CN102967583A - Measuring apparatus and method used for measuring liquid phase gas refraction index - Google Patents
Measuring apparatus and method used for measuring liquid phase gas refraction index Download PDFInfo
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- CN102967583A CN102967583A CN2012104471550A CN201210447155A CN102967583A CN 102967583 A CN102967583 A CN 102967583A CN 2012104471550 A CN2012104471550 A CN 2012104471550A CN 201210447155 A CN201210447155 A CN 201210447155A CN 102967583 A CN102967583 A CN 102967583A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/4133—Refractometers, e.g. differential
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/43—Refractivity; Phase-affecting properties, e.g. optical path length by measuring critical angle
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Abstract
本发明公开了一种用于测量液相气体折射率的测量仪，包括：点光源照明模块，其产生光束以对待检测液相气体进行检测；探测棱镜，其一棱镜面与所述待测液体表面接触形成反射面，点光源照明模块出射后的光束在该反射面上聚焦形成光斑，并发生全反射和部分反射；反射光接收模块，其用于收集经所述反射面反射的光线，并将收集的光斑图像信息转换成电信号输出；图像分析模块，其对输出的光斑图像信息进行处理，提取出光斑中的明暗界限，进而即可得到待测物的折射率。本发明还公开了一种测量液相气体折射率的方法。本发明的装置和方法可以有效测量液相气体折射率，具有精度高、维护简单、实现容易、抗干扰能力强、受测量环境影响小等优点。
The invention discloses a measuring instrument for measuring the refractive index of liquid-phase gas, which comprises: a point light source lighting module, which generates light beams to detect the liquid-phase gas to be detected; Surface contact forms a reflective surface, and the light beam emitted by the point light source lighting module is focused on the reflective surface to form a light spot, and total reflection and partial reflection occur; the reflected light receiving module is used to collect the light reflected by the reflective surface, and The collected light spot image information is converted into electrical signal output; the image analysis module processes the output light spot image information, extracts the light and dark boundaries in the light spot, and then obtains the refractive index of the object to be measured. The invention also discloses a method for measuring the refractive index of liquid-phase gas. The device and method of the invention can effectively measure the refractive index of the liquid-phase gas, and has the advantages of high precision, simple maintenance, easy realization, strong anti-interference ability, and little influence by the measurement environment.
Description
Technical field
The present invention relates to the light refractive index fields of measurement, be specifically related to a kind of light refractive index measuring instrument and measuring method, be used for measurement and the qualitative analysis of the various characteristics parameter of the liquid-phase gas under the high pressure, also can measure liquid solution under normal temperature, the normal pressure simultaneously.
Background technology
Refractive index is not only the fundamental physical quantity that characterizes optical characteristic of substance, and be that new material is synthetic, material is differentiated and scientific research in an important performance parameter, its density, concentration, temperature and stress and so on physical quantities with material is relevant, is widely used in the technical fields such as optics, oil refining, papermaking, food, material.
Liquid-phase gas refractive index and gas physics and chemistry performance parameter exist linear relationship, and the measurement of refractive index is easier to realize with respect to the measurement of other physical quantity.According to the Lorentz-Lorenz formula, the refractive index of material is the function of the number N of the microscopic particle (atom or molecule) in the material in the unit volume.Also can be applicable to gas by this liquid-phase gas refractometer of above-mentioned principle differentiates and proximate analysis.
At present, the measuring method of liquid-phase gas refractive index mainly is divided into wave optics, SPR technology, optical fiber sensing technology, critical angle method.The wave optics advantage is that measuring accuracy is high, but the method realizability is poor, higher to equipment requirement, anti-interference is poor, cost is higher is not suitable for large-scale production and application.The advantage of SPR technology be measuring accuracy high, be fit to commercial the application, but the method Measuring Time is longer, can't realize that on-line measurement, anti-introduced contaminants disturb relatively poor, interface metal film to be corroded easily, are not suitable for refractometry under the extreme condition.The advantage of optical fiber sensing technology is that to measure highly sensitive, anti-outside electromagnetic interference stronger, but the method is higher to requirement on devices, system realizes that cost is higher, be subjected to bubble and interface impurity effect large.
The advantage of critical angle method is measuring accuracy height, strong interference immunity, simple, the suitable large-scale production of system maintenance and application, is fit to the refractometry of extreme condition liquid-phase gas.The Abbe refractometer is the Typical Representative of critical angle method, and is simple because of its measuring principle, precision is high, system reliability is high, anti-external interference is used in a large number in industrial and agricultural production and field of scientific study by force.
Spot size is divided into focus type critical method and divergence form critical method to critical angle method on the interface by surveying.CN 102012359 discloses a kind of divergence form critical angle and has sent out the method for measuring liquid parameter.The method is incident ray to be radiated at survey on the matter of interface, thereby is surveying interface generating unit sub reflector and total reflection measuring refractive indexes of liquid by light.The required test surface of the method is larger, is only suitable for measuring the parameter of liquid under normal temperature, normal pressure.And, because its light beam that incides the prism test surface of divergence form critical method has the fixing angle of divergence, the refractive index of surveying boundary material is inhomogeneous, therefore the refractometry scope is narrow, test surface is subjected to impurity effect, constraint light beam ability relatively poor easily, reveal the air-gap that affects system accuracy, prism inclined-plane because of light easily and be subjected to easily ectocine, and make thrashing.
The focus type critical method is to utilize plano-convex lens that incident beam is focused on to measure on the interface, thereby measures the refractive index of focal spot.The advantage of the method is that measuring accuracy is not subjected to that index distribution on the interface is different and influenced, the terminator of imaging end hot spot obviously, measurement range is large more than the divergence form critical method, maintain easily, be easy to large-scale production and application.Can improve the interference of system's anti-interface bubble and impurity by installing to be inverted, improve system accuracy thereby reduce systematic error.The focal length of image distance, object distance and lens by changing illuminator can increase the scope of prism test surface incident angle, enlarges the refractometry scope thereby reach.
Summary of the invention
The object of the invention is to propose a kind of measuring instrument of measuring the refractive index of liquid-phase gas based on total reflection principle, it utilizes the focus type critical method to measure the refractive index of liquid-phase gas, for gas is differentiated and proximate analysis is laid a good foundation, simultaneously this refractive index have sampling less, measurement, precision height, on-line measurement, the advantage such as easy to maintenance of liquid or liquid-phase gas under the extreme condition such as suitable high pressure.
Realize a kind of measuring instrument for measuring the liquid-phase gas refractive index of the object of the invention, comprising:
The spot light module, it comprises led light source, coupling mechanism, multimode optical fiber and output lens, the light of described led light source output is coupled in the multimode optical fiber through described coupling mechanism, and outgoing after the multimode optical fiber transmission is by described lens focus is to detect liquid-phase gas to be detected;
Survey prism, surface thereof and described testing liquid Surface Contact form reflecting surface, and the light beam after the outgoing of described spot light module is focused to a bit at this reflecting surface, form hot spot, and total reflection and part reflection occur;
The reflected light receiver module, it is used for collecting the light through described prismatic reflection face reflection, and converts the light signal of collecting the output of to electric signal formation image information;
Image analysis module, its image information to output is processed, and extracts the terminator in the hot spot, and then obtains the refractive index of determinand.
As improvement of the present invention, described measuring instrument comprises that also the sampling cavity volume is used for accommodating testing liquid, and its upper face has circular hole, and described testing liquid forms described reflecting surface by the Surface Contact of this circular hole and described detection prism.
As improvement of the present invention, incide in the light beam of bottom surface, incident angle is greater than the light beam generation total reflection of critical angle, and incident angle is less than the light beam generating unit sub reflector of critical angle, and its portion of energy is transmitted in the liquid-phase gas to be measured.
As improvement of the present invention, the terminator that described image analysis module is extracted in the hot spot can adopt following method:
(a) in light spot image, draw and get a zone that comprises described terminator;
(b) to selected zone, with the wherein view data stack of every delegation, obtain the view data after delegation superposes;
(c) to the view data after the stack of this row, with wherein arbitrarily the difference between row pixel and its previous column pixel as slope, with the point of slope maximum as boundary point.
Spot light module of the present invention can be by changing the distance that shaven head and lens of light source, the distance of the focal length of plano-convex lens and plano-convex lens and prism upper surface, change the size of the angle of divergence of incident beam, thereby strengthen measurement range and the system accuracy of refractive index.According to Si Nieer (Snell) principle, when light was refracted into optically thinner medium from optically denser medium, the refraction angle was greater than incident angle, and the refraction angle increases with the increase of incident angle, and when incident angle increases to certain value, the refraction angle will be increased to 90 degree.Light beam middle part light splitter is with total reflection, and the energy of other a part of light is with the transmission of part reflecting part in the light beam.Such as Fig. 3, when incident angle was greater than or equal to critical angle, transmission did not occur in incident ray; When incident angle during less than critical angle, incident ray generation transmission, energy of reflection light reduces.Incident beam is constant and Refractive Index of Glass Prism n1 is certain, and when liquid refractivity n2 occurs relatively to change, critical angle θ c will change along with the variation of n2.By calculating the position of terminator in the flare, just can be by calculating the organic solution density value.
The optical prism of refractometer of the present invention can be equilateral prism, and the light beam that pointolite sends is through lens focus, and converging ray is focused into a bit at prism test surface S2 through prism S1 face.Sensing point contacts with testing liquid on the S2 face, a part of angle light generation total reflection, in addition a part of light generating unit sub reflector.Light through the reflection of S2 face is converged on the CCD image planes by lens through the S3 face.
The effect of the ray-collecting module of refractometer of the present invention is thereby that flare is coupled to the whole receptions that realize flare on the light-sensitive surface of CCD, and converts the light signal that receives to electric signal output.This CCD can be the line array CCD of one dimension, also can be the area array CCD of two dimension.
The spot light module of refractometer of the present invention is to be made of LED, coupling mechanism, multimode optical fiber and output lens.The light of LED output couples light in the multimode optical fiber through coupling mechanism, can think a branch of pointolite with certain angle of divergence through the light beam of multimode optical fiber.The coupling fiber output beam enlarges the angle of divergence through lens and focuses of the light beam on the prism test surface.This module can improve by the angle of divergence of expanded light beam measurement range and the precision of system.
Refractometer of the present invention adopts the focus type critical angle method, can overcome the inhomogeneous impact of prism test surface material refractive index.Can be inverted at the measurement timer, can guarantee that like this measurement point contacts with liquid-phase gas to be measured or liquid, thereby improve the system rejection to disturbance ability.The present invention does not need the specialized designs fine structure will survey prism to carry out encapsulation process, and the air-gap on prism inclined-plane is not subject to external action simultaneously.This refractometer utilizes the focus type critical angle method can measure the liquid gas with high strength pressure, and the divergence form critical angle method is because prism bottom surface and testing liquid contact area are larger, and the prism encapsulation process is difficult.
Another object of the present invention is to provide a kind of method for measuring the liquid-phase gas refractive index, comprising:
S1: utilize light source to produce the LED light beam that is used for measurement;
S2: light beam is focused on the prism facets of surveying prism, and this prism facets and described liquid-phase gas Surface Contact to be measured form reflecting surface, and light beam focuses at this reflecting surface and forms hot spot, and total reflection and part reflection occur;
S3: collect the light through described reflecting surface reflection, and the light spot image of collecting is processed, extract the terminator in the hot spot, and then can obtain the refractive index of determinand.
That apparatus and method of the present invention are measured the liquid-phase gas refractive index and had the precision height, safeguard is simple, realize easily, antijamming capability is strong, measured the advantages such as environmental impact is little.
Description of drawings
Fig. 1 is a kind of for liquid-phase gas refractive index on-line measurement instrument of the embodiment of the invention.
Fig. 2 is the structural drawing of spot light module in the embodiment of the invention.
Fig. 3 is critical angle method reflection ray and transmitted ray synoptic diagram in the embodiment of the invention.
Fig. 4 is flare figure ideally in the embodiment of the invention.
Among Fig. 5, (a) being the principle schematic of focus type critical method of the present invention, (b) is the principle schematic of the divergence form critical method of prior art.
Fig. 6 be certain liquid-phase gas on the CCD image planes terminator with component variations in refractive index figure.
When Fig. 7 is the refractive index measuring instrument measurement saline solution of the embodiment of the invention, the graph of relation of saline solution concentration and pixel.
Fig. 8 is the refractometer of the embodiment of the invention when measuring certain liquid phase mixed gas, the terminator figure of light spot received.
Embodiment
The present invention will be further described below in conjunction with the drawings and specific embodiments, but the present invention is not limited only to this embodiment.
Such as Fig. 1, the refractive index measuring instrument of present embodiment comprises LED optical fibre illumination module 1, surveys prism 3, high pressure liquid phase gas sample cavity volume 4, energy of reflection light collection module 5 and image processing module 7.
Liquid-phase gas to be measured enters sampling cavity volume 4 by the entrance in the sampling module 4 of measuring instrument, and the liquid-phase gas that enters sampling cavity volume 4 contacts with detection prism 3 bottom surfaces and forms reflecting surface.Air in the sampling cavity volume 4 or impurity are discharged by the outlet of sampling cavity volume 4.This sampling cavity volume 4 in the present embodiment can bear 50 atmospheric pressure, is fit to the sampling of most liquid-phase gas.
LED fiber optic point source lighting module 1 will incide the light beam of surveying prism 3 and focus on detection prism 3 bottom surfaces.Incide the light beam of bottom surface, incident angle is greater than the light beam generation total reflection of critical angle; Incident angle is less than the light beam generating unit sub reflector of critical angle, and namely some energy transmission is in liquid-phase gas to be measured.Flare is coupled on the CCD image planes of receiver module 5 through lens 5 through the light beam of surveying boundary reflection.CCD converts the light signal that receives to electric signal and is input in the image processing module 7.The flare image that is obtained by image processing module 7 extracts the terminator in the hot spot, and obtains the relational expression of terminator position and liquid-phase gas refractive index to be measured, then can obtain the refractive index of liquid-phase gas to be measured.
Extract for the terminator in the hot spot in the present embodiment that can preferably to adopt the differential method differential method be to judge critical angle by the difference of reflected light light intensity relatively, this is so that it possesses anti-interference strong advantage.According to the Fresnel reflection principle, when the liquid of a certain density covers sensor prism surperficial, there is a terminator in the image of the hot spot that cmos image sensor photographs, density is higher, the boundary movement of more turning right, and the displacement of the recruitment of density and boundary is linear.This image boundary can be extracted by the differential method.Demarcate the position of the known titer boundary in image of several groups of density, just can calculate by the boundary recognizer density and the refractive index of liquid to be measured.
Adopt the concrete image algorithm principle of the differential method as follows in the present embodiment: a) to draw and get the zone, as shown in Figure 4, border circular areas is that CMOS claps the hot spot in the image, there is a terminator in the hot spot, in order to guarantee measurement range and measuring accuracy, at first draw in the circular light spot zone and get a rectangular region (rectangular region in the upper figure hot spot), the data of only taking out in the square frame are processed; (b) by the row stack, for selected rectangular region, the stacked data of every delegation is added up, finally obtain the data after delegation superposes.This method by the row stack can increase the interference free performance of system; (c) FIR filtering, design FIR low-pass filter, filtering high frequency noise, the interference free performance of increase algorithm; (d) boundary is extracted, and native system adopts Slope Method to extract boundary, and namely for i row pixel, the difference between i+1 row pixel and the i row pixel is as slope, and with the point of the slope maximum position as boundary, wherein i is arbitrary integer.
Online liquid-phase gas refractive index measuring instrument of the present invention not only can be surveyed the refractive index of solution, the refractive index of electrolytic solution can also be measured the refractive index of liquid-phase gas.In the constant situation of liquid-phase gas air pressure, because that glass material bears pressure capability is generally less, glass is stressed simultaneously is directly proportional with contact area, thereby so the area that should be smaller than liquid-phase gas to be measured avoid glass prism because of stressed excessive breaking.Traditional refractometer is because detection area is larger, can only measure solution and can not measure the refractive index of the liquid-phase gas with larger pressure.This refractive index measuring instrument is the principle of utilizing total reflection in the physical optics, and employing focus type critical angle method measurement liquid-phase gas refractive index can realize the measurement to the liquid-phase gas refractive index, and the required sampling face of the method is little, is easy to the liquid-phase gas of high pressure is measured.
Measuring instrument of the present invention can carry out refractometry to the liquid-phase gas under the high pressure, can certainly measure the refractive index of the liquid under the high pressure or the various liquid under the normal pressure.
A kind of method for measuring the liquid-phase gas refractive index of the present invention comprises:
S1: utilize light source to produce the LED light beam that is used for measurement;
S2: light beam is focused on the prism facets of surveying prism, and this prism facets and described liquid-phase gas Surface Contact to be measured form reflecting surface, and light beam focuses at this reflecting surface and forms hot spot, and total reflection and part reflection occur;
S3: collect the light through described reflecting surface reflection, and the light spot image of collecting is processed, extract the terminator in the hot spot, and then can obtain the refractive index of determinand.
The reflecting surface that the contact of liquid-phase gas to be measured and prism facets forms is can be with the spot size of light beam consistent or adapt.Liquid-phase gas to be measured is contained in one and opens in the round-meshed cavity volume 4, this cavity volume surface and prism facets butt, and liquid-phase gas to be measured contacts with prism facets by this circular hole and forms reflecting surface.This circular hole is very little, can bear the high pressure of liquid-phase gas to guarantee it, and this circular hole can be consistent with spot size.
The physical model of measuring instrument of the present invention can be determined by Snell law, Fresnel reflection law and total reflection principle.The refractometer measurement range can be evaluated by following formula,
n
x＝n
g?sinθ
c
In the formula, n
xBe test substance refractive index, n
gBe glass refraction, θ
cBe critical angle, θ
iBe incident angle, θ
zBe angle of transmission, R
nReflectivity for the prism test surface.Determine and the formula of measuring principle refractometer measurement range [n according to the ranges of incidence angles of interface glazed thread
Min, n
Max] have:
The below describes with specific performance and the use of concrete example to refractive index measuring instrument of the present invention.
Example 1
Utilize measuring instrument of the present invention when room temperature saline solution density to be measured and compared with the standard hand-held Density Measuring Instrument, measuring method is as follows:
With the common salt aqueous solution of different densities gradient, utilize the Abbe refractometer instrument to measure first, by the standard hand-held Density Measuring Instrument its concentration is measured again.
With the sampling module of distilled water cleaning the present invention type model machine, common salt aqueous solution to be measured is put into sampling module.The spot light module focuses on the light beam of light source on the interface of surveying prism and saline solution, and the light beam of process boundary reflection is coupled on the light-sensitive surface of CCD by receiving light path.By the VC interface boundary information in the light spot received is extracted, and obtain refractive index and the density of testing liquid by image algorithm, and refractive index value and density value and Abbe refractometer apparatus measuring value and standard hand-held Density Measuring Instrument measured value compared, calculate simultaneously relative error.It is that the LED of 532nm is coupled to multimode optical fiber that above-mentioned LED coupled fiber module is selected wavelength.
Use the same method and to be left common salt aqueous solution and to measure, and obtain common salt aqueous solution refractive index and variable density curve.
Example 2
Utilize measuring instrument of the present invention when room temperature distilled water, 75% medicinal alcohol, saturated Nacl solution and certain concentration sucrose solution density to be measured and compared with the Abbe refractometer instrument, measuring method is as follows:
With mentioned solution, utilize the Abbe refractometer instrument to measure first, again solution is put into respectively the sampling module of the invention type model machine of having calibrated.Obtain the refractive index of each solution by the VC algorithm.Solution refractive index and Abbe refractometer measured value are compared, and calculate relative error.Table 1 measures various normal fluid refractive index value for this refractometer and Abbe refractometer compares.
The comparison of the various liquid measure values of table 1. and Abbe measured value
Example 3
Utilize measuring instrument of the present invention at low temperatures certain liquid phase component gases refractive index to be measured, and by refractive index qualitative analysis gas composition, measuring method is as follows:
Liquid-phase gas to be measured is exported the entrance that is connected on the model machine sampling module by copper pipe, when liquid-phase gas enters sampling module, outlet valve and liquid-phase gas inlet valve are closed.Liquid-phase gas to be measured is because action of gravitation contacts and form reflecting surface with detection prism S3 face.LED optical fibre illumination module and CCD are powered on, and LED optical fibre illumination module will be pooled to the light beam of certain angle of divergence on the reflecting surface of surveying prism S3 and liquid-phase gas to be measured formation, and convergent beam at reflecting surface total reflection and part reflection occurs.The light beam of generating unit sub reflector has part energy and projects in the liquid-phase gas to be measured, energy-producing loss.The energy that the light beam of generating unit sub reflector enters receiving system is determined by the Fresnel reflection rate curve.Light beam through reflection is coupled on the image planes of CCD by receiving system.Along with the variation of component, the terminator of hot spot also changes on the CCD image planes.Fig. 8 is that terminator is with component variations in refractive index figure.
Claims (7)
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| CN103454247A (en) * | 2013-08-26 | 2013-12-18 | 华中科技大学 | Wide-range refractive index measuring device and method |
| CN103645119A (en) * | 2013-12-17 | 2014-03-19 | 哈尔滨工程大学 | Point light source-based measuring device for measuring liquid density of matrix CCD (Charged Coupled Device) |
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