CN109142253A - Liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchronous measuring apparatus and method - Google Patents
Liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchronous measuring apparatus and method Download PDFInfo
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Classifications
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- G—PHYSICS
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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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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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Abstract
The invention belongs to liquid phase hybrid reaction kinetic test technical field, in particular to a kind of device and method in milli/musec order, realizing liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchro measure.Including computer and sequential control system, detection light incident system, sample cell, chemical liquids sampling system, waste liquid storage system, liquid phase reactor chemical kinetic systems measuring system, electrochemical meter and data collector, wherein chemical liquids sampling system and waste liquid storage system are connected to the entry to mixed solution of sample cell and mixture export；Detect flow direction emission detection light of the light incident system for the reaction solution along sample cell；Liquid phase reactor chemical kinetic systems measuring system is used to measure the Absorption and fluorescence spectrum of reaction solution；Electrochemical meter is used to measure the electrochemistry spectrum of reaction solution；Data collector is for acquiring spectral signal and electrochemistry spectrum signal.The present invention realizes that absorption spectrum, emission spectrum and electrochemistry compose three parameter synchronic measurements, and it is accurate to measure experimental result.
Description
Technical field
It is the invention belongs to liquid phase hybrid reaction kinetic test technical field, in particular to a kind of in milli/musec order, in fact
The device and method of existing liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchro measure.
Technical background
With the effect machine of protein folding procedure, enzyme kinetics, antibody and antigen binding process and drug molecule
Reason research is that the kinetics of the complicated Polymer Systems of representative controls chemical reaction to the mechanism for understanding chemical reaction
Speed and design new chemical reaction are of great significance.Complicated Polymer Systems react the characteristics of mainly have reaction condition compared with
For complexity, the characteristics such as influence factor is various and reaction rate is slower.The completion of various biochemical processes is be unable to do without various in human body
The catalysis of biological enzyme, the suitable solvated conditions of many enzymes needs or activator activation ability activity with higher, and mesh
The preceding active means of widely applied studying enzyme are exactly the depression effect of inhibitor, this can mean that needs in specific solvent item
The quick mixing of two or three of solution is realized under part, and the rate of enzymatic reaction can pass through the suction of observation reactants and products
It receives the variation that spectrum, fluorescence spectrum or electrochemistry are composed and is calculated.The catalytic constant of most of enzymes is about per second 1 to arrive
10000s-1, such as the catalysis anti-rate constant of alkaline phosphatase and chymotrypsin is about 14s-1And 100s-1, milli microsecond
The liquid phase hybrid reaction chemical kinetic systems and electrochemistry spectrometry technology of resolution be analyze the most strong means of the process (document 1:
Kleniewska,P.,et al.,The NADPH Oxidase Family and its Inhibitors.Archivum
Immunologiae Et Therapiae Experimentalis,2012.60(4),277-294.).The folding of protein and
Unfolding process, it usually needs the conditions such as suitable temperature, ionic type and ionic strength, but due to spectrum widening effect,
The folding process of protein is difficult to observe the change of spectrum in many cases, and the change of electrochemical parameter may be just relatively more aobvious
It writes.Combination of these electrochemical parameters to the metal ion and enzyme active center of description photoinduction, light-catalyzed reaction small molecular
Or the change of pH value has great significance.Such as under the conditions of different temperatures, different pH values, metal in chlorophyll porphyrin ring
In the substitution reaction of ion and proton, single detection means is difficult to accurately describe reaction process, only passes through synchronous light
Spectrum and electrochemistry spectrum combine, and could establish clearly physical image.(document 2:Ke, Z.G., et al., A
fluorescence approach to the unfolding thermodynamics of horseradish
peroxidase based on heme degradation by hydrogen peroxide.Chemical Physics
Letters, 2016.657,49-52. document 3:Qian, Y.D., et al., Electrochemical probing of the
solution pH-induced structural alterations around the heme group in
Myoglobin.Physical Chemistry Chemical Physics, 2013.15 (39), 16941-16948. document 4:
Zhao,X.J.,et al.,Electrochemically Monitoring the Acid and Acidic Urea-
Induced Unfolding of Hemoglobin and Its Electrocatalytic
Ability.Electroanalysis, 2010.22 (19), 2277-2283. document 5:Fedurco, M., et al.,
Electrochemistry of unfolded cytochrome c in neutral and acidic urea
solutions.Journal of the American Chemical Society,2005.127(20),7638-7646.)。
Therefore milli the liquid phase hybrid reaction chemical kinetic systems differentiated of microsecond and electrochemistry spectrometry device will parse complicated polymer body
It is the effective means of dynamic process.
The milli of existing maturation gsec differentiate liquid phase hybrid reaction kinetic test device be concentrated mainly on spectroscopy
In measurement, produce two of the model represent Applied Photophysics company that company is respectively Britain (document 6:
Https: //www.photophysics.com) and France Bio-Logic company (document 7:http: //www.bio-
logic.net/en).The device of the Applied Photophysics company of Britain using high pressure gas as power output, due to
Air pressure, which is affected by temperature larger and different solution viscosity, to be led to flow resistance and changes, and therefore, it is difficult to accurately control solution
Flow velocity and mixing ratio, and mixed process can not form effective feedback；France Bio-Logic company using stepper motor as
Sample introduction power, stepper motor itself have the disadvantages of lower torque, lower overload capacity and slower response, are easy to cause
The inaccuracy of step and sample introduction is lost, and due to only having sample introduction motor to provide sample introduction power, is easy to cause over-voltage effect, causes to measure
Inaccuracy；The sample cell function of two companies is all relatively simple simultaneously, sample cell can only measure spectrum parameter or
Electrochemical parameter, and cannot achieve the synchro measure of two or more parameters in reaction process.
Summary of the invention
In view of the deficiencies of the prior art with the demand of complicated Polymer Systems kinetics multi-parameter synchro measure, this hair
It is bright to be designed to provide a kind of liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchronous measuring apparatus and method, can milli
Microsecond is differentiated, and in 200nm to 800nm wave-length coverage, realizes that two or more solution quickly mix and stop its flowing, in turn
The parameters such as reaction solution absorption spectrum, fluorescence spectrum and electrochemistry spectrum in synchro measure chemical reaction process.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of liquid phase reactor chemical kinetic systems and electrochemistry compose synchronous measuring apparatus, which is characterized in that including computer and
Sequential control system, detection light incident system, sample cell, chemical liquids sampling system, waste liquid storage system, liquid phase reactor dynamics
Spectral measurement system, electrochemical meter and data collector, wherein the sample cell is used for the storage and circulation of reaction solution,
The chemical liquids sampling system and the waste liquid storage system respectively with the entry to mixed solution and mixture export of the sample cell
Connection；The detection light incident system is set to the outside of the sample cell, the flowing for the reaction solution along the sample cell
Direction emission detection light；The liquid phase reactor chemical kinetic systems measuring system is set to the outside of the sample cell, for measuring
The Absorption and fluorescence spectrum of reaction solution；The electrochemical meter is set in the sample cell, for measuring reaction solution
Electrochemistry spectrum；The data collector is connect with the liquid phase reactor chemical kinetic systems measuring system and electrochemical meter,
For acquiring spectral signal and electrochemistry spectrum signal；The detection light incident system, chemical liquids sampling system, waste liquid storage system
System, liquid phase reactor chemical kinetic systems measuring system, electrochemical meter and data collector with computer and timing control system
System connection.
The liquid phase reactor chemical kinetic systems measuring system includes absorbing light intensity detector, fluorescence monochromator and fluorescent intensity
Detector is oppositely disposed opposite two in the sample cell with the detection light incident system wherein absorbing light intensity detector
Side, the absorption spectrum for absorbing light intensity detector and being used to measure reaction solution, the fluorescence monochromator and fluorescent intensity detector
It is set gradually along the flow direction perpendicular to reaction solution in the sample cell, the fluorescence monochromator is used to export the unicast of fluorescence
In long or full spectrum to fluorescent intensity detector, the fluorescent intensity detector is used to measure the fluorescence spectrum of reaction solution, described glimmering
Light light intensity detector and absorption light intensity detector are connect with the data collector.
The detection light incident system includes probe source and incident monochromator, and the incidence monochromator is along the detection light
The optical path direction in source is arranged, for export the probe source Single wavelength or full spectrum.
The flow cell for reaction solution circulation is equipped in the sample cell, the electrochemical meter is described including being set to
The electrode of two sides and the first electrode data line and second electrode data line that are connect respectively with two electrodes inside flow cell.
The chemical liquids sampling system includes two groups or more single-pipeline liquid-supplying system；
When having two groups of single-pipeline liquid-supplying systems, two groups of single-pipeline liquid-supplying system parallel connections are mixed liquor feed flow pipeline all the way
It is connected to afterwards with the entry to mixed solution of the sample cell；
When with single-pipeline liquid-supplying system more than two, wherein two groups of single-pipeline liquid-supplying system parallel connections are first via mixing
Liquid feed flow pipeline, it is the second road mixed liquor feed flow that first via mixed liquor feed flow pipeline is in parallel with third group single-pipeline liquid-supplying system again
Pipeline, and so on, last mixed liquor feed flow pipeline all the way and the sample cell after multiple single-pipeline liquid-supplying systems are in parallel
Entry to mixed solution connection.
The single-pipeline liquid-supplying system include liquid line, sampling injector, liquid storage syringe, two-position three-way valve and with into
The sample introduction servo motor of sample syringe connection, wherein sampling injector, liquid storage syringe and liquid line be and two-position three-way valve
Connection, for the sample introduction servo motor for driving the sampling injector to carry out imbibition or drain, the sample introduction servo motor is logical
Cross servo control system control.
The waste liquid storage system includes waste liquid syringe, waste liquid servo motor, waste liquid bottle and tapping line, wherein waste liquid
Syringe, waste liquid bottle and tapping line are connect with two-position three-way valve, and the mixed liquor of the tapping line and the sample cell goes out
Mouth connection；The waste liquid servo motor is connect with waste liquid syringe, described for driving the waste liquid syringe imbibition or drain
Waste liquid servo motor is controlled by servo control system.
The liquid feeding pipeline of the chemical liquids sampling system is placed in pipeline thermostat, the sample cell and pipeline thermostat
Temperature pass through temperature controller control.
A kind of measurement method of liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchronous measuring apparatus, the method includes with
Lower step:
1) measure background spectra: the chemical liquids sampling system and waste liquid storage system cooperate, and buffer solution is injected
In sample cell, in the detection light to sample cell of detection light incident system transmitting setting wavelength, pass through liquid phase reactor chemical kinetic systems
The spectrum and electrochemistry of measuring system and electrochemical meter synchro measure buffer solution spectrum are used as background signal；
2) measurement experiment is composed: the chemical liquids sampling system and waste liquid storage system cooperate, and will inject sample to test sample
In product pond, spectral signal and electrochemistry spectrum signal are carried out by liquid phase reactor chemical kinetic systems measuring system and electrochemical meter
Synchronous acquisition；
3) data processing is carried out by computer and sequential control system, synchronous spectrum and electrochemistry spectrum can be obtained.
The liquid phase reactor chemical kinetic systems measuring system includes the absorption light intensity detection along the setting of reaction solution flow direction
Device and edge absorb the absorption of light intensity detector measurement reaction solution perpendicular to the fluorescent intensity detector of reaction solution flow direction setting
Spectrum, fluorescent intensity detector measurement reaction solution fluorescence spectrum, the chemical liquids sampling system and the waste liquid storage system
Time of measuring of the time to stop working relative to the absorption light intensity detector, fluorescent intensity detector and electrochemical meter
There is delay.
The present invention have the advantages that beneficial effect below and:
1. the present invention may be implemented absorption spectrum, emission spectrum and electrochemistry and compose three parameter synchronic measurements.
2. in the present invention introducing of waste liquid servo motor can effectively shorten device measurement dead time, reduce reaction process in
The generation of over-voltage and turbulence effect keeps the experimental result measured more accurate.
3. the present invention uses independent control pipeline thermostat temperature and sample cell temperature, it can be ensured that the storage temperature of reaction solution
The temperature independent control that degree and chemical reaction occur, the condition that more really simulation biochemical reaction carries out.
Detailed description of the invention
Fig. 1 is structure principle chart of the invention；
Fig. 2 is the axonometric drawing of sample cell of the invention；
Fig. 3 is the main view of sample cell of the invention；
Fig. 4 is temperature conditioning unit schematic diagram of the invention；
Fig. 5 is synchronous spectrum measured by the present invention and electrochemistry spectrogram.
Wherein: 1-1 is the first sample introduction servo motor, and 1-2 is the second sample introduction servo motor, and 1-3 is third sample introduction servo electricity
Machine, 1-4 are waste liquid servo motor, and 2-1 is the first sampling injector, and 2-2 is the second sampling injector, and 2-3 is third sample introduction note
Emitter, 2-4 are waste liquid syringe, and 3-1 is the first liquid storage syringe, and 3-2 is the second liquid storage syringe, and 3-3 is third liquid storage note
Emitter, 3-4 are waste liquid bottle, and 4-1 is the first two-position three-way valve, and 4-2 is the second two-position three-way valve, and 4-3 is third two-position three-way valve,
4-4 is the 4th two-position three-way valve two-position three-way valve, and 5-1 is the first mixer, and 5-2 is the second mixer, and 6 be sample cell, 7-1,
7-2,7-4,7-5,7-6 are liquid line, and 7-6 is tapping line, and 7-3 is premixing pipeline, and 8-1 is incident monochromator, and 8-2 is
Fluorescence monochromator, 9-1 are to absorb light intensity detector, and 9-2 is fluorescent intensity detector, and 10-1 is electrochemical meter, and 11 be number
According to collector, 12 be computer and control system, and 13 be servo control system, and 14 be temperature controller, and 15 is permanent for pipeline
Warm slot, 16 be semiconductor chilling plate, and 17 be sample cell temperature sensor, and 18 be pipeline thermostat temperature sensor, and 19 be detection
Light source, a1 are entry to mixed solution, and a2 is mixture export, and b1 is detection light incident surface, and b2 is detection light-emitting face, and c1 is front side
Fluorescence detection face, c2 are rear side fluorescence detection face, and d1 is upper surface electrode, and d2 is lower surface electrode, and e1 is that left first light transmission is close
Quartz plate is sealed, e2 is that the second light transmission seals quartz plate, and f1 is first electrode data line, and f2 is second electrode data line.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, right in the following with reference to the drawings and specific embodiments
The present invention is described in detail.
As shown in Figure 1-3, a kind of liquid phase reactor chemical kinetic systems provided by the invention and electrochemistry compose synchronous measuring apparatus,
Including computer and sequential control system 12, detection light incident system, sample cell 6, chemical liquids sampling system, waste liquid storage system
System, liquid phase reactor chemical kinetic systems measuring system, electrochemical meter 10-1 and data collector 11, wherein sample cell 6 is used for
The storage and circulation of reaction solution, chemical liquids sampling system and waste liquid storage system respectively with the entry to mixed solution a1 of sample cell 6 and
Mixture export a2 connection；Detection light incident system is set to the outside of sample cell 6, the stream for the reaction solution along sample cell 6
Dynamic direction emission detection light；Liquid phase reactor chemical kinetic systems measuring system is set to the outside of sample cell 6, for measuring reaction solution
Absorption and fluorescence spectrum；Electrochemical meter 10-1 is set in sample cell 6, for measuring the electrochemistry of reaction solution
Spectrum；Data collector 11 is connect with liquid phase reactor chemical kinetic systems measuring system and electrochemical meter 10-1, for acquiring light
Spectrum signal and electrochemistry spectrum signal；Detect light incident system, chemical liquids sampling system, waste liquid storage system, liquid phase reactor power
Optical spectra measuring system, electrochemical meter 10-1 and data collector 11 are connect with computer and sequential control system 12.
Liquid phase reactor chemical kinetic systems measuring system includes absorbing light intensity detector 9-1, fluorescence monochromator 8-2 and fluorescence light
Strong detector 9-2 is oppositely disposed opposite two in sample cell 6 wherein absorbing light intensity detector 9-1 and detecting light incident system
Side absorbs the absorption spectrum that light intensity detector 9-1 is used to measure reaction solution, fluorescence monochromator 8-2 and fluorescent intensity detector 9-2
Set gradually along perpendicular to the flow direction of reaction solution in sample cell 6, fluorescence monochromator 8-2 be used to export fluorescence Single wavelength or
In full spectrum to fluorescent intensity detector 9-2, fluorescent intensity detector 9-2 is used to measure the fluorescence spectrum of reaction solution, fluorescent intensity
Detector 9-2 and absorption light intensity detector 9-1 are connect with data collector 11.
Detection light incident system includes probe source 19 and incident monochromator 8-1, and incident monochromator 8-1 is along probe source 19
Optical path direction setting, Single wavelength or full spectrum output for probe source 19.
Incident monochromator monochromator 8-1 can export the Single wavelength in probe source, can also export its full spectrum, fluorescence list
Color instrument 8-2 can export the Single wavelength of fluorescence, can also export its full spectrum.Incident monochromator monochromator 8-1 and fluorescence monochromator
8-2 can also carry out length scanning with certain rate, by adjusting slit width, can export different spectral bandwidths.Enter
The long axis that the detection light that monochromator 8-1 comes out passes through sample cell 6 is penetrated, along mixed liquor flow direction, while absorbing light intensity detection
Device 9-1 is also in the same direction.
The flow cell for reaction solution circulation is equipped in sample cell 6, electrochemical meter 10-1 includes being set to flow cell
The electrode of internal two sides and the first electrode data line f1 being connect respectively with two electrodes and second electrode data line f2.
As Figure 2-3, sample cell 6 uses four sides light-transmitting materials, and if light transmission seals quartz plate, four sides may be implemented thoroughly
Light, while guaranteeing the sealing of sample cell 6.The horizontal direction both ends of flow cell in sample cell 6 are respectively to detect light incident surface b1
With detection light-emitting face b2, the front and back side of flow cell is respectively front side fluorescence detection face c1 and rear side fluorescence detection face c2.With
The vertical vertical direction in reaction solution flow direction has two panels inert electrode, i.e. upper surface electrode d1 and lower surface electrode d2, can be with
The variation of electrochemical parameter in monitoring reaction course reaction solution, first electrode data line f1 and second electrode data line f2 can be used
In the control and signal acquisition of electrode.The two sides of flow cell is equipped with electrode slice, while lower cuvette volume can be into one
Step improves temporal resolution.
In the embodiment of the present invention, the electricity of the inertia material such as platinum, silver, palladium or graphite is installed in flow cell upper and lower surface
Pole piece, electrode surface form micro-structure by the surface preparations such as plating and deposition.Electrode slice is embedded in the interior table of sample cell 6
Face, and its upper surface is made to flush and seal with sample cell 6.The transmission region of sample cell 6 is planar structure, and non-transparent region passes through
Surface melanism inhibits stray light, improves spectral resolution；It is chamfering structure between the inner wall of wide-angle, rapids can be efficiently reduced
The generation of stream.
Chemical liquids sampling system includes two groups or more single-pipeline liquid-supplying system；When with two groups of single-pipeline feed flows
When system, two groups of single-pipeline liquid-supplying system parallel connections connect for the entry to mixed solution a1 after mixed liquor feed flow pipeline all the way with sample cell 6
It is logical；When with single-pipeline liquid-supplying system more than two, wherein two groups of single-pipeline liquid-supplying system parallel connections are the confession of first via mixed liquor
Liquid pipe line, it is the second road mixed liquor liquid supply pipe that first via mixed liquor feed flow pipeline is in parallel with third group single-pipeline liquid-supplying system again
Line, and so on, the mixed liquor of last mixed liquor feed flow pipeline and sample cell 6 all the way after multiple single-pipeline liquid-supplying systems are in parallel
Entrance a1 connection.
Single-pipeline liquid-supplying system includes liquid line, sampling injector, liquid storage syringe, two-position three-way valve and infuses with sample introduction
The sample introduction servo motor of emitter connection, wherein sampling injector, liquid storage syringe and liquid line are connect with two-position three-way valve,
For driving, sampling injector carries out imbibition to sample introduction servo motor or drain, sample introduction servo motor pass through servo control system
13 controls.
In the embodiment of the present invention, chemical liquids sampling system includes three groups of single-pipeline liquid-supplying systems, and first group of single-pipeline supplies
Liquid system includes the first sample introduction servo motor 1-1, the first sampling injector 2-1, the first liquid storage syringe 3-1, the first two three
Port valve 4-1 and liquid line 7-1, the first sample introduction servo motor 1-1 are connect with the first sampling injector 2-1, the injection of the first sample introduction
Device 2-1, the first liquid storage syringe 3-1 and liquid line 7-1 are connect with the first two-position three-way valve 4-1, liquid line 7-1 and
Two groups of single-pipeline liquid-supplying systems are connect with the first mixer 5-1, and the first mixer 5-1 is connect with premixing pipeline 7-3, are pre-mixed
Pipeline 7-3 and third road liquid feeding pipeline are connect with the second mixer 5-2, and the second mixer 5-2 passes through liquid line 7-5 and sample
The entry to mixed solution a1 in product pond 6 is connected to.
Reaction solution after second mixer 5-2 mixing injects sample by liquid line 7-5 at entry to mixed solution a1
In pond 6, the detection light after incidence monochromator 8-1 light splitting is shining into reaction solution by detecting light incident surface b1 later, is inhaled
The measurement of ultraviolet-visible absorption spectroscopy can be carried out in detection light-emitting face b2 by receiving light intensity detector 9-1.Reaction solution issues glimmering
Light can pass through front side fluorescence detection face c1 or rear side fluorescence detection face c2 along perpendicular to reaction solution flow direction, by fluorescence list
Color instrument 8-2 light splitting and then the measurement that fluorescence emission spectrum is carried out by fluorescent intensity detector 9-2.
First two-position three-way valve 4-1 to third two-position three-way valve 4-3 can control reaction solution from liquid storage syringe flow into
Sample syringe, or sample cell 6 is flowed into from sampling injector.
First sampling injector 2-1 and the first built-in buffer solution of liquid storage syringe 3-1, flushing, background for pipeline
The measurement of spectrum or electrochemistry spectrum and the mixed diluting of different proportion.
Waste liquid storage system includes waste liquid syringe 2-4, waste liquid servo motor 1-4, waste liquid bottle 3-4, the 4th two-bit triplet
Valve 4-4 and tapping line 7-6, wherein waste liquid syringe 2-4, waste liquid bottle 3-4 and tapping line 7-6 with the 4th two-position three-way valve
4-4 connection, tapping line 7-6 are connected to the mixture export a2 of sample cell 6；Waste liquid servo motor 1-4 and waste liquid syringe 2-4
Connection, for driving waste liquid syringe 2-4 imbibition or drain, waste liquid servo motor 1-4 is controlled by servo control system 13
System.4th two-position three-way valve 4-4 can control waste liquid and flow into waste liquid syringe 2-4 from sample cell 6, or from waste liquid syringe 2-
4 flow into waste liquid bottle 3-4.
Sampling injector and waste liquid syringe are inertia material, and internal diameter is uniform, can by the revolving speed of servo motor and
Rotation time accurately controls the flow velocity, mixed volume and mixed proportion of reaction solution.Waste liquid servo motor 1-4 cooperates with sample introduction servo
Motor work, while guaranteeing faster sample introduction speed, it is also ensured that mixed liquor flow stability, while reducing liquid line
The generation of over-voltage effect in line.
Liquid line 7-1,7-2,7-4,7-5 and tapping line 7-6 are as short as possible under the premise of assurance function, premixing
Pipeline 7-3 can adjust its volume according to different requirement of experiment, can be used for the activation of enzyme.Sample introduction servo motor and waste liquid servo
The time that motor stops working is relative to absorption light intensity detector 9-1, fluorescent intensity detector 9-2 and electrochemical meter 10-1
Time of measuring have delay, can guarantee the integrality of signal acquisition in this way.By adding polarizing film, Ke Yishi in light path system
The measurement of existing absorbance, circular dichroism, fluorescent emission and fluorescence polarization；PH value, electricity may be implemented in electrochemical meter 10-1
The measurement of conductance and ionic strength.
As shown in figure 4, the liquid feeding pipeline of chemical liquids sampling system is placed in pipeline thermostat 15, sample cell 6 and pipeline
The temperature of thermostat 15 is controlled by temperature controller 14.The temperature of pipeline thermostat 15 is controlled by liquid circulation, sample
The temperature in product pond 6 is controlled by semiconductor chilling plate 16.Sample cell temperature is respectively equipped in sample cell 6 and pipeline thermostat 15
Spend sensor 17 and pipeline thermostat temperature sensor 18.
Measurement process of the invention is:
Firstly, the solution of three liquid storage syringes is injected into sampling injector simultaneously flushing pipeline, switch two later
Triple valve is connected to sampling injector with sample cell 6.The temperature of pipeline thermostat and sample cell semiconductor chilling plate is set,
Incident monochromator 8-1 and fluorescence monochromator 8-2 set wavelength.Pipeline and sampling injector etc. are pre-mixed according to using in equipment
The type of accessory sets the sequence of sample introduction, sample introduction delay and sample volume.Servo motor is according to according to the work set later
Program sample introduction, and quickly stop, while absorbing light intensity detector 9-1, fluorescent intensity detector 9-2 and electrochemical meter 10-1
It starts to work, measures background spectra.Servo motor works on later, is repeatedly rinsing pipeline and sample cell and then secondary is pressing
According to the program sample introduction set, and quickly stop, while absorbing light intensity detector 9-1, fluorescent intensity detector 9-2 and electrochemistry
Measuring instrument 10-1 start to work, measurement experiment spectrum, by data processing software carry out data processing, can obtain synchronous spectrum and
Electrochemistry spectrum, as shown in Figure 5.It can be seen that the progress with reaction, the reduction of reaction substrate concentration to be measured, absorption spectrum and hair
It penetrates the intensity of spectrum and is gradually reduced, and thus product is a kind of acidic materials, the pH value of mixed liquor gradually decreases.
Device in the present invention can in 200nm-800nm wavelength, milli in micro- time scale to hour, pass through servo
The fast sample of motor and stopping, measurement solution mixing after kinetics process, by UV absorption, fluorescence spectrum and
Reaction rate constant is calculated in the parameter that electrochemistry spectrum synchro measure obtains, thus the centre inferring reaction mechanism and being related to
Body.
Device in the present invention can be directly used for the measurement of stable state spectrum and electrochemistry spectrum, the independent control of temperature control system
The temperature of sample cell and pipeline thermostat, so as to realize the accurate control of experiment condition.
As stated above, the device of the invention may be implemented milli microsecond differentiate under, liquid phase reactor chemical kinetic systems and electrochemistry
The synchro measure of spectrum, wherein probe source 19 and light path system, incident monochromator 8-1, sample cell 6, fluorescence monochromator 8-2 and glimmering
The 9-2 connection of light light intensity detector；Probe source 19 and light path system, incident monochromator 8-1, sample cell 6 and absorption light intensity detection
Device 9-1 connection；Computer and sequential control system respectively with absorb light intensity detector 9-1, fluorescent intensity detector 9-2, electrification
Measuring instrument 10-1, data collector 11, incident monochromator 8-1, fluorescence monochromator 8-2, servo control system 13 is learned to connect.
Its measurement method are as follows: the solution in liquid storage syringe is injected into sampling injector, the output wavelength of incident monochromator 8-1 is set
Good, spectrum and the electrochemistry spectrum of first synchro measure buffer solution are used as background signal, later according to the program set, injection to
Test sample, while the accurate control time carries out the synchronous acquisition of spectral signal and electrochemistry spectrum signal.Pass through control sample introduction servo electricity
The collaborative work of machine and waste liquid servo motor realizes fast sample and inhibits the generation of over-voltage and turbulent phenomenon.The present apparatus is
The device that Hao microsecond differentiates liquid phase reactor chemical kinetic systems and electrochemistry spectrum synchro measure may be implemented at present, compared to more existing
Commercialization instrument can realize the flowing of mixed liquor and precisely control, and can obtain in one-shot measurement more fully crucial
Kinetic parameter has bigger universality to different complex system kineticses.
A kind of method of synchro measure liquid phase reactor chemical kinetic systems and electrochemistry spectrum, method the following steps are included:
1) measure background spectra: chemical liquids sampling system and waste liquid storage system cooperate, and buffer solution is injected sample
In pond 6, in the detection light to sample cell 6 of detection light incident system transmitting setting wavelength, surveyed by liquid phase reactor chemical kinetic systems
The spectrum and electrochemistry of amount system and electrochemical meter 10-1 synchro measure buffer solution spectrum are used as background signal；
2) measurement experiment is composed: chemical liquids sampling system and waste liquid storage system cooperate, and will inject sample cell 6 to test sample
It is interior, spectral signal and electrochemistry spectrum signal are carried out by liquid phase reactor chemical kinetic systems measuring system and electrochemical meter 10-1
Synchronous acquisition；
3) data processing is carried out by computer and sequential control system 12, synchronous spectrum and electrochemistry spectrogram can be obtained.
Liquid phase reactor chemical kinetic systems measuring system includes the absorption light intensity detector 9-1 along the setting of reaction solution flow direction
With along the fluorescent intensity detector 9-2 perpendicular to the setting of reaction solution flow direction, light intensity detector 9-1 measurement reaction solution is absorbed
Absorption spectrum, fluorescent intensity detector 9-2 measurement reaction solution fluorescence spectrum, chemical liquids sampling system and waste liquid storage system are stopped
The time only to work is relative to the measurement for absorbing light intensity detector 9-1, fluorescent intensity detector 9-2 and electrochemical meter 10-1
There is delay in time, can guarantee the integrality of signal acquisition in this way.
The present invention by the sample cell of autonomous Design, absorption spectrum may be implemented, fluorescence spectrum composed with electrochemistry it is synchronous
Measurement has more wide application prospect, such as the change of light-catalyzed reaction intermediate ion concentration or pH value；Sample introduction servo motor and
For waste liquid servo motor by cooperating, over-voltage and turbulence effect is can be effectively prevented in the sample cell for our autonomous Designs of arranging in pairs or groups
Generation, so as to realize that more quick solution sample introduction and sample introduction stop operation, to measure more accurate dynamics
Parameter；The pipeline thermostat temperature and sample cell temperature of independent control, on the one hand ensure that the storage temperature of reaction solution and chemistry are anti-
The temperature independent control that should occur, another aspect semiconductor chilling plate can more quickly change the temperature of reaction solution in sample cell
Degree, may be applicable in the reaction of temperature jump, the condition that more really simulation biochemical reaction carries out.
Mode the above is only the implementation of the present invention is not intended to limit the scope of the present invention.It is all in the present invention
Spirit and principle within any modification, equivalent replacement, improvement, extension etc., be all contained in protection scope of the present invention
It is interior.
Claims (10)
1. a kind of liquid phase reactor chemical kinetic systems and electrochemistry compose synchronous measuring apparatus, which is characterized in that timely including computer
Sequence control system (12), detection light incident system, sample cell (6), chemical liquids sampling system, waste liquid storage system, liquid phase reactor
Chemical kinetic systems measuring system, electrochemical meter (10-1) and data collector (11), wherein
The sample cell (6) is used for the storage and circulation of reaction solution, the chemical liquids sampling system and the waste liquid storage system
It is connected to respectively with the entry to mixed solution (a1) of the sample cell (6) and mixture export (a2)；
The detection light incident system is set to the outside of the sample cell (6), for along the sample cell (6) interior reaction solution
Flow direction emission detection light；
The liquid phase reactor chemical kinetic systems measuring system is set to the outside of the sample cell (6), for measuring reaction solution
Absorption and fluorescence spectrum；
The electrochemical meter (10-1) is set in the sample cell (6), and the electrochemistry for measuring reaction solution is composed；
The data collector (11) and the liquid phase reactor chemical kinetic systems measuring system and electrochemical meter (10-1) are even
It connects, for acquiring spectral signal and electrochemistry spectrum signal；
The detection light incident system, chemical liquids sampling system, waste liquid storage system, liquid phase reactor chemical kinetic systems measurement system
System, electrochemical meter (10-1) and data collector (11) are connect with computer and sequential control system (12).
2. liquid phase reactor chemical kinetic systems according to claim 1 and electrochemistry compose synchronous measuring apparatus, which is characterized in that
The liquid phase reactor chemical kinetic systems measuring system includes absorbing light intensity detector (9-1), fluorescence monochromator (8-2) and fluorescence light
Strong detector (9-2) is oppositely disposed with the detection light incident system in the sample wherein absorbing light intensity detector (9-1)
The opposite sides in pond (6), the absorption spectrum for absorbing light intensity detector (9-1) and being used to measure reaction solution, the fluorescence are monochromatic
Instrument (8-2) and fluorescent intensity detector (9-2) are set gradually along the flow direction perpendicular to the sample cell (6) interior reaction solution,
The fluorescence monochromator (8-2) is used to export the Single wavelength of fluorescence or is composed entirely to fluorescent intensity detector (9-2), the fluorescence
Light intensity detector (9-2) is used to measure the fluorescence spectrum of reaction solution, the fluorescent intensity detector (9-2) and absorption light intensity detection
Device (9-1) is connect with the data collector (11).
3. liquid phase reactor chemical kinetic systems according to claim 1 and electrochemistry compose synchronous measuring apparatus, which is characterized in that
The detection light incident system includes probe source (19) and incident monochromator (8-1), and the incidence monochromator (8-1) is along described
The optical path direction of probe source (19) is arranged, for export the probe source (19) Single wavelength or full spectrum.
4. liquid phase reactor chemical kinetic systems according to claim 1 and electrochemistry compose synchronous measuring apparatus, which is characterized in that
The flow cell for reaction solution circulation is equipped in the sample cell (6), the electrochemical meter (10-1) includes being set to institute
State the electrode of two sides and the first electrode data line (f1) and second electrode data that connect respectively with two electrodes inside flow cell
Line (f2).
5. liquid phase reactor chemical kinetic systems according to claim 1 and electrochemistry compose synchronous measuring apparatus, which is characterized in that
The chemical liquids sampling system includes two groups or more single-pipeline liquid-supplying system；
When having two groups of single-pipeline liquid-supplying systems, two groups of single-pipeline liquid-supplying system parallel connections be all the way after mixed liquor feed flow pipeline with
The entry to mixed solution (a1) of the sample cell (6) is connected to；
When with single-pipeline liquid-supplying system more than two, wherein two groups of single-pipeline liquid-supplying system parallel connections are the confession of first via mixed liquor
Liquid pipe line, it is the second road mixed liquor liquid supply pipe that first via mixed liquor feed flow pipeline is in parallel with third group single-pipeline liquid-supplying system again
Line, and so on, last mixed liquor feed flow pipeline all the way and the sample cell (6) after multiple single-pipeline liquid-supplying systems are in parallel
Entry to mixed solution (a1) connection.
6. liquid phase reactor chemical kinetic systems according to claim 5 and electrochemistry compose synchronous measuring apparatus, which is characterized in that
The single-pipeline liquid-supplying system includes liquid line, sampling injector, liquid storage syringe, two-position three-way valve and and sampling injector
The sample introduction servo motor of connection, wherein sampling injector, liquid storage syringe and liquid line are connect with two-position three-way valve, described
For driving, the sampling injector carries out imbibition to sample introduction servo motor or drain, the sample introduction servo motor pass through servo motor
Control system (13) control.
7. liquid phase reactor chemical kinetic systems according to claim 1 and electrochemistry compose synchronous measuring apparatus, which is characterized in that
The waste liquid storage system includes waste liquid syringe (2-4), waste liquid servo motor (1-4), waste liquid bottle (3-4) and tapping line
(7-6), wherein waste liquid syringe (2-4), waste liquid bottle (3-4) and tapping line (7-6) are connect with two-position three-way valve, the row
Liquid pipe line (7-6) is connected to the mixture export (a2) of the sample cell (6)；The waste liquid servo motor (1-4) and waste liquid are infused
Emitter (2-4) connection, for driving waste liquid syringe (2-4) imbibition or drain, the waste liquid servo motor (1-4) passes through
Servo control system (13) control.
8. liquid phase reactor chemical kinetic systems according to claim 1 and electrochemistry compose synchronous measuring apparatus, which is characterized in that
The liquid feeding pipeline of the chemical liquids sampling system is placed in pipeline thermostat (15), the sample cell (6) and pipeline thermostat
(15) temperature is controlled by temperature controller (14).
9. a kind of compose synchronous measuring apparatus using the described in any item liquid phase reactor chemical kinetic systems of claim 1-8 and electrochemistry
Measurement method, which is characterized in that the described method comprises the following steps:
1) measure background spectra: the chemical liquids sampling system and waste liquid storage system cooperate, and buffer solution is injected sample
In pond (6), in detection light to the sample cell (6) of detection light incident system transmitting setting wavelength, pass through liquid phase reactor dynamics light
The spectrum and electrochemistry of spectral measurement system and electrochemical meter (10-1) synchro measure buffer solution spectrum are used as background signal；
2) measurement experiment is composed: the chemical liquids sampling system and waste liquid storage system cooperate, and will inject sample cell to test sample
(6) in, spectral signal and electrochemistry are carried out by liquid phase reactor chemical kinetic systems measuring system and electrochemical meter (10-1)
The synchronous acquisition of spectrum signal；
3) data processing is carried out by computer and sequential control system (12), synchronous spectrum and electrochemistry spectrum can be obtained.
10. according to the method described in claim 9, it is characterized in that, the liquid phase reactor chemical kinetic systems measuring system includes
Along the absorption light intensity detector (9-1) of reaction solution flow direction setting and along the fluorescence light perpendicular to the setting of reaction solution flow direction
Strong detector (9-2) absorbs the absorption spectrum of light intensity detector (9-1) measurement reaction solution, fluorescent intensity detector (9-2) measurement
The time of reaction solution fluorescence spectrum, the chemical liquids sampling system and the waste liquid storage system to stop working is relative to described
The time of measuring for absorbing light intensity detector (9-1), fluorescent intensity detector (9-2) and electrochemical meter (10-1) has delay.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112930477A (en) * | 2019-01-18 | 2021-06-08 | 国立研究开发法人产业技术综合研究所 | Inductively coupled plasma analysis system and inductively coupled plasma analysis method |
| CN114113003A (en) * | 2020-08-28 | 2022-03-01 | 中国科学院大连化学物理研究所 | In-situ monitoring chemical reaction double-cascade buckle stray light emission spectrum measuring device |
| CN116773472A (en) * | 2023-06-21 | 2023-09-19 | 中国科学技术大学 | Space-time resolution device combining spectrum and imaging |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996014569A2 (en) * | 1994-11-05 | 1996-05-17 | Cognitive Solutions Ltd. | Detector for chemical analysis |
| CN1424579A (en) * | 2003-01-21 | 2003-06-18 | 南开大学 | Online interface for capillary calaphorestic hydride generated atomic spectrofluorimetry |
| CN101672788A (en) * | 2009-09-16 | 2010-03-17 | 广西师范大学 | Method for measuring materials inside human single blood erythrocyte by mocro-fluidic chip chemiluminescence |
| CN104569090A (en) * | 2014-12-26 | 2015-04-29 | 浙江清华长三角研究院萧山生物工程中心 | Electrochemical impedance and ultraviolet visible absorption spectrum combined analysis device and method |
| CN106501334A (en) * | 2016-12-08 | 2017-03-15 | 中国科学技术大学 | For Ultraviolet visible spectroelectrochemistry and fluorescence spectrum electrochemical investigating pond |
-
2018
- 2018-10-19 CN CN201811218459.3A patent/CN109142253B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996014569A2 (en) * | 1994-11-05 | 1996-05-17 | Cognitive Solutions Ltd. | Detector for chemical analysis |
| CN1424579A (en) * | 2003-01-21 | 2003-06-18 | 南开大学 | Online interface for capillary calaphorestic hydride generated atomic spectrofluorimetry |
| CN101672788A (en) * | 2009-09-16 | 2010-03-17 | 广西师范大学 | Method for measuring materials inside human single blood erythrocyte by mocro-fluidic chip chemiluminescence |
| CN104569090A (en) * | 2014-12-26 | 2015-04-29 | 浙江清华长三角研究院萧山生物工程中心 | Electrochemical impedance and ultraviolet visible absorption spectrum combined analysis device and method |
| CN106501334A (en) * | 2016-12-08 | 2017-03-15 | 中国科学技术大学 | For Ultraviolet visible spectroelectrochemistry and fluorescence spectrum electrochemical investigating pond |
Non-Patent Citations (3)
| Title |
|---|
| [德]施威特 著: "《图释分析化学》", 31 July 2002, 辽宁师范大学出版社 * |
| 刘立华 主编: "《制药工程专业实验》", 31 July 2018, 中国矿业大学出版社 * |
| 郑荣梁: "《生物自由基》", 31 October 1992 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112930477A (en) * | 2019-01-18 | 2021-06-08 | 国立研究开发法人产业技术综合研究所 | Inductively coupled plasma analysis system and inductively coupled plasma analysis method |
| US11538672B2 (en) * | 2019-01-18 | 2022-12-27 | National Institute Of Advanced Industrial Science And Technology | Inductively coupled plasma spectrometric system and inductively coupled plasma spectrometric method |
| CN114113003A (en) * | 2020-08-28 | 2022-03-01 | 中国科学院大连化学物理研究所 | In-situ monitoring chemical reaction double-cascade buckle stray light emission spectrum measuring device |
| CN114113003B (en) * | 2020-08-28 | 2024-05-07 | 中国科学院大连化学物理研究所 | In-situ monitoring chemistry chemical reaction double cascade button stray light emission spectrum measuring device |
| CN116773472A (en) * | 2023-06-21 | 2023-09-19 | 中国科学技术大学 | Space-time resolution device combining spectrum and imaging |
| CN116773472B (en) * | 2023-06-21 | 2024-03-29 | 中国科学技术大学 | Space-time resolution device combining spectrum and imaging |
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