liquid can be known.
- 根据权利要求1所述的一种液体吸收系数测量装置,其特征在于:所述样品池前板(201)、样品池后板(202)上均设置有刻度主尺,所述样品池上方搭接有刻度标尺(3),所述刻度标尺(3)处于所述位置控制单元(4)上方。The liquid absorption coefficient measuring device according to claim 1, characterized in that: the front plate (201) of the sample cell and the rear plate (202) of the sample cell are both provided with a graduated ruler, and the upper part of the sample cell A scale ruler (3) is connected, and the scale ruler (3) is located above the position control unit (4).
- 根据权利要求1所述的一种液体吸收系数测量装置,其特征在于:所述第一通孔(203)内安装有石英透光准直窗口,所述第二通孔(401)内安装有聚光透镜窗口,所述第三通孔(402)处于所述 第二通孔(401)下方。The liquid absorption coefficient measuring device according to claim 1, characterized in that: a quartz transparent collimating window is installed in the first through hole (203), and a quartz light-transmitting collimating window is installed in the second through hole (401). Condenser lens window, the third through hole (402) is located below the second through hole (401).
- 根据权利要求1所述的一种液体吸收系数测量装置,其特征在于:所述探测单元(5)包括光纤(8),所述光纤(8)伸入所述样品池单元(2)内并连接所述聚光透镜窗口。A liquid absorption coefficient measuring device according to claim 1, characterized in that: the detection unit (5) comprises an optical fiber (8), and the optical fiber (8) extends into the sample cell unit (2) and Connect the condenser lens window.
- 根据权利要求1所述的一种液体吸收系数测量装置,其特征在于:所述位置控制单元(4)下板、前侧板、后侧板均精密抛光且分别与所述样品池底板、样品池前板(201)、样品池后板(202)精密嵌合。The liquid absorption coefficient measuring device according to claim 1, characterized in that: the lower plate, the front side plate, and the rear side plate of the position control unit (4) are all precisely polished and are respectively connected with the bottom plate of the sample cell and the sample The cell front plate (201) and the sample cell back plate (202) are precisely fitted.
- 根据权利要求1所述的一种液体吸收系数测量装置,其特征在于:所述光源单元(1)灯泡采用氙灯和钨丝灯组合,分光部分采用棱镜分光或光栅分光。The liquid absorption coefficient measuring device according to claim 1, characterized in that: the bulb of the light source unit (1) adopts a combination of a xenon lamp and a tungsten lamp, and the light splitting part adopts prism light splitting or grating light splitting.
- 根据权利要求1所述的一种液体吸收系数测量装置的测量方法,包括以下步骤,其特征在于:The measuring method of a liquid absorption coefficient measuring device according to claim 1, comprising the following steps, characterized in that:1)、介质吸收光的一般规律可用式(2)表示:1) The general law of light absorption by the medium can be expressed by formula (2):I=I 0·e -αx (2) I=I 0 ·e -αx (2)式中I 0表示入射光的光强,I表示入射光在介质传播x距离后的光强,在双光束紫外可见吸收光谱仪中,用参比室后测量的光强代替入射到样品池的光强,所以有: In the formula, I 0 represents the light intensity of the incident light, I represents the light intensity of the incident light after x distance travels through the medium. In a dual-beam UV-visible absorption spectrometer, the light intensity measured after the reference chamber is used to replace the light incident on the sample cell. Strong, so there are:其中,A为吸光度,α为吸收系数;Among them, A is the absorbance and α is the absorption coefficient;2)、光强为I 0的热射光通过样品池后,探测器探测到的光强可用下式描述: 2) After the thermal light with light intensity I 0 passes through the sample cell, the light intensity detected by the detector can be described by the following formula:I=(I 0-ΔI)·e -ax (4) I = (I 0 -ΔI) · e -ax (4)式中α为介质的光吸收系数,x为光在介质中的传播距离,ΔI为界面反射等因素损失的光强,I 0为样品池的入射光强,通过测量样品池不同长度x位置的光强I x,就可以计算出样品的光吸收系数α; Where α is the light absorption coefficient of the medium, x is the propagation distance of light in the medium, ΔI is the light intensity lost by factors such as interface reflection, and I 0 is the incident light intensity of the sample cell. With light intensity I x , the light absorption coefficient α of the sample can be calculated;3)、选取某确定波长的光照入样品池,将位置控制单元(4)及光纤(8)探头靠近样品池设有石英透光准直窗口的第一通孔(203),测得入射光的强度为I 0;在样品池中注入待测液体,将位置控制单元(4)及光纤(8)探头移至位置x处,测得光强为I x,记录多组位置x和光强I x值,用式(4)计算出待测液体某波长的光吸收系数。 3) Select a certain wavelength of light into the sample cell, place the position control unit (4) and the optical fiber (8) probe close to the first through hole (203) of the sample cell with a quartz transparent collimating window, and measure the incident light The intensity of is I 0 ; inject the liquid to be tested into the sample cell, move the position control unit (4) and the optical fiber (8) probe to position x, the measured light intensity is I x , record multiple sets of positions x and light intensity I x value, use formula (4) to calculate the light absorption coefficient of a certain wavelength of the liquid to be measured.
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CN112763184B (en) * | 2020-12-23 | 2023-08-29 | 中国人民解放军国防科技大学 | Gain fiber absorption coefficient measuring device and method based on side scattered light detection |
CN114397270A (en) * | 2021-12-06 | 2022-04-26 | 华中光电技术研究所(中国船舶重工集团公司第七一七研究所) | Water attenuation coefficient measuring system |
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