CN203606278U - Double-beam infrared spectrometric analyzer - Google Patents

Double-beam infrared spectrometric analyzer Download PDF

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Publication number
CN203606278U
CN203606278U CN201320687825.6U CN201320687825U CN203606278U CN 203606278 U CN203606278 U CN 203606278U CN 201320687825 U CN201320687825 U CN 201320687825U CN 203606278 U CN203606278 U CN 203606278U
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infrared
sample
light
detecting device
monochromator
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CN201320687825.6U
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Chinese (zh)
Inventor
严九洲
马启睿
张博然
陈薇羽
张炳铖
王文喆
漆星剑
李萌
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Southwest Petroleum University
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Southwest Petroleum University
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Abstract

The utility model discloses a double-beam infrared spectrometric analyzer. The double-beam infrared spectrometric analyzer is characterized by being composed of a light source, a monochromator, an absorption tank, a detector and a recording instrument. Two infrared light beams generated by the light source respectively pass through a sample tank and a reference tank; a reference light beam passes through an attenuator, and a sample light beam passes through a light slitter; the two light beams are collected on a light collector to form one beam to enter the monochromator; when a sample absorbs the infrared light with a certain wavelength, the sample light beam is weakened, and the strengths of the two light beams are unequal; the detector generates a signal, the signal is amplified by a pre-amplifier, a synchronous rectifier and a filtering and modulating amplifier to obtain an amplified electric signal, and the amplified electric signal drives a synchronous motor to drive the attenuator to be inserted into a reference light path, so that the strength of the reference light beam is weakened to be equal to the strength of the sample light beam. According to the instrument, the self noise interferences are overcome, an analysis result is more accurate and reliable, and the application range of an infrared spectrum technology is enlarged.

Description

A kind of twin-beam infrared spectrometric analyzer
Technical field
The utility model belongs to Infrared spectroscopy determination techniques field, relates in particular to a kind of twin-beam infrared spectrometric analyzer.
Background technology
Infrared light is the electromagnetic wave between visible ray and microwave, and its wavelength coverage is 0.80--1000 μ m, can be divided into near-infrared region, middle infrared and far infrared region.The wavelength coverage of near-infrared region is 0.80-2.5 μ m, and the wavelength coverage of middle infrared is 2.5-25 μ m,, the wavelength coverage of far infrared region is 25-1000 μ m.Material molecule produces to the infrared ray of different wave length the absorption curve absorbing and obtain and is called infrared spectrum.In chemical field, infrared spectroscopy (infrared spectroscopy, IR) is mainly used in Study of Molecular Structure, also can carry out compound qualitative, quantitative test.Peak position in spectrogram, peak is strong, and peak shape and peak number are the foundations of infrared analysis.The infrared spectrum of molecule is normally caused by the vibrational energy level of each group and chemical bond in molecule and rotational energy level transition, therefore claim again vibrational spectrum.
The application of infrared spectrum is very extensive, in geologic prospecting, and petroleum industry, petrochemical industry, textile industry, daily chemical industry, many fields such as energy technology can be used.For example, in petroleum industry, can utilize the kerogenic structure of postgraduate's petrologen of infrared spectrum quantitative and qualitative analysis, type and the variation in geology evolution process, evaluate raw hydrocarbon potentiality, determines organic degree of ripeness; Study design feature and the mechanism of action of various treating agents.In petrochemical complex, utilize infrared spectrum to carry out octane number and diesel cetane-number must be predicted, measure the analysis of oil dope and the analysis of railway grease etc.
Infrared spectrum is also one of important means of heterogeneous catalyst research.It can provide the much information about absorption, understands the Active sites of catalyzer, the crystallization process of Study of Catalyst and crystallization degree, identify the type of catalyst surface acid sites, content and intensity, determine that catalyst backbone element compares and catalyzer intermediate ion location, movement and valence state etc.
At biology, in medical science and pharmacy, can be with GC-FTIR coupling technique to the medicine in biological fluid, anesthetic, excitant and metabolic product thereof are analyzed, to blood, carbamate in urine samples carries out Accurate Determining, explores atherosclerotic formation mechanism and process.Can also classify to bacterium rapidly and differentiate with FTIR is easy, the structure of the biomacromolecule such as Study on Protein and nucleic acid, the complex system of research cell and tissue, carry out the clinical medicine auxiliary diagnosis of early diagnosis of tumor and other various diseases, evaluate various preparation formulations, the research crystal formation of polymorph medicine and the relation of drug effect, distinguish medicine isomers, chemical reaction course during drugs is synthetic, purity and the quality etc. of evaluation response product.In addition, infrared spectrum is drug identification according to one of, can also determine the chemical constitution of unknown medicine in conjunction with other Spectrum Analysis.
Abney and Fesiting first record the near infrared spectrum of organic compound (NIR, near infrared spectroscopy), nineteen twenty-eight, Brackett has recorded first high-resolution NIR figure, and has explained the spectral signature about group.There is afterwards commercial NIR instrument, and adopted NIR to measure the moisture in agricultural byproducts, grease and protein content, and NIR is applied to organic chemistry, the fields such as polymkeric substance and pharmaceutical chemistry.But because the analytical test sensitivity of NIR is low, noise of instrument serious interference, makes test result undesirable, and more difficult to microcomponent and gas analysis, the rationality of mensuration and deal with data, also can have influence on net result.
Therefore be necessary to improve the sensitivity of spectral analysis test, overcome the noise of instrument self, make analysis result become more accurately reliable, expand the range of application of infrared spectrum technology.
Summary of the invention
The purpose of this utility model is to provide a kind of twin-beam infrared spectrometric analyzer, and this spectrometer can overcome the deficiencies in the prior art, improves the degree of accuracy of analytical test.
A kind of twin-beam infrared spectrometric analyzer, is characterized in that: this instrument is by light source, monochromator, absorption cell, detecting device and record instrument composition; Produce two infrared beams respectively by sample cell and reference cell by light source; Reference beam is through attenuator, and sample beam is through chopper, and two-beam line merges into a light beam at light manifold, enter into monochromator, monochromator produces two light wire sizes, and a light signal is transferred to synchronous motor after amplifying, and another optical signal transmission is in detecting device; If sample is to the infrared ray of a certain wavelength without absorption, two-beam intensity equates on detecting device, there is no signal output; When sample produces while absorbing the infrared ray of a certain wavelength, sample beam is weakened, and two-beam intensity not etc., does not have signal to produce on detecting device; This signal is through prime amplifier, synchronous rectifier, and the amplification signal that filtering modulated amplifier obtains after amplifying drives synchronous motor to drive attenuator to insert reference light paths, and reference beam remitted its fury to sample beam is equated; Registering instrument can be synchronizeed with attenuator, and in the time that attenuator moves, registering instrument is drawn out the Strength Changes of absorption of sample signal simultaneously, and the infrared ray that monochromator can produce different wave length arrives detecting device.
A kind of twin-beam infrared spectrometric analyzer, is characterized in that, described chopper is fan-shaped catoptron.
A kind of twin-beam infrared spectrometric analyzer, is characterized in that, described light source can be stablized the high-intensity continuous infrared light of transmitting, adopts Elema, Nernst glower, iodine-tungsten lamp or the red-hot Aze of 1100 ℃ of left and right.
A kind of twin-beam infrared spectrometric analyzer, is characterized in that, described monochromator is by prism or grating dispersion original paper, incident and exit slit, and catoptron, concave mirror forms.
A kind of twin-beam infrared spectrometric analyzer, is characterized in that, described monochromator is selected NaCl, KBr, KRS-5, CaF 2infrared light transmission material is made prism, absorption cell window, detector window.
A kind of twin-beam infrared spectrometric analyzer, is characterized in that, described sample cell is divided into two kinds of gas sample cell and liquid sample pools, and its part and parcel is infrared light transmission window, with the non-aqueous solution of NaCl crystal, or CaF 2aqueous solution infrared light transmission material make infrared light transmission window.
A kind of twin-beam infrared spectrometric analyzer, is characterized in that, described detecting device adopts sulfuric acid three glycosides peptide (TGS) pyroelectricity detecting devices, and mercury cadmium tellurium (MCT) detecting device or vacuum thermocouple are as detecting device.
The vibrational energy level of molecule is quantized, and the structure of vibrational energy level extent and molecule is closely related.When molecule absorption after the infrared radiation of certain frequency, during from vibrational energy level ground state transition to first excited state, the absorption peak of generation is at fundamental frequency peak, its corresponding vibration frequency equals the ultrared frequency that it absorbs.From vibrational energy level ground state transition to Second Excited State, the absorption peak that the 3rd excited state etc. produces, is respectively two frequency multiplication peaks and frequency tripling peak.In fact, the vibration frequency at frequency multiplication peak is always more lower slightly than the integral multiple of the vibration frequency at fundamental frequency peak.Weak many in the strength ratio fundamental frequency peak at frequency multiplication peak, and more than frequency tripling peak is difficult to directly measure because intensity is extremely weak.
In infrared spectrum, often have multiple absorption peaks, a kind of fundamental vibration form that each main absorption peak is corresponding conventionally, has its eigen vibration frequency.The vibration of polyatomic molecule has two large types, i.e. stretching vibration (stretching vibration) and flexural vibrations (bending vibration).It is flexible along key direction of principal axis that stretching vibration refers to into key atom, makes the variation vibration of bond distance's generating period, and its bond angle remains unchanged.In the time that the atomicity in molecule is greater than 3, its stretching vibration can also be divided into two kinds of symmetrical stretching vibration and asymmetric stretching vibrations.The former each key in the time of vibration elongates or shortens simultaneously; When the latter is illustrated in vibration, when some key extends, other keys shorten.
While carrying out flexural vibrations, the variation of the bond angle generating period of group, and its bond distance remains unchanged.Because the force constant of flexural vibrations is less than stretching vibration, therefore corresponding absorption peak appears at conventionally compared with low frequency end.The various groups that contain in polyatomic molecule and chemical bond may produce multiple fundamental vibration form, and each fundamental vibration form may produce an infrared absorption peak.But in fact, the peak number on infrared spectrum is often less than fundamental vibration number, its main cause is: infrared inactivity vibration wherein does not produce infrared absorption peak, and the identical vibration of frequency is merged into an absorption peak; Wide and strong absorption peak can be covered contiguous narrow and weak absorption peak; Peak and the intensity too weak peak instrument of frequency outside instrument frequency range all can not show.
Based on above analysis, a kind of twin-beam infrared spectrometric analyzer mainly comprises light source, monochromator, absorption cell, the part such as detecting device and recording system composition.Launch two bundle infrared rays by light source, respectively by sample cell and reference cell.Reference beam meets on chopper with sample beam after attenuator, chopper is fan-shaped catoptron, rotated with the frequency of 10Hz by synchronous machine drives, can make reference beam and sample beam alternately enter into monochromator by entrance slit, in monochromator, continuous radiant light by grating (or prism) dispersion after, through collimating mirror, exit slit, more alternately arrive detecting device.If sample is to the infrared ray of a certain wavelength without absorption, two-beam intensity equates on detecting device, there is no signal output.When sample produces and absorbs the infrared ray of a certain wavelength, sample beam is weakened, and two-beam intensity is unequal, has signal to produce on detecting device.This signal inserts reference light paths through amplifying the synchronous electronic drive attenuator of rear drive, and reference beam remitted its fury to sample beam is equated.In registering instrument, recording pointer is synchronizeed with attenuator, and in the time that attenuator moves, recording pointer is drawn out the Strength Changes of absorption of sample signal simultaneously; Recording pointer is also synchronized with the movement with grating, and the rotation of grating makes the infrared ray of different wave length from monochromator, penetrate and arrive detecting device successively.So can obtain take T% or A as ordinate the infrared spectrum that absorption of sample was produced that is horizontal ordinate with wavelength or wave number.
A kind of twin-beam infrared spectrometric analyzer, its light source can be stablized the high-intensity continuous infrared light of transmitting, can adopt the Elema of 1100 ℃ of left and right, Nernst glower, iodine-tungsten lamp or red-hot Aze etc.Monochromator is the core component of infrared spectroscopy spectroanalysis instrument, mainly by the dispersion such as prism or grating original paper, incident and exit slit, catoptron, the formations such as concave mirror.For fear of producing aberration, in instrument, do not use lens.Due to glass, quartz almost all absorbs infrared ray, therefore should select suitable infrared light transmission material to make prism, absorption cell window, detector window etc.Conventional infrared light transmission material comprises: NaCl, KBr, KRS-5, CaF 2deng, except rear both, all easily moisture absorptions of most of infrared light transmission materials, therefore should guarantee that instrument works except in wet environment specific.
Infrared absorption of sample pond is divided into two kinds, gas absorption cell and liquid absorption pond, and its part and parcel is infrared light transmission window.Conventionally use the non-aqueous solution of NaCl crystal, or CaF 2the infrared light transmission material such as aqueous solution make window.For fixed sample, can be dispersed in KBr and be added after being pressed into translucent sheet and be measured, also can make solution and be encased in absorption cell and measure.For the superpolymer sample of hot melt, also can be made into film and measure for analyzing.Because infrared photon energy is lower, be not enough to cause photoelectron emissions, therefore can not make detecting device with photoelectric tube or photomultiplier.Can adopt sulfuric acid three glycosides peptide (TGS) pyroelectricity detecting devices, mercury cadmium tellurium (MCT) detecting device or vacuum thermocouple are as infrared detector.
Registering instrument adopts the operation of computer control instrument, carries out data processing and spectrogram retrieval.
Accompanying drawing explanation
1--light source; 2--infrared beam; 3--sample cell; 4--reference cell; 5--chopper; 6--attenuator;
7--light manifold; 8--monochromator; 9--detecting device; 10--prime amplifier; 11--synchronous rectifier;
12--filtering modulated amplifier; 13--synchronous motor; 14--registering instrument; 15--synchronous motor; 16--amplification signal;
17--reference beam; 18--sample beam;
Embodiment
Produce two infrared beams (2) respectively by sample cell (3) and reference cell (4) by light source (1).Reference beam (17) is through attenuator (6), sample beam (18) is through chopper (5), chopper (5) is fan-shaped catoptron, two-beam line merges into a light beam at light manifold (7), enter into monochromator (8), monochromator (8) produces two light wire sizes, and a light signal is transferred to synchronous motor (13) after amplifying, and another optical signal transmission is in detecting device (9).
If sample is to the infrared ray of a certain wavelength without absorption, two-beam intensity equates on detecting device (9), there is no signal output.When sample produces while absorbing the infrared ray of a certain wavelength, sample beam (18) is weakened, and two-beam intensity not etc., does not have signal to produce on detecting device (9).This signal is through prime amplifier (10), synchronous rectifier (11), the amplification signal (16) that filtering modulated amplifier (12) obtains after amplifying drives synchronous motor (15) to drive attenuator (6) to insert reference light paths, and reference beam (17) remitted its fury to sample beam (18) is equated.
Registering instrument (14) can be synchronizeed with attenuator (6), and in the time that attenuator (6) is mobile, registering instrument (14) is drawn out the Strength Changes of absorption of sample signal simultaneously, and the infrared ray that monochromator (8) can produce different wave length arrives detecting device (9); So can obtain take T% or A as ordinate the infrared spectrum that absorption of sample was produced that is horizontal ordinate with wavelength or wave number.

Claims (7)

1. a twin-beam infrared spectrometric analyzer, is characterized in that: this instrument is by light source, monochromator, absorption cell, detecting device and record instrument composition; Produce two infrared beams respectively by sample cell and reference cell by light source; Reference beam is through attenuator, and sample beam is through chopper, and two-beam line merges into a light beam at light manifold, enter into monochromator, monochromator produces two light wire sizes, and a light signal is transferred to synchronous motor after amplifying, and another optical signal transmission is in detecting device; If sample is to the infrared ray of a certain wavelength without absorption, two-beam intensity equates on detecting device, there is no signal output; When sample produces while absorbing the infrared ray of a certain wavelength, sample beam is weakened, and two-beam intensity not etc., does not have signal to produce on detecting device; This signal is through prime amplifier, synchronous rectifier, and the amplification signal that filtering modulated amplifier obtains after amplifying drives synchronous motor to drive attenuator to insert reference light paths, and reference beam remitted its fury to sample beam is equated; Registering instrument can be synchronizeed with attenuator, and in the time that attenuator moves, registering instrument is drawn out the Strength Changes of absorption of sample signal simultaneously, and the infrared ray that monochromator can produce different wave length arrives detecting device.
2. a kind of twin-beam infrared spectrometric analyzer as claimed in claim 1, is characterized in that, described chopper is fan-shaped catoptron.
3. a kind of twin-beam infrared spectrometric analyzer as claimed in claim 1, is characterized in that, described light source can be stablized the high-intensity continuous infrared light of transmitting, adopts Elema, Nernst glower, iodine-tungsten lamp or the red-hot Aze of 1100 degrees Celsius of left and right.
4. a kind of twin-beam infrared spectrometric analyzer as claimed in claim 1, is characterized in that, described monochromator is by prism or grating dispersion original paper, incident and exit slit, and catoptron, concave mirror forms.
5. a kind of twin-beam infrared spectrometric analyzer as claimed in claim 1, is characterized in that, described monochromator is selected NaCl, KBr, KRS-5, CaF 2infrared light transmission material is made prism, absorption cell window, detector window.
6. a kind of twin-beam infrared spectrometric analyzer as claimed in claim 1, is characterized in that, described sample cell is divided into two kinds of gas sample cell and liquid sample pools, and its part and parcel is infrared light transmission window, with the non-aqueous solution of NaCl crystal, or CaF 2aqueous solution infrared light transmission material make infrared light transmission window.
7. a kind of twin-beam infrared spectrometric analyzer as claimed in claim 1, is characterized in that, described detecting device adopts sulfuric acid three glycosides peptide (TGS) pyroelectricity detecting devices, and mercury cadmium tellurium (MCT) detecting device or vacuum thermocouple are as detecting device.
CN201320687825.6U 2013-11-03 2013-11-03 Double-beam infrared spectrometric analyzer Expired - Fee Related CN203606278U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106442377A (en) * 2016-09-24 2017-02-22 大连理工大学 Real-time double-beam in-situ infrared spectrum system and method thereof
CN109085134A (en) * 2018-10-12 2018-12-25 江苏省精创电气股份有限公司 A kind of gas leakage infrared radiation detection apparatus and its detection method
CN110887793A (en) * 2018-09-10 2020-03-17 中国石油化工股份有限公司 Modulation wave driving type precision photoelectric detector
CN116465852A (en) * 2023-04-20 2023-07-21 振电(苏州)医疗科技有限公司 Liquid-phase infrared spectrum measuring method and device based on infrared short pulse excitation

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106442377A (en) * 2016-09-24 2017-02-22 大连理工大学 Real-time double-beam in-situ infrared spectrum system and method thereof
WO2018053978A1 (en) * 2016-09-24 2018-03-29 大连理工大学 Real-time double light beam in-situ infrared spectroscopy system and method thereof
CN106442377B (en) * 2016-09-24 2018-11-09 大连理工大学 A kind of real-time dual-beam in-situ ft-ir system and method
CN110887793A (en) * 2018-09-10 2020-03-17 中国石油化工股份有限公司 Modulation wave driving type precision photoelectric detector
CN109085134A (en) * 2018-10-12 2018-12-25 江苏省精创电气股份有限公司 A kind of gas leakage infrared radiation detection apparatus and its detection method
CN116465852A (en) * 2023-04-20 2023-07-21 振电(苏州)医疗科技有限公司 Liquid-phase infrared spectrum measuring method and device based on infrared short pulse excitation

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