CN100491974C - Combined chemical spectral detection system - Google Patents

Combined chemical spectral detection system Download PDF

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CN100491974C
CN100491974C CNB2005100318000A CN200510031800A CN100491974C CN 100491974 C CN100491974 C CN 100491974C CN B2005100318000 A CNB2005100318000 A CN B2005100318000A CN 200510031800 A CN200510031800 A CN 200510031800A CN 100491974 C CN100491974 C CN 100491974C
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light
detection system
spectral detection
combined chemical
sample cell
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CN1880943A (en
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易江平
黄莉
李文生
周小平
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Microvast Power Systems Huzhou Co Ltd
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Microvast Technology Huzhou Co Ltd
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Abstract

The invention discloses a spectro-detecting system, which is characterized by the following: realizing synchronous multi-group detection for multiple samples in the composite sample library through different frequency optical sources; containing variable frequency or utility serial filtrate light source, detecting plate with M*N transmission sample pools (M and N is between 2 and 100 or more) and high-resolution CCD digital detector for device (as picture displays); detecting transmission information through high-resolution CCD digital camera; calculating the density of specific material in kinds of samples according to background and data through self-designed software; analyzing quantatively for hundreds of samples within several seconds for combined chemical samples.

Description

Combined chemical spectral detection system
Technical field
The present invention relates to a kind of material that utilizes and had the characteristic of specific absorption frequency, analyzed the spectral detection system of hundreds and thousands of organic or inorganic samples simultaneously, be particularly suitable for the analysis of combinatorial chemistry sample Library at ultraviolet and visible region.
Background technology
The characteristics of combinatorial chemistry are can synthesize the sample of big quantity at short notice and carry out fast detecting, and whether having the ability of analyzing big quantity sample simultaneously and handling mass data then is decision combinatorial chemistry research key of success.Product sign and quantitative test be the bottleneck of combinatorial chemistry normally.
In assembly catalyze research, people designed hyperchannel gas chromatography (GC) detection system carry out product analysis (Thomas N.Corso et al., US 6,318,157; Fermier, US 6,743, and 356; Reetz et al.Catalysis Today 67 (2001) 389-396).Hyperchannel GC installs the detecting device of big quantity and the chromatographic column of big quantity owing to impossible, thus also can only reach limited number of channels usually, such as: 4 to 6 passages.For Library with more sample, must adopt clack box to switch, its complex structural designs and Control Software design are also complicated.Another shortcoming of hyperchannel GC is that its mensuration also is list type rather than high-throughout.Liquid chromatography (LC) also faces same problem (Safir et a1.US 6,475,391).
Another kind of method is to utilize scanning of the mass spectrum (Armin et al.US 6,723,983:Claus et al.Catalysis Today 67 (2001) 319-339; Maier et al.Angew.Chem.Int.Ed.38 (1999) 2791-2792).Mass spectrum can be realized quick scanning, if but scanning not with the chromatographic column coupling, at each material that many times can not distinguish in the potpourri.If application of gas chromatorgraphy/mass, sweep velocity are very slow.For example scan the alkene and the complicated compound of some molecular structures of alkane and same carbon number, the mass spectrum probe must carry out machinery and move, and mensuration is list type, and it is not high to detect flux.
Willson and Maier (Willson et al.Ind.Eng.Chem.Res.35 (1996) 4801-4803; Maier et al.Angew.Chem.Int.Ed.37 (1998) 2644) etc. having developed with infrared thermal imaging IR-CCD camera is the detection method of detecting device, but they be Preparation of Catalyst on a flat board, when what take place on catalyzer is because the temperature of catalyst surface raises or during the chemical reaction that reduces, the IR-CCD camera directly reads the temperature of catalyst surface, thereby judges the degree of carrying out of reaction.This method has following shortcoming: 1) because many chemical reactions all have thermal effect, can't judge to generate what product; 2) product on the catalyst sample plate and product counterdiffusion mutually, product also can be on other sample exothermic heat of reaction; 3) solid catalytic material is owing to form difference, even under same temperature, its infrared intensity also can be different, thereby produce noise, and ground unrest is very strong.Employing IRspectroscopy imaging technology such as Snively are carried out express-analysis (the Snively et al.OPTICSLETTERS 24 (1999) 1841 of product; Catalysis Today 67 (2001) 357-368).This The Application of Technology can have the different different materials of infrared signature frequency difference according to each material, and detect when carrying out various product, but there be the infrared problem low to gas detection sensitivity, and because the restriction of infrared beam diameter, a branch of infrared light can not pass a plurality of sample cells simultaneously, and (otherwise infrared energy density is lower, sensitivity also can be lower), usually this method also can only be measured 1-4 sample simultaneously, may not accomplish high throughput analysis, in addition because many materials do not have infrared active, so limited the range of application of this method yet.
Senkan etc. have designed a multiphoton Ionization Detection device (Resonance-enhanced multiphoton ionization (REMPI) that resonance strengthens, Selim M.Senkan, NATURE 394 (1998) 350), its principle is to adopt the valency layer electronics of Ultra-Violet Laser ionized molecule to make molecule charged, thereby is applying the material that the detection of discharge generation current signal is ionized on the electrode of certain voltage then.Can detect various materials on this theoretical method, but in fact the ionization energy difference is little owing to various materials,, can only distinguishes and resemble benzene and the king-sized material of this class ionization energy difference of thiacyclohexane so use is little in actual applications with different ionization energy.
McFarland (J.Comb.Chem.4 (2002) 563-568) etc. has designed a kind of hydrogen detecting device, and its principle is WO 3Evaporation on glass plate, and then the Metal Palladium evaporation in WO 3On, hydrogen can be W under the effect of palladium 6+Be reduced into W oxide at a low price, W oxide at a low price has color, can obtain the growing amount of hydrogen by colorimetric analysis.But this detecting device is only effective to hydrogen, does not have universal use.
Edward S.Yeung waits and has designed a kind of laser fluorescence imaging method (Anal.Chem.73 (2001) 4434-4440) analysis can produce molecular fluorescence under laser radiation gaseous material.That this method has is highly sensitive, can realize characteristics such as big quantity sample scanning, but only be useful for the detection of some palycyclic aromatics, because have only the big Polycyclic aromatic hydrocarbons of this class under action of ultraviolet laser, just to send molecular fluorescence, so being of limited application of this class methods.
U.S. Pat 6,410,332 disclose a kind of molecular fluorescence imaging method analyzes from the synthetic product of combinatorial chemistry.Its principle of work is to use a kind of chemical reagent and the reaction of a certain analysans to generate epipolic material, under the effect of ultraviolet light, produce fluorescence then, adopt the fluorescence imaging method to collect data, this method has been expanded the range of application of the fluorescence imaging method of Edward S.Yeung development effectively, but does not still analyze the compound that those can not after chemical reaction generation fluorescent substance, its range of application is less.
Summary of the invention
The combined chemical spectral detection system that the present invention relates to as shown in the drawing, it is made up of light source, light distribution plate, sample holder, transmission sample pond array board, filter plate (if light source is the monochromatic source of frequency adjustable, then need not filter plate), CCD camera, data acquisition and processing (DAP) software and computing machine.The light that comes out from light source becomes the uniform light of intensity after through the light distribution plate, and described smooth distribution plate is plastics or frosted glass.These light are through the analysans in each sample cell in the sample cell array, arrive the CCD camera then and measure the transmitted intensity of each sample simultaneously, obtain the absorbance of each sample by contrast, determine the concentration of the material in each sample then by typical curve and Beer law with blank sample.The collection of these data is all finished by specially designed software and computing machine with processing.We just can realize analyzing simultaneously hundreds and thousands of samples like this.The advantage of this method is that instruments design is simple, cost is low, almost can analyze all substances that have characteristic absorption wavelength after all substances with characteristic absorption wavelength of ultraviolet light and visible region and after chemical reaction.Because Beer law is the formula that everybody uses always, the colorimetric analysis that is based upon on the Beer law is very accurately, and its quantitative analytical data is very reliable, so native system is a cheap and good-quality high throughput analysis systems.
Description of drawings
Fig. 1 is the principle schematic of this combined chemical spectral detection system.
Fig. 2 is the sample photo.
Fig. 3 makees the photo of background for water.
Embodiment
Measure acryl aldehyde concentration
With the potassium bichromate solution 1.0mL of 0.10M, the sulfuric acid 1.0mL of 1.0M and 200 μ L concentration be the acrolein solution of 0.15M, 0.25M, 0.35M, 0.55M, 0.75M and 0.85M mix six solution examples.After reacting half an hour, respectively get 80 μ L and in the array sample pond, analyze, get Fig. 2 photo (other blank is a water sample).Other prepares a blank contrast water sample array, gets Fig. 3 photo after the analysis, and the data of Fig. 2 and Fig. 3 correspondence are respectively listed in the table 1,2.The difference of the transmission integrated value of counter sample is equivalent to absorbance in table 2 and the table 1.Determine the concentration value of acryl aldehyde by absorbance and typical curve.Actual compound concentration value, absorbance, actual measurement concentration and the error of acryl aldehyde have been listed in the table 3.
The transmission integrated value of counter sample among table 1 Fig. 2
The transmission integrated value of table 2 Fig. 3 empty sample
Figure C200510031800D00052
The concentration determination of table 3 acryl aldehyde
Figure C200510031800D00062

Claims (14)

1, a kind of combined chemical spectral detection system is characterized in that it is made up of digital detecting device of light source, optical filter, light distribution plate, sample holder, combinatorial chemistry transmission pond array board, CCD and part of data acquisition; Described smooth distribution plate is assigned to all directions equably to the light that light source sends, make the light intensity that sees through any one sample cell in the array of transmission pond almost equal, each sample cell on the sample cell array board is crossed in described only transmission simultaneously through light source and light distribution plate, the digital detecting device of described CCD writes down the transmitted light information by each sample cell simultaneously, and described light source is the ordinary light source of ultraviolet, visible region.
2, combined chemical spectral detection system according to claim 1 is characterized in that, before described optical filter is added in the digital detecting device camera lens of CCD, optical filter see through the characteristic absorption wavelength that wavelength should be material to be analyzed.
3, combined chemical spectral detection system according to claim 1 is characterized in that, described smooth distribution plate is plastics or frosted glass.
4, combined chemical spectral detection system according to claim 1, it is characterized in that, having M * N to be arranged in the transparent but opaque sample cell of pool wall in the bottom of array on the array board of described combinatorial chemistry transmission pond forms, each sample cell bottom requires to see through ultraviolet light and visible light, its material can maybe can see through other material of ultraviolet light and visible light for quartz glass, M wherein, N 〉=2.
5, combined chemical spectral detection system according to claim 4 is characterized in that, M, N are 2-100.
6, combined chemical spectral detection system according to claim 1 is characterized in that, the digital detecting device of described CCD is black and white or colored CCD digital camera, array diode, video camera or similar detecting device.
7, combined chemical spectral detection system according to claim 1 is characterized in that, algorithm that described part of data acquisition is related and software can carry out while integration and processing to transmitted light information strength on each sample of the digital detector recording of CCD.
8, a kind of combined chemical spectral detection system is characterized in that it is made up of digital detecting device of light source, light distribution plate, sample holder, combinatorial chemistry transmission pond array board, CCD and part of data acquisition; Described smooth distribution plate is assigned to all directions equably to the light that light source sends, make the light intensity that sees through any one sample cell in the array of transmission pond almost equal, each sample cell on the sample cell array board is crossed in described only transmission simultaneously through light source and light distribution plate, the digital detecting device of described CCD writes down the transmitted light information by each sample cell simultaneously, and described light source is the monochromatic source of ultraviolet, visible region frequency adjustable.
9, combined chemical spectral detection system according to claim 8 is characterized in that, described smooth distribution plate is plastics or frosted glass.
10, combined chemical spectral detection system according to claim 8, it is characterized in that, having M * N to be arranged in the transparent but opaque sample cell of pool wall in the bottom of array on the array board of described combinatorial chemistry transmission pond forms, each sample cell bottom requires to see through ultraviolet light and visible light, its material can maybe can see through other material of ultraviolet light and visible light for quartz glass, M wherein, N 〉=2.
11, combined chemical spectral detection system according to claim 10 is characterized in that, M, N are 2-100.
12, combined chemical spectral detection system according to claim 8 is characterized in that, the digital detecting device of described CCD is black and white or colored CCD digital camera, array diode, video camera or similar detecting device.
13, combined chemical spectral detection system according to claim 8, it is characterized in that algorithm that described part of data acquisition is related and software can carry out while integration and processing to transmitted light information strength on each sample of the digital detector recording of CCD.
14, combined chemical spectral detection system according to claim 8 is characterized in that, described monochromatic source is to be realized by the method for manually or automatically regulating light frequency.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103323564B (en) * 2013-06-28 2015-01-14 北京大学 Research device for generating singlet oxygen through natural organic matter, and control method of research device
CN104964927B (en) * 2015-06-08 2018-09-21 上海蓝怡科技股份有限公司 A kind of multisample detection device
CN105136684A (en) * 2015-08-14 2015-12-09 上海蓝怡科技股份有限公司 Multi-sample detection device and method
CN109100305B (en) * 2018-07-13 2022-02-18 陕西师范大学 Digital substance information acquisition device and method for liquid dispersion system
CN110243816A (en) * 2019-07-05 2019-09-17 北京知几未来医疗科技有限公司 A kind of device detected for material concentration in body fluid

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
Development of A High Throughput Method IncorporatingTranditional Analytical Devices. C.C. White 等.Journal of Research of the National Institute of Standards and Technology,Vol.109 No.5. 2004
Development of A High Throughput Method IncorporatingTranditional Analytical Devices. C.C. White 等.Journal of Research of the National Institute of Standards and Technology,Vol.109 No.5. 2004 *
High-Throughput Screening in Heterogeneous ReactionUsing Chemical Indicators. 孙波等.催化学报,第26卷第5期. 2005
High-Throughput Screening in Heterogeneous ReactionUsing Chemical Indicators. 孙波等.催化学报,第26卷第5期. 2005 *
高通量筛选技术在多相催化研究中的应用. 任军等.化工进展,第21卷第7期. 2002
高通量筛选技术在多相催化研究中的应用. 任军等.化工进展,第21卷第7期. 2002 *

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