CN106950250A - The thermal power measurement device of function is measured with visible ultraviolet spectra - Google Patents
The thermal power measurement device of function is measured with visible ultraviolet spectra Download PDFInfo
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- CN106950250A CN106950250A CN201710311093.3A CN201710311093A CN106950250A CN 106950250 A CN106950250 A CN 106950250A CN 201710311093 A CN201710311093 A CN 201710311093A CN 106950250 A CN106950250 A CN 106950250A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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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
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The present invention relates to a kind of thermal power measurement device that function is measured with visible ultraviolet spectra, including between thermal measurement system, spectral measurement system, acquisition and control system and constant temperature and humidity, thermal measurement system is used for the thermal power for measuring solution reaction system；Spectral measurement system is used for the visible ultraviolet spectra for measuring solution；Acquisition and control system includes being provided with calorimetric module, spectroscopic module and calorimetric spectrum combination module in data acquisition device, computer and nanovolt meter, computer；Data acquisition device is used to gather the constant temperature bath temperature of thermal measurement system and the electric current and voltage signal of programme-controlled dc power and be sent to calorimetric module, nanovolt meter is used to gather the heat flow signal of solution reaction system and sends it to calorimetric module, and calorimetric module is used for the demarcation and thermal power measurement of thermal measurement system；Spectroscopic module is used to gather spectrometer signal and carries out handling the spectral signal for realizing solution measurement；Calorimetric spectrum combination module is used for the measurement control for realizing thermal power and spectral signal.
Description
Technical field
The present invention relates to a kind of thermal power measurement device, especially with regard to one kind there is Visible imaging simulation to measure function
Thermal power measurement device.
Background technology
Thermal power measurement device (i.e. calorimeter) is widely used in scientific domain and the oil such as physics, chemistry and biology
The technical fields such as work, secondary cell, food processing, pharmacy.Wherein, isothermal titration calorimeter be particularly suitable for use in biosystem and point
Weak interaction research between son.Due to the complexity of such system, it can typically be aided with spectral measurement to obtain microscopic information.Isothermal
Titrating calorimetric can be with multiple spot Continuous Titration, the characteristics of being scanned with concentration.And spectrum etc. is used for the instrument of Study on Microstructure at present
Device does not have this scan function in design, can only pointwise test respectively.So, in face of calorimetric curve complicated and changeable with
And the limited spectral result that can not continuously measure, usually make one to determine the interval corresponding structure of different calorimetric curvilinear motions and
Phase.For large biological molecule and molecular self-assembly, the conversion of interaction, structure and phase has very
Strong dynamics dependence, the temperature even fine difference such as agitating mode, mixing speed and time this may result in different knots
Structure.This allow for carrying out titration calorimetric respectively and spectral measurement be often difficult to be interacted it is strict right between microstructure
It should be related to.
Once someone is put into optical fiber probe the change of direct measurement solution turbidity in the reaction tank of titration calorimeter in the world
(P.Johansson, I.Wadso, Thermochimica Acta 1999,342,19), but its optical measurement section have it is bright
Aobvious limitation, is that can not provide detailed spectral information first, next to that optical fiber probe is immersed directly in solution, structure is multiple
It is miscellaneous, limit it and use.Hereafter the energy of solution system and the synchro measure of microstructure can be realized without instrument again.
The content of the invention
Regarding to the issue above, present invention offer is a kind of can realize that the energy of solution system is synchronous with microstructure simultaneously
The instrument of measurement, i.e., measure the thermal power measurement device of function with Visible imaging simulation.
To achieve the above object, the present invention takes following technical scheme：It is a kind of to measure function with Visible imaging simulation
Thermal power measurement device, it is characterised in that the thermal power measurement device includes thermal measurement system, spectral measurement system, data and adopted
Between collection and control system and constant temperature and humidity, the thermal measurement system, spectral measurement system and acquisition and control system are put
Put in the constant temperature and humidity；The thermal measurement system is used for the thermal power for measuring solution reaction system；The spectral measurement
System is used for the Visible imaging simulation for measuring solution, and the spectral measurement system includes light source, and the light that the light source is sent is through Y
Type bifurcation fiber is divided into two-way light, and two-way light enters the solution reaction system and bottom by fibre optic attenuator and optical fiber respectively
Liquid, the light of outgoing enters spectrometer through fiber coupling lens and optical fiber respectively after the solution reaction system and bottom liquid；It is described
Acquisition and control system includes data acquisition device, computer and nanovolt meter, be provided with the computer calorimetric module,
Spectroscopic module and calorimetric-spectrum combination module；The data acquisition device is used for the constant temperature bath temperature for gathering the thermal measurement system
The electric current and voltage signal of degree and programme-controlled dc power are simultaneously sent to the calorimetric module, and the nanovolt meter is used to gather described molten
The heat flow signal of liquid reaction system simultaneously sends it to the calorimetric module, and the calorimetric module is used for the thermal measurement system
Demarcation and thermal power measurement；The spectroscopic module is used to gather the spectrometer signal and carry out after the solution spectrum signal
Processing；The calorimetric-spectrum combination module is used for the measurement control for realizing thermal power and spectral signal.
Further, the thermal measurement system includes constant temperature bath, heat sink, calorimetric pond, reaction tank and hot calibration system, the perseverance
Place described heat sink in warm bath, the heat sink interior placement calorimetric pond, the calorimetric pond is included greatly using the design of Shuangzi pond
Small and completely identical in structure sample cell and reference cell, the sample cell and reference cell include heat-conducting block, temperature difference heat pile and
The reaction tank for holding the solution reaction system or bottom liquid is placed in reaction tank, each heat-conducting block, it is each described
Heat-conducting block is provided with the optical measurement hole for placing the fiber coupling lens, and the hot calibration system includes program control direct current
Power supply and the thermal resistance being fixed in the heat-conducting block being attached thereto, the programme-controlled dc power heat institute using different electric currents
Thermal resistance is stated so that the temperature difference heat pile has different output voltage signals, the sample cell in the case of different input thermal powers
With the temperature difference heat pile output end reversal connection of reference cell, i.e., described sample cell thermoelectric pile output head anode connects the reference cell thermoelectricity
Heap output head anode, the external nanovolt meter of temperature difference heat pile negative pole of output end is used as output signal described in two.
Further, temperature control is required between the constant temperature and humidity at 20 to 25 DEG C, temperature-controlled precision ± 0.5 DEG C, relative humidity (45~
70) %RH.
Further, the thermal measurement system uses isothermal titration formula calorimetry.
Further, each reaction tank uses quartz glass tube.
Further, the constant temperature bath requires temperature control between 15 to 60 DEG C, and temperature-controlled precision is ± 0.0001 DEG C, the constant temperature bath
Using water-bath or oil bath.
Further, each heat-conducting block is made using highly heat-conductive material.
Further, the light source adds deuterium lamp using Halogen lamp LED.
Further, after spectral measurement terminates by the programme-controlled dc power the calorimetric pond the temperature difference heat pile
Upper application electric current directly cools down reaction tank and reference cell makes it be rapidly achieved thermal balance, realizes quick measurement.
The present invention is due to taking above technical scheme, and it has advantages below：1st, light-path is placed in reaction tank by the present invention
Outside, it is to avoid the reaction system that reaction tank built-in fiber probe is caused is complicated, operate more simple and efficient.2nd, the present invention is used
Sample cell and reference cell carry out thermal measurement and spectral measurement simultaneously, while realizing double pond thermal measurements and two-way photo measure, offset
The heat produced in spectral measurement does not interfere with each other two kinds of measurements, improves flash ranging amount efficiency.3rd, the present invention is imitated by peltier
It should actively cool and further speed up thermal balance, so as to reduce influence of the photo measure to thermal measurement, improve measurement efficiency.To sum up institute
State, the present invention can both measure thermal power and spectrum simultaneously, also can independent measurement thermal power and spectrum, can be widely applied to biological big
The research of weak interaction and other solution reaction systems and application field between molecule and molecular self-assembling equimolecular.
Brief description of the drawings
Fig. 1 is the structural representation of thermal power measurement device of the present invention；
Fig. 2 is the structural representation of spectral measurement system of the present invention；
Fig. 3 is the structural representation of the heat-conducting block of the present invention；
Fig. 4 is that lauryl sodium sulfate (SDS) is instilled in bovine serum albumin (BSA) course of reaction in the embodiment of the present invention
Heat and ultraviolet spectra measurement result, wherein, figure (a) is thermal measurement result in course of reaction, and figure (b) is ultraviolet light in course of reaction
Spectrometry result.
Embodiment
Come to carry out the present invention detailed description below in conjunction with accompanying drawing.It should be appreciated, however, that accompanying drawing has been provided only more
Understand the present invention well, they should not be interpreted as limitation of the present invention.
The solution reaction system of the present invention includes solution and bottom liquid, in sample cell and the reaction tank of reference cell before general experiment
Inside place bottom liquid (such as the BSA in specific embodiment), the bottom liquid in the reaction tank of reference cell is constant, be only used as thermal measurement and
The reference of photo measure；To be instilled in the reaction tank of sample cell in solution (such as the SDS in embodiment), the reaction tank of sample cell
Bottom liquid reacts with instilling solution while release heat, spectrum also respective change.
As shown in Figures 1 to 3, the thermal power measurement device with Visible imaging simulation measurement function that the present invention is provided, bag
Include 4 between thermal measurement system 1, spectral measurement system 2, acquisition and control system 3 and constant temperature and humidity；Wherein, thermal measurement system
1st, spectral measurement system 2 and acquisition and control system 3 are both placed in 4 between constant temperature and humidity.
The thermal measurement system 1 of the present invention includes constant temperature bath 11, heat sink 12, calorimetric pond and hot calibration system.In constant temperature bath 11
Heat sink 12 are placed further to improve temperature stability.Calorimetric pond is placed in heat sink 12, calorimetric pond is measured using the design of Shuangzi pond
Hot pond includes a sample cell 13 and a reference cell 14, and sample cell 13 and the size of reference cell 14 are identical with structure, and sample
Pond 13 and reference cell 14 are symmetrically placed to ensure that thermal environment is identical in heat sink 12.Sample cell 13 and reference cell 14 are led including one
Hot block 141, a temperature difference heat pile and a reaction tank.Each center of heat-conducting block 141 place for hold solution reaction system or
Two optical measurement holes 142 are provided with the reaction tank of bottom liquid, each heat-conducting block 141.Hot calibration system, which is used to set up, to be exported
Corresponding relation (be usually linear relationship) between voltage signal and thermal power, it includes programme-controlled dc power 15 and is attached thereto
The thermal resistance being fixed in heat-conducting block 141, programme-controlled dc power 15 causes different input heat using different electric currents heating thermal resistance
Temperature difference heat pile has the temperature difference heat pile output end of different output voltage signals, sample cell 13 and reference cell 14 under power situation
The temperature difference heat pile output head anode of reversal connection, i.e. sample cell 13 connects the temperature difference heat pile output head anode of reference cell 14, two temperature
The external nanovolt meter of differential thermoelectric pile negative pole of output end can offset disturbing for heat sink temperature as whole calorimetric pond output signal, such a connection
The dynamic influence to temperature difference heat pile output signal.In addition, the present invention is also existed using peltier effect by programme-controlled dc power 15
Temperature difference heat pile, which applies electric current active cooling sample cell and reference cell, makes it be rapidly achieved thermal balance with heat sink, to eliminate ring as early as possible
Border and the heat affecting of optical signal.
The spectral measurement system 2 of the present invention is used to measure the solution reaction system and reference cell in sample cell 13 in reaction tank
In 14 in reaction tank bottom liquid Visible imaging simulation, and then can measure obtain solution Visible imaging simulation change.Spectrum
Measuring system 2 includes light source 21, Y shape bifurcation fiber 22, fibre optic attenuator 23, optical fiber 24, fiber coupling lens 25 and carried
The spectrometer 26 of grating.The light that light source 21 is sent is divided into two-way light by Y types bifurcation fiber 22, and two-way light is taken up in order of priority by light
Fine attenuator 23, optical fiber 24 and the fiber coupling lens 25 that are placed in optical measurement hole 142 enter (or the reference cell of sample cell 13
14) solution reaction system (or bottom liquid) in, the light of outgoing is again respectively through opposite optics after solution reaction system and bottom liquid
Fiber coupling lens 25 and optical fiber 24 in measured hole 142 enter spectrometer 26；The light source 21 of the present invention is arranged on outside reaction tank
Portion, while realizing double-optical path using sample cell 13 and reference cell 14；Fibre optic attenuator 23 makes two ways of optical signals intensity consistent,
That is regulation optical signal relative intensity makes thermal signal offset minimum, to eliminate as much as influence of the photo measure to thermal measurement.Two
Road spectral signal can simultaneously be measured by the different passages of same spectrometer, or be measured respectively with same spectrometer.
Acquisition and control system 3 includes data collecting card 31 or the digital multimeter blocked with scanning, the and of nanovolt meter 32
Calorimetric module, spectroscopic module and calorimetric-spectrum combination module are provided with computer, computer.Wherein, calorimetric module is used for
The demarcation of thermal measurement system 1 and thermal power measurement, data collecting card 31 or the digital multimeter with scanning card are used to gather constant temperature
Gathered data is simultaneously sent to calorimetric module by the electric current and voltage signal of bath temperature and programme-controlled dc power 15, and nanovolt meter is used to adopt
Collect the heat flow signal of temperature difference heat pile generation and send it to calorimetric module and be processed and displayed；Spectroscopic module is used to gather
The signal of spectrometer 26 simultaneously carries out the spectral signal measurement that Data Post realizes solution to be measured；Calorimetric-spectrum combination module is used
Controlled in the measurement for realizing thermal power and spectral signal, because spectral measurement optical signal can heat sample cell 13 and reference cell
14, severe jamming thermal measurement, so needing to be combined module control thermoelectricity of the programme-controlled dc power 15 to two ponds by calorimetric-spectrum
Heap, which applies electric current and cools down two reaction tanks, arrives design temperature, and next step thermal measurement and spectrum survey could be carried out after force revert thermal balance
Amount, this process, which needs to be combined module by calorimetric-spectrum to measure thermal signal and apply appropriate cooling electric current, to be completed.
In a preferred embodiment, 4 require temperature control in 20 to 25 DEG C, temperature-controlled precision ± 0.5 DEG C, phase between constant temperature and humidity
To humidity (45~70) %RH.
In a preferred embodiment, thermal measurement system 1 can use isothermal titration formula calorimetry, but be not limited to titration
Formula, can be selected according to practical application.
In a preferred embodiment, each reaction tank can use quartz glass tube.
In a preferred embodiment, constant temperature bath 11 requires temperature control between 15 to 60 DEG C, temperature-controlled precision ± 0.0001 DEG C,
Constant temperature bath 11 can be water-bath or oil bath.
In a preferred embodiment, heat-conducting block 141 can be made using highly heat-conductive materials such as aluminium alloy or copper.
In a preferred embodiment, temperature difference heat pile can be assembled using Commercial semiconductors electrothermal module, according to
Thermal measurement specific requirement selects different model, does not limit herein.
In a preferred embodiment, light source 21 can add deuterium lamp using Halogen lamp LED.
Below with lauryl sodium sulfate (SDS) and the thermal power and purple of the drop reaction process of bovine serum albumin (BSA)
External spectrum is measured as the use that embodiment illustrates the thermal power measurement device with Visible imaging simulation measurement function of the present invention
Process.
Measure the ultraviolet spectra of 0.6ml 5mg/ml BSA water solution systems first before drop reaction, then drip every time
Enter 10 microlitres of SDS, measurement titration heat, titration thermal measurement measures ultraviolet spectra, alternately thermal measurement and spectral measurement after terminating.
Totally 33 titration results and 34 UV adsorption results are respectively as shown in Fig. 4 (a) and (b) for the present embodiment, and top is bent in Fig. 4 (b)
Line sequence number 0 represents the spectral results before first time thermal measurement, from fig. 4, it can be seen that the present invention can measure the thermal signal of the system simultaneously
And spectral signal.
Above-described embodiment is merely to illustrate the present invention, wherein the structure of each part, connected mode and manufacture craft etc. are all
It can be varied from, every equivalents carried out on the basis of technical solution of the present invention and improvement should not be excluded
Outside protection scope of the present invention.
Claims (9)
1. a kind of thermal power measurement device that function is measured with Visible imaging simulation, it is characterised in that thermal power measurement dress
Put including between thermal measurement system, spectral measurement system, acquisition and control system and constant temperature and humidity, the thermal measurement system,
Spectral measurement system and acquisition and control system are both placed in the constant temperature and humidity；
The thermal measurement system is used for the thermal power for measuring solution reaction system；
The spectral measurement system is used for the Visible imaging simulation for measuring solution, and the spectral measurement system includes light source, described
The light that light source is sent is divided into two-way light through Y type bifurcation fibers, and two-way light is saturating by fibre optic attenuator, optical fiber and fiber coupling respectively
Mirror enters the solution reaction system and bottom liquid, and the light through the solution reaction system and bottom liquid outgoing is respectively through the optical fiber coupling
Close lens and optical fiber enters spectrometer；
The acquisition and control system includes being provided with data acquisition device, computer and nanovolt meter, the computer
Calorimetric module, spectroscopic module and calorimetric-spectrum combination module；The data acquisition device is used to gather the thermal measurement system
The electric current and voltage signal of constant temperature bath temperature and programme-controlled dc power are simultaneously sent to the calorimetric module, and the nanovolt meter is used to adopt
Collect the heat flow signal of the solution reaction system and send it to the calorimetric module, the calorimetric module is used for the heat and surveyed
The demarcation of amount system and thermal power measurement；The spectroscopic module is used to gather the spectrometer signal and carries out the solution spectrum
The post processing of signal；The calorimetric-spectrum combination module is used for the measurement control for realizing thermal power and spectral signal.
2. the thermal power measurement device of function is measured with Visible imaging simulation as claimed in claim 1, it is characterised in that
The thermal measurement system includes placing described in constant temperature bath, heat sink, calorimetric pond, reaction tank and hot calibration system, the constant temperature bath
It is heat sink, the heat sink interior placement calorimetric pond, the calorimetric pond includes size and the complete phase of structure using the design of Shuangzi pond
Same sample cell and reference cell, the sample cell and reference cell include heat-conducting block, temperature difference heat pile and reaction tank, each described
The reaction tank for holding the solution reaction system or bottom liquid is placed in heat-conducting block, each heat-conducting block is provided with use
In the optical measurement hole for placing the fiber coupling lens, the hot calibration system includes programme-controlled dc power and is attached thereto
The thermal resistance being fixed in the heat-conducting block, the programme-controlled dc power heats the thermal resistance using different electric currents and causes difference
The temperature difference heat pile has different output voltage signals, the temperature difference heat of the sample cell and reference cell in the case of input thermal power
Pile output end reversal connection, i.e., described sample cell thermoelectric pile output head anode connects the reference cell thermoelectric pile output head anode, two
The external nanovolt meter of temperature difference heat pile negative pole of output end is used as output signal.
3. the thermal power measurement device of function is measured with Visible imaging simulation as claimed in claim 1, it is characterised in that
Require temperature control in 20 to 25 DEG C, temperature-controlled precision ± 0.5 DEG C, relative humidity (45~70) %RH between the constant temperature and humidity.
4. the thermal power measurement device with Visible imaging simulation measurement function as described in any one of Claim 1-3, its
It is characterised by, the thermal measurement system uses isothermal titration formula calorimetry.
5. the thermal power measurement device of function is measured with Visible imaging simulation as claimed in claim 2, it is characterised in that
Each reaction tank uses quartz glass tube.
6. the thermal power measurement device of function is measured with Visible imaging simulation as claimed in claim 2, it is characterised in that
The constant temperature bath requires temperature control between 15 to 60 DEG C, and temperature-controlled precision is ± 0.0001 DEG C, and the constant temperature bath uses water-bath or oil bath.
7. the thermal power measurement device of function is measured with Visible imaging simulation as claimed in claim 2, it is characterised in that
Each heat-conducting block is made using highly heat-conductive material.
8. the thermal power measurement device with Visible imaging simulation measurement function as described in any one of Claim 1-3, its
It is characterised by, the light source adds deuterium lamp using Halogen lamp LED.
9. the thermal power measurement device with Visible imaging simulation measurement function as described in Claims 2 or 3 or 5 or 6 or 7,
Characterized in that, spectral measurement is applied after terminating by the programme-controlled dc power on the temperature difference heat pile in the calorimetric pond
Plus electric current directly cools down reaction tank and reference cell makes it be rapidly achieved thermal balance, realizes quick measurement.
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| CN107976467A (en) * | 2017-12-04 | 2018-05-01 | 中国科学院化学研究所 | There is the thermal power measurement device of raman spectroscopy measurement |
| CN108061726A (en) * | 2017-12-04 | 2018-05-22 | 中国科学院化学研究所 | There is the isotherm formula thermal power measurement device of fluorescence spectral measuring |
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| CN106950250B (en) | 2019-09-27 |
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