CN102252983A - Deep ultraviolet spectrum measurement and spectrophotometry measurement device - Google Patents

Deep ultraviolet spectrum measurement and spectrophotometry measurement device Download PDF

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Publication number
CN102252983A
CN102252983A CN2011101183769A CN201110118376A CN102252983A CN 102252983 A CN102252983 A CN 102252983A CN 2011101183769 A CN2011101183769 A CN 2011101183769A CN 201110118376 A CN201110118376 A CN 201110118376A CN 102252983 A CN102252983 A CN 102252983A
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China
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deep
drop
deep ultraviolet
ultraviolet
silica fibre
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黄国亮
李强
黎新
丘天
王同舟
张也
马丽
陈圣伊
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Tsinghua University
CapitalBio Corp
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Tsinghua University
CapitalBio Corp
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/33Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N2021/0346Capillary cells; Microcells
    • G01N2021/035Supports for sample drops

Abstract

The invention discloses a deep ultraviolet spectrum measurement and spectrophotometry measurement device. The measurement device comprises a transmissive deep ultraviolet deep ultraviolet spectrum measurement and spectrophotometry measurement device and a reflective deep ultraviolet spectrum measurement and spectrophotometry measurement device. A liquid drop holder, an optical fiber sensor, a deep ultraviolet spectrum detection device and signal extraction and multiple-order derivative analysis software are sequentially arranged on the light path of incident light output by an excitation light source of deep ultraviolet; a liquid drop to be detected is arranged between two opposite and parallel solid end faces of the liquid drop holder and the optical fiber sensor. The deep ultraviolet spectrum measurement and spectrophotometry measurement device can be used for measuring a deep ultraviolet spectrum and absorbancy; trace samples of hard drugs and explosives have higher absorption peaks at the deep ultraviolet band than that at the longer wavelength, therefore, the detection sensitivity and resolution ratio for measuring the trace samples of the hard drugs and the explosives can be improved by performing the spectrum measurement and the spectrophotometry measurement in the deep ultraviolet area in an extension manner. According to difference information of absorption spectrum peaks of various hard drugs and explosives at the deep ultraviolet band, the various hard drugs and explosives can be rapidly distinguished and identified, therefore, rapid, sensitive and accurate identification and quantitative analysis on various common hard drugs and explosives can be realized.

Description

A kind of deep UV (ultraviolet light) spectrometry and spectrophotometry device
Technical field
The present invention relates to a kind of deep UV (ultraviolet light) spectrometry and spectrophotometry device, the spectrophotometry and the spectrum detection technique field that belong to sample, the particularly deep UV (ultraviolet light) spectrometry and the spectrophotometry of micro-sample can be widely used in the analyses such as drugs, biological sample, chemical example and explosive.
Background technology
At present, China is obtaining great achievement and new progress aspect beat drugs and the terrified crime of blast, but the situation of the terrified crime of anti-drug struggle and blast protection class still allows of no optimist.Domestic drug addiction personnel relapse rate is still higher, increases comparatively fast based on the number of teenager's abuse novel drug, presents the drug species diversification, and the diversified situation of drug abuse has proposed new challenge to police law execution personnel's banning drugs work.Explosive crime mainly shows as terrorist activity, and serious harm social security is stable, and effectively detecting and taking precautions against explosive terrified crime is the necessary guarantee of building a Harmonious Society.
Drug species is various, and in general, it has 4 features: the pressure of force majeure is sucked; Use continuously and escalated dose; This medicine is produced spirit and physical dependence; Produce behind the disconnected medicine and block symptom.The World Health Organization (WHO) is divided into 8 big classes with the material that drugs use: 1. morphine class; 2. barbiturates; 3. alcohol type; 4. cocaines; 5. cunjah class; 6. amphetamine; 7. Ke Te class; 8. psychedelic class.At this type of situation, " about the determine a crime explanation of criterion for imposing penalty relevant issues of trial drug-related case " article one, second that on June 10th, 2000 was played implementation in by the Supreme People's Court stipulated the quantitative criteria of amphetamine, cannabis, cocaine, morphine, Sauteralgyl, Dihydroetorphine Hydrochloride, caffeine, 8 kinds of drugs of pappy shell.This explanation is 9 kinds of novel drug crimes quantitative criteria of the measurement of penalty of having stipulated to determine a crime with regard to common in the present domestic Drug-related crimes, outstanding (methylenedioxy) crystal methamphetamine amphetamines such as (MDMA), ketamine, methadone, triazolam, methaqualone, chlordiazepoxide, estazolam, diazepam (stabilizing), Bromazepam etc.
The terrified crime of exploding often uses the main kind of explosive to comprise PETN (too grace), CE (tetryl), TNT, DNT, RDX (RDX), HMX (HMX), picric acid etc., is that object is identified in the criminal important detection anti-riot, the traffic safety check of public security.
No matter be traffic safety check or the criminal evaluation of public security field, all need to develop a kind of can be at the scene to multiple drugs, explosive etc. carry out fast, sensitive, trace, accurate analytical method.Adopt chromatography (thin-layered chromatography, high performance liquid chromatography, vapor-phase chromatography etc.), combined gas chromatography mass spectrometry (as GC-MS, HPLC-MS, GC-MS-MS, GC-HRMS etc.) etc. that drugs, explosive etc. are detected (CN 1609610A at present mostly; CN 101750458A).But, still there is the bottleneck problem of applying in these analytical approachs, as the pre-service of needs process complicated sample, expensive and bulky instrument and equipment, and require operating personnel with higher technical merit and skill level, it is consuming time and cost is high to analyze sample.Can not satisfy that criminal scene is reconnoitred and the needs of clinical treatment large scale application, this just requires to develop more fast, sensitive, accurate analytical method.
Spectrographic method is based on light and material is done the time spent, the transition between the electronics generation energy level of material molecule inside and the optical wavelength of the emission, absorption or the scattered radiation that produce and the analytical approach of intensity variation, and spectrum and molecular spectrum can atomize.A kind of as molecular spectrum, the uv-visible absorption spectroscopy method is a method of utilizing the radiation of the molecule absorption 200-800nm spectral region of some material to carry out assay determination.This molecular absorption spectrum mainly produces the transition of outer valence electron between electron level in the material molecule.As a kind of analytical approach commonly used, the uv-visible absorption spectroscopy method can be applicable in the differentiation evaluation and quantitative detection field of multiple drug numerator.
Traditional uv-visible absorption spectroscopy method is used quartz sample pool, though can obtain higher sensitivity, it has, and the one-shot measurement amount of samples is too much, sample cell cleans shortcomings such as difficulty and apparatus structure complexity.In addition, at present popular uv-visible absorption spectroscopy method is measured inaccurate at the 200-230nm spectral region, and can not provide the absorbance information of deep ultraviolet wave band, so just make the deep ultraviolet measurement Research seldom, it is blank to can be described as approximate research, business-like pertinent instruments product is still less (1.M.Veronico et al., International journal of pharmaceutics, 1995 (119): 109-114 just; 2.Eda Satana et al., Journal of Pharmaceutical and Biomedical Analysis, 2001 (25): 1009-1013).
In Explosive Residues is measured, also face the constructed problem that similar drugs are measured, use traditional UV-VIS spectrophotometry in the detection of explosive and Analysis and Identification, to have bigger limitation.Therefore, some new detection methods of necessary development and instrument solve the problem that traditional UV-VIS spectrophotometry exists in drugs and explosive are measured, utilize deep UV (ultraviolet light) spectrometry and spectrophotometry method that micro-drugs and explosive are carried out fast detecting and Analysis and Identification and have favorable actual application and be worth.
Summary of the invention
The purpose of this invention is to provide a kind of deep UV (ultraviolet light) spectrometry and spectrophotometry device, this device can solve the problems that traditional ultraviolet spectrophotometry and visible light measuring method exist, can be at the scene to multiple micro-example carry out fast, sensitive, walk abreast, analyzing and testing accurately.
Transmission-type deep UV (ultraviolet light) spectrometry provided by the invention and spectrophotometry device are provided with drop clamper, silica fibre sensor, deep ultraviolet spectrum sniffer, signal extraction and pluriderivative and norm analysis software on the light path of the incident light of deep UV (ultraviolet light) excitation source output successively; Drop to be measured is located between the solid end face of two opposing parallel of described drop clamper and described silica fibre sensor; Described deep ultraviolet spectrum sniffer comprises the circular hole diaphragm that sets gradually along the light path of described incident light or narrow slit, catoptron, quartzy Amici prism or deep ultraviolet spectro-grating, deep UV (ultraviolet light) detector; Described incident light is successively through obtaining the deep ultraviolet absorption spectrum signal of drop to be measured behind described drop clamper, silica fibre sensor, deep ultraviolet spectrum sniffer, signal extraction and pluriderivative and the norm analysis software.
In the above-mentioned measurement mechanism, described deep UV (ultraviolet light) excitation source can be the light beam that deuterium lamp, xenon lamp, LED, laser, tungsten lamp bioluminescence or chemiluminescence etc. produce; Described silica fibre sensor is single mode silica fibre, multimode silica fibre, quartzy optical waveguide, silica fibre array or silica fibre bundle; Described silica fibre array can be the fiber array of being made up of single mode or multimode quartz fibre; Described silica fibre bundle can be the fibre bundle of being made up of single mode or multimode quartz fibre.
In the above-mentioned measurement mechanism, described Fibre Optical Sensor has hydrophobic characteristics with the surface that described drop to be measured contacts, and described testing sample solution can form a pearl drop to be measured on the surface of described Fibre Optical Sensor, and does not extend.
In the above-mentioned measurement mechanism, described drop clamper can be quartz lens, quartzy dull and stereotyped or other optical elements with optical alignment function; The one side that described drop clamper contacts with described drop to be measured is plane or concave surface, described plane or concave surface need be handled examination with dichlorodimethylsilane or other deactivation, soak or wipe examination and handle as the octyl group trimethoxy silane, make the surface have hydrophobic character, liquid stands and does not spread apart rapidly at surface energy, and the described micrometer drop for the treatment of is in stable compression or draws loose state by the effect of surface force.
In the above-mentioned measurement mechanism, described catoptron can be deep UV (ultraviolet light) concave reflection collimating mirror or plane mirror; Described deep UV (ultraviolet light) detector can be line ccd detector, face ccd detector, photomultiplier, photoelectric cell, photodiode or other opto-electronic conversion detecting elements, requirement has good response characteristic to deep UV (ultraviolet light), can improve its deep UV (ultraviolet light) response characteristic by plating deep ultraviolet anti-reflection film.
In the above-mentioned measurement mechanism, described signal extraction and pluriderivative analysis software are located on the computing machine, can read the signal of described deep ultraviolet spectrum sniffer by described computer interface in real time, and show, storage, pluriderivative and norm analysis, calculate the content of absorbance and sample.
Reflective deep UV (ultraviolet light) spectrometry provided by the invention and spectrophotometry device are provided with silica fibre sensor, drop clamper, deep ultraviolet spectrum sniffer, signal extraction and pluriderivative and norm analysis software on the light path of the incident light of deep UV (ultraviolet light) excitation source output successively; Drop to be measured is located between the solid end face of two opposing parallel of described drop clamper and described Fibre Optical Sensor; Described deep ultraviolet spectrum sniffer comprises the circular hole diaphragm that sets gradually along the light path of described incident light or narrow slit, catoptron, quartzy Amici prism or deep ultraviolet spectro-grating, deep UV (ultraviolet light) detector; Described drop clamper is provided with reflectance coating with the one side that described drop to be measured contacts; Through being obtained reflected light by the reflection of the reflectance coating of described drop clamper behind described silica fibre sensor, drop to be measured and the drop clamper, described reflected light is more successively through obtaining the deep ultraviolet absorption spectrum signal of drop to be measured behind described drop to be measured, silica fibre sensor, deep ultraviolet spectrum sniffer, signal extraction and pluriderivative and the norm analysis software successively for described incident light.
In the above-mentioned measurement mechanism, described deep UV (ultraviolet light) excitation source can be the light beam that deuterium lamp, xenon lamp, LED, laser, tungsten lamp bioluminescence or chemiluminescence etc. produce; Described Fibre Optical Sensor can be single mode silica fibre, multimode silica fibre, quartzy optical waveguide, silica fibre array or silica fibre bundle; Described silica fibre array can be the silica fibre array of being made up of single mode or multimode quartz fibre; Described silica fibre bundle can be the fibre bundle of being made up of single mode or multimode quartz fibre.
In the above-mentioned measurement mechanism, described drop clamper can be quartz lens, quartzy dull and stereotyped or other optical elements with optical alignment function; The one side that described drop clamper contacts with described drop to be measured is plane or concave surface, described plane or concave surface need be with dichlorodimethylsilane or other deactivation reagent treatment, soak or wipe examination and handle as the octyl group trimethoxy silane, make the surface have hydrophobic character, liquid stands and does not spread apart rapidly at surface energy, and the described micrometer drop for the treatment of is in stable compression or draws loose state by the effect of surface force; Deielectric-coating or the metal film of described reflectance coating for having good reflection efficient at the deep UV (ultraviolet light) wave band, reflectance coating preferably is plated in the one side that described drop clamper does not contact with described drop to be measured, can improve serviceable life like this.
In the above-mentioned measurement mechanism, described catoptron can be deep UV (ultraviolet light) concave reflection collimating mirror or plane mirror; Described detector can be line ccd detector, face ccd detector, photomultiplier, photoelectric cell, photodiode or other opto-electronic conversion detecting elements, requirement has the good response characteristic to deep UV (ultraviolet light), can improve its deep UV (ultraviolet light) response characteristic by plating deep ultraviolet anti-reflection film.
In the above-mentioned measurement mechanism, described signal extraction and pluriderivative analysis software are located on the computing machine, can read the signal of described deep ultraviolet spectrum sniffer by described computer interface in real time, and show, storage, pluriderivative and norm analysis, calculate the content of absorbance and sample.
The invention provides the application in measuring drugs and/or explosive of above-mentioned transmission-type deep UV (ultraviolet light) spectrometry and spectrophotometry device; Described drugs are morphine class, barbiturates, alcohol type, cocaines, cunjah class, amphetamine, Ke Te class or psychedelic class; Described explosive is pentaerythritol tetranitrate (PETN, grace too), tetryl (CE, tetryl), trinitro-toluene (TNT), dinitrotoluene (DNT) (DNT), cyclotrimethylene trinitramine (RDX, RDX), cyclotetramethylene-tetranitramine (HMX, HMX) or 2,4,6-trinitrophenol (picric acid).
The present invention also provides above-mentioned reflective deep UV (ultraviolet light) spectrometry and the application of spectrophotometry device in measuring drugs and/or explosive; Described drugs are morphine class, barbiturates, alcohol type, cocaines, cunjah class, amphetamine, Ke Te class or psychedelic class; Described explosive is pentaerythritol tetranitrate (PETN, grace too), tetryl (CE, tetryl), trinitro-toluene (TNT), dinitrotoluene (DNT) (DNT), cyclotrimethylene trinitramine (RDX, RDX), cyclotetramethylene-tetranitramine (HMX, HMX) or 2,4,6-trinitrophenol (picric acid).
Device provided by the invention adopts the pluriderivative method that deep ultraviolet spectrum is carried out single order, second order or higher derivation analysis and norm analysis, null value, minimal value and maximum position at the all-order derivative curve obtain multistage δ (λ) impulse function, realization is accurately located in deep ultraviolet to the whole specificity absorption peaks of near infrared light wave band, emission peak or other spectral signals wavelength location that there were significant differences test substance, the resolution that raising is identified sample composition reaches the purpose that visualized distinguishing is identified heterogeneity in the potpourri.The norm analysis can be used for the composition that identification and detection is mixed drugs or explosive.At first, make up the deep ultraviolet spectrum storehouse of various drugs or explosive; To mix single drugs or explosive spectrum of planting in the spectrum of drugs or explosive and the library of spectra then, the stack spectrum of perhaps multiple drugs or explosive compares; At last their SPECTRAL DIVERSITY is found the solution norm,, reach and identify the purpose of mixing drugs or explosive composition in order to weigh the accuracy of comparison result.
The specific performance index that measurement mechanism provided by the invention can reach is as follows:
(1) the micro-example detection amount ranges of this measurement mechanism adaptation is 0.5 μ L-2 μ L.
(2) the detection sensitivity 0.1 μ g/mL of this measurement mechanism.
(3) the dynamic detection range 0.1 μ g/mL-1000 μ g/mL of this measurement mechanism.
By studies show that, a lot of materials, as drugs, explosive etc., there are specific absorption peak or emission peak at the deep ultraviolet wave band, its peak height and precipitous degree are bigger, more remarkable than the spectrum of ultraviolet-visible optical band, utilize this characteristic can improve the detection sensitivity of substance spectra measurement and spectrophotometry.Simultaneously, the deep ultraviolet wave band is existed specific absorption peak or emission peak, the absorption spectrum of ultraviolet-visible optical band or emission spectrum, and the absorption spectrum of near infrared or infrared band or emission spectrum etc. are joined together, can realize the multispectral survey of test substance and the specificity evaluation at a plurality of absorption or emission spectrum peak, improve the accuracy of identifying material, especially distinguish material close, similar quality; Compare with traditional uv-visible absorption spectroscopy method, utilize measurement mechanism measurement provided by the invention have amount of samples few (receive be raised to 50 microlitres from 1), can be in characteristics such as deep ultraviolet wave band (reaching 180nm) detections.
Description of drawings
Fig. 1 is the transmission-type deep UV (ultraviolet light) spectrometry of the embodiment of the invention 1 and the structural representation of spectrophotometry device.
Fig. 2 is the reflective deep UV (ultraviolet light) spectrometry of the embodiment of the invention 2 and the structural representation of spectrophotometry device.
Fig. 3 is the deep ultraviolet spectrum sniffer structural representation in the embodiment of the invention 1 and the example 2.
Fig. 4 is the deep UV (ultraviolet light) spectrometry spectrogram of drugs cocainehydrochloride in the embodiment of the invention 3.
Fig. 5 is the characteristic peak analysis processing result of the deep UV (ultraviolet light) spectrometry spectrogram of drugs cocainehydrochloride in the embodiment of the invention 3, wherein Fig. 5 (1) is the first order derivative of the cocainehydrochloride curve of spectrum, and Fig. 5 (2) is differentiate δ (λ) impulse function of back null value, minimal value and maximum position correspondence of the cocainehydrochloride curve of spectrum.
Fig. 6 is the picric deep UV (ultraviolet light) spectrometry of an explosive spectrogram in the embodiment of the invention 4.
Fig. 7 is the characteristic peak analysis processing result of the picric deep UV (ultraviolet light) spectrometry of explosive spectrogram in the embodiment of the invention 4, wherein Fig. 7 (1) is the first order derivative of the picric acid curve of spectrum, and Fig. 7 (2) is differentiate δ (λ) impulse function of back null value, minimal value and maximum position correspondence of the picric acid curve of spectrum.
Each mark is as follows among Fig. 1, Fig. 2 and Fig. 3: 11 deuterium lamps, 21 xenon lamps, 12 and 22 silica fibres, 13 and 23 deep ultraviolet spectrum sniffers, 14 and 24 drops to be measured, 15 and 25 signal extractions and pluriderivative and norm analysis software, 16 and 26 is quartzy dull and stereotyped, 17 and 27 computing machines, 31 circular hole diaphragms, 32 deep ultraviolet spectro-gratings, 33 deep UV (ultraviolet light) concave reflection collimating mirrors, 34 deep UV (ultraviolet light) ccd detectors.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing, but the present invention is not limited to following examples.
Embodiment 1, transmission-type deep UV (ultraviolet light) spectrometry and spectrophotometry device
Transmission-type deep UV (ultraviolet light) spectrometry that present embodiment provides and spectrophotometry device, be provided with quartzy dull and stereotyped 16 on the light path of the incident light of deuterium lamp 11 outputs successively, single mode silica fibre 12, deep ultraviolet spectrum sniffer 13, signal extraction and pluriderivative and norm analysis software 15 and computing machine 17, drop 14 to be measured be located at quartzy dull and stereotyped 16 and the solid end face of two opposing parallel of single mode silica fibre 12 between, quartzy flat board 16 soaks with dichlorodimethylsilane with drop 14 contacted one sides to be measured or wipes examination and handle, make the surface have hydrophobic character, liquid stands and does not spread apart rapidly at surface energy, makes drop 14 to be measured be in stable compression or draw loose state by the effect of surface force; Deep ultraviolet spectrum sniffer 13 comprises circular hole diaphragm 31, deep UV (ultraviolet light) concave reflection collimating mirror 32, deep ultraviolet spectro-grating 33 and the deep UV (ultraviolet light) ccd detector 34 (be a kind of typical spectrometer architecture, but require concave reflection collimating mirror, spectro-grating, ccd detector etc. to have good deep UV (ultraviolet light) responding ability) that sets gradually along the light path of incident light; Incident light passes through quartzy dull and stereotyped 16 successively, single mode silica fibre 12, deep ultraviolet spectrum sniffer 13, obtain the deep ultraviolet absorption signal of drop 14 to be measured behind signal extraction and pluriderivative and the norm analysis software 15, signal extraction and pluriderivative and norm analysis software 15 are installed on the computing machine 17, can read the signal of deep ultraviolet spectrum sniffer 13 by computer interface in real time, handle deep ultraviolet-near infrared light spectral curve that the back shows sample, obtain null value with the all-order derivative curve, multistage δ (λ) impulse function of minimal value and maximum position correspondence, and calculate the content of absorbance and sample.
In the above-mentioned measurement mechanism, the deep UV (ultraviolet light) excitation source can also be xenon lamp, LED, laser, tungsten lamp or other illuminating source; Fibre Optical Sensor can also be multimode silica fibre or optical waveguide, also can also be fiber array, the fibre bundle of single mode or multimode silica fibre composition; The one side that single mode silica fibre 12 contacts with drop 14 to be measured requires to carry out surface hydrophobicity and handles, and also available octyl group trimethoxy silane soaks or wipes examination and handle, and makes the surface have hydrophobic character, and liquid stands and do not spread apart rapidly at surface energy; Deep ultraviolet spectrum sniffer 13 also can be made up of narrow slit, plane mirror, quartz prism and deep UV (ultraviolet light) ccd detector 34 etc.; Detector also can be photomultiplier, photodiode, photoelectric cell or other opto-electronic conversion detecting element, and requiring has the good response characteristic to deep UV (ultraviolet light), can improve its deep UV (ultraviolet light) response characteristic by plating deep ultraviolet anti-reflection film; The drop clamper can also be quartz lens or other optical element with optical alignment function.
Embodiment 2, reflective deep UV (ultraviolet light) spectrometry and spectrophotometry device
Reflective deep UV (ultraviolet light) spectrometry and spectrophotometry device that present embodiment provides are provided with quartzy flat board 26, single mode silica fibre 22, deep ultraviolet spectrum sniffer 23 and signal extraction and pluriderivative and norm analysis software 25 successively on the light path of the incident light of xenon lamp 21 outputs; Drop 24 to be measured be located at quartzy dull and stereotyped 26 and the solid end face of two opposing parallel of single mode silica fibre 22 between, quartzy flat board 26 soaks with dichlorodimethylsilane with drop 24 contacted one sides to be measured or wipes examination and handle, make the surface have hydrophobic character, liquid stands and does not spread apart rapidly at surface energy, makes drop 24 to be measured be in stable compression or draw loose state by the effect of surface force; Deep ultraviolet spectrum sniffer 23 comprises circular hole diaphragm 31, deep UV (ultraviolet light) concave reflection collimating mirror 32, deep ultraviolet spectro-grating 33 and the deep UV (ultraviolet light) ccd detector 34 (be a kind of typical spectrometer architecture, but require concave reflection collimating mirror, spectro-grating, ccd detector etc. to have good deep UV (ultraviolet light) responding ability) that sets gradually along the light path of incident light; Be coated with the reflectance coating (not shown) on quartzy flat board 26 and the drop 24 contacted one sides to be measured, this reflectance coating is the deielectric-coating that has good reflection efficient at the deep UV (ultraviolet light) wave band, reflectance coating also can be plated in quartzy dull and stereotyped 26 upper surface (promptly not with drop 24 contacted one sides to be measured), can improve serviceable life like this; Incident light passes through single mode silica fibre 22 successively, reflectance coating reflection on drop 24 to be measured and the quartzy dull and stereotyped 26 back quilts quartzy dull and stereotyped 26 obtains reflected light, this reflected light passes through drop 24 to be measured more successively, single mode silica fibre 22, obtain the deep ultraviolet absorption signal of drop to be measured behind deep ultraviolet spectrum sniffer 23 and signal extraction and pluriderivative and the norm analysis software 25, signal extraction and pluriderivative and norm analysis software 25 are installed on the computing machine 27, can read the signal of deep ultraviolet spectrum sniffer 23 by computer interface in real time, handle deep ultraviolet-near infrared light spectral curve that the back shows sample, obtain null value with the all-order derivative curve, multistage δ (λ) impulse function of minimal value and maximum position correspondence, and calculate the content of absorbance and sample.
In the above-mentioned measurement mechanism, the deep UV (ultraviolet light) excitation source can also be deuterium lamp, LED, laser, tungsten lamp or other illuminating source; The silica fibre sensor can also be multimode silica fibre or optical waveguide, also can also be fiber array, the fibre bundle of single mode or multimode silica fibre composition; The one side that single mode silica fibre 22 contacts with drop 24 to be measured requires to carry out surface hydrophobicity and handles, and also available octyl group trimethoxy silane soaks or wipes examination and handle, and makes the surface have hydrophobic character, and liquid stands and do not spread apart rapidly at surface energy; Deep ultraviolet spectrum sniffer 23 can be made up of narrow slit, plane mirror, quartzy Amici prism and deep UV (ultraviolet light) ccd detector 34 etc.; Detector also can be photomultiplier, photodiode, photoelectric cell or other opto-electronic conversion detecting element, requires deep UV (ultraviolet light) is had good response characteristic, can improve deep ultraviolet spectrum response characteristic by plating deep UV (ultraviolet light) anti-reflection film; The drop clamper can also be quartz lens or other optical element with optical alignment function; Reflectance coating also can be metal film.
The measurement mechanism of embodiment 3, use embodiment 1 is measured the drugs cocainehydrochloride
(1) be that 2: 1: 1 proportioning is miscible with water, ethanol, chloroform according to volume ratio, solvent is measured in preparation, and low temperature is frozen.Solvent also can be the water of one matter composition or the chloroform (as 50%) of Different concentrations of alcohol (as 100%) or variable concentrations etc.
(2) utilize the solution that disposes, dissolving drugs cocainehydrochloride.
(3) (preparation has the specimen of variable concentrations gradient to get the sample solution of cocainehydrochloride, from 0.1 μ g/mL-1000 μ g/mL), utilize micropipettor with the surface of 0.5 μ L sample drop, adjust incident light and make it can be coupled into sample drop to single mode silica fibre 12.
(4) utilize the transmission-type deep UV (ultraviolet light) spectrometry of embodiment 1 and spectrophotometry device to survey the spectrum of transmitted light in deep ultraviolet-near infrared range, the spectral detection experimental result as shown in Figure 4, effectively spectral measurement ranges is 180nm-1100nm, the curve of spectrum of the corresponding solvent of solid black lines among the figure, the corresponding curve of spectrum that adds the cocainehydrochloride sample solution of light grey dotted line clearly has tangible spectral absorption at dark purple outskirt.
(5) absorbance of calculation sample in deep ultraviolet-near infrared range, and the curve of spectrum carried out single order, second order or multistage differentiate, obtain multistage δ (λ) impulse function corresponding with null value, minimal value and the maximum position of all-order derivative curve, to determine the position at each absorption peak, emission peak or the remarkable flex point place that suddenlys change, analysis result as shown in Figure 5, Fig. 5 (1) is the first order derivative of the cocainehydrochloride curve of spectrum, and Fig. 5 (2) is differentiate δ (λ) impulse function of back null value, minimal value and maximum position correspondence of the cocainehydrochloride curve of spectrum.
(6) position difference of utilizing the absorption peak of different drugs or explosive sample correspondence and playing the peak dot corresponding wavelength can be distinguished fast and differentiates it, and utilizes the absorbance of absorption peak correspondence can realize quantitative measurment to sample size concentration.
The measurement mechanism of embodiment 4, use embodiment 2 is measured explosive picric acid
(1) be that 1: 1 proportioning is miscible with water, acetonitrile according to volume ratio, solvent is measured in preparation, and low temperature is frozen.Solvent also can be the water of one matter composition or the acetonitrile of variable concentrations (as 10%, 100%).
(2) utilize the solution that disposes, dissolving explosive picric acid.
(3) (preparation has the specimen of variable concentrations gradient to get picric sample solution, from 0.1 μ g/mL-1000 μ g/mL), utilize micropipettor with the surface of 2 μ L sample drops, adjust incident light and make it can be coupled into sample drop to single mode silica fibre 22.
(4) utilize the reflective deep UV (ultraviolet light) spectrometry of embodiment 2 and spectrophotometry device to survey the spectrum of reflected light in deep ultraviolet-near infrared range, the spectral detection experimental result as shown in Figure 6, effectively spectral measurement ranges is 180nm-1100nm, the curve of spectrum of the corresponding solvent of solid black lines among the figure, the corresponding curve of spectrum that adds the picric acid sample solution of light grey dotted line clearly has tangible spectral absorption at dark purple outskirt.
(5) absorbance of calculation sample in deep ultraviolet-near infrared range, and the curve of spectrum carried out single order, second order or multistage differentiate, obtain multistage δ (λ) impulse function corresponding with null value, minimal value and the maximum position of all-order derivative curve, to determine the position at each absorption peak, emission peak or the remarkable flex point place that suddenlys change etc., analysis result as shown in Figure 7, Fig. 7 (1) is the first order derivative of the picric acid curve of spectrum, and Fig. 7 (2) is differentiate δ (λ) impulse function of back null value, minimal value and maximum position correspondence of the picric acid curve of spectrum.
(6) position difference of utilizing the absorption peak of different drugs or explosive sample correspondence and playing the peak dot corresponding wavelength can be distinguished fast and differentiates it, and utilizes the absorbance of absorption peak correspondence can realize quantitative measurment to sample size concentration.
Measurement mechanism provided by the invention can be applicable to but is not limited to the quick differentiation and the quantitative measurment of amphetamine (example hydrochloric acid ketamine etc.), barbiturates (as barbital, phenobarbital etc.), cunjah class (as tetrahydrocannabinol etc.), cocaines (example hydrochloric acid cocaine etc.), psychedelic class (as MDMA etc.) and other kinds (as stable, surazepam etc.) drugs.The present invention also can be applicable to but is not limited to pentaerythrite four nitric acid (PETN, grace too), tetryl (CE, tetryl), trinitro-toluene (TNT), dinitrotoluene (DNT) (DNT), cyclotrimethylene trinitramine (RDX, RDX), cyclotetramethylene-tetranitramine (HMX, HMX), 2,4, the quick differentiation and the quantitative measurment of 6-trinitrophenol (picric acid) and other kind explosive.The measurement mechanism of embodiment 1 and embodiment 2 all is fit to explosive and drugs are measured.

Claims (11)

1. deep UV (ultraviolet light) spectrometry and spectrophotometry device is characterized in that: be provided with drop clamper, silica fibre sensor, deep ultraviolet spectrum sniffer, signal extraction and pluriderivative and norm analysis software successively on the light path of the incident light of deep UV (ultraviolet light) excitation source output; Drop to be measured is located between the solid end face of two opposing parallel of described drop clamper and described Fibre Optical Sensor; Described deep ultraviolet spectrum sniffer comprises circular hole diaphragm or narrow slit, quartzy Amici prism or deep ultraviolet grating, catoptron and the deep UV (ultraviolet light) detector that sets gradually along the light path of described incident light; Described incident light is successively through obtaining the deep ultraviolet absorption spectrum signal of drop to be measured behind described drop clamper, silica fibre sensor, deep ultraviolet spectrum sniffer, signal extraction and pluriderivative and the norm analysis software.
2. measurement mechanism according to claim 1 is characterized in that: described deep UV (ultraviolet light) excitation source is deuterium lamp, xenon lamp, LED, laser or tungsten lamp; Described silica fibre sensor is single mode silica fibre, multimode silica fibre, quartzy optical waveguide, silica fibre array or silica fibre bundle.
3. measurement mechanism according to claim 1 and 2 is characterized in that: described drop clamper is a quartz lens or quartzy dull and stereotyped; Described catoptron is deep UV (ultraviolet light) concave reflection collimating mirror or plane mirror; Described deep UV (ultraviolet light) detector is the opto-electronic conversion detecting element, is specially line ccd detector, face ccd detector, photomultiplier, photodiode or photoelectric cell.
4. according to arbitrary described measurement mechanism among the claim 1-3, it is characterized in that: described signal extraction and pluriderivative and norm analysis software are located on the computing machine.
5. according to arbitrary described measurement mechanism among the claim 1-4, it is characterized in that: the one side that described drop clamper contacts with described drop to be measured is plane or concave surface.
6. deep UV (ultraviolet light) spectrometry and spectrophotometry device is characterized in that: be provided with drop clamper, silica fibre sensor, deep ultraviolet spectrum sniffer and signal extraction and pluriderivative and norm analysis software successively on the light path of the incident light of deep UV (ultraviolet light) excitation source output; Drop to be measured is located between the solid end face of two opposing parallel of described drop clamper and described Fibre Optical Sensor; Described deep ultraviolet spectrum sniffer comprises circular hole diaphragm or narrow slit, quartzy Amici prism or deep ultraviolet grating, catoptron and the deep UV (ultraviolet light) detector that sets gradually along the light path of described incident light; Described drop clamper is provided with reflectance coating with the one side that described drop to be measured contacts; Through being obtained reflected light by the reflection of the reflectance coating of described drop clamper behind described Fibre Optical Sensor, drop to be measured and the drop clamper, described reflected light is more successively through obtaining the deep ultraviolet absorption spectrum signal of drop to be measured behind described drop to be measured, silica fibre sensor, deep ultraviolet spectrum sniffer, signal extraction and pluriderivative and the norm analysis software successively for described incident light.
7. measurement mechanism according to claim 6 is characterized in that: described deep UV (ultraviolet light) excitation source is deuterium lamp, xenon lamp, LED, laser or tungsten lamp; Described silica fibre sensor is single mode silica fibre, multimode silica fibre, quartzy optical waveguide, silica fibre array or silica fibre bundle.
8. according to claim 6 or 7 described measurement mechanisms, it is characterized in that: described drop clamper is a quartz lens or quartzy dull and stereotyped; Described catoptron is deep UV (ultraviolet light) concave reflection collimating mirror or plane mirror; Described deep UV (ultraviolet light) detector is the opto-electronic conversion detecting element, is specially line ccd detector, face ccd detector, photomultiplier, photodiode or photoelectric cell.
9. according to arbitrary described measurement mechanism among the claim 6-8, it is characterized in that: described signal extraction and pluriderivative and norm analysis software are located on the computing machine.
10. according to arbitrary described measurement mechanism among the claim 6-9, it is characterized in that: the one side that described drop clamper contacts with described drop to be measured is plane or concave surface.
11. arbitrary described deep UV (ultraviolet light) spectrometry and the spectrophotometry device application in measuring drugs and/or explosive among the claim 1-10; Described drugs are morphine class, barbiturates, alcohol type, cocaines, cunjah class, amphetamine, Ke Te class or psychedelic class; Described explosive is pentaerythritol tetranitrate, tetryl, trinitro-toluene, dinitrotoluene (DNT), cyclotrimethylene trinitramine), cyclotetramethylene-tetranitramine or 2,4, the 6-trinitrophenol.
CN2011101183769A 2011-05-09 2011-05-09 Deep ultraviolet spectrum measurement and spectrophotometry measurement device Pending CN102252983A (en)

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Application publication date: 20111123