CN106950250B - Thermal power measurement device with Visible imaging simulation measurement function - Google Patents
Thermal power measurement device with Visible imaging simulation measurement function Download PDFInfo
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- 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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- 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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Abstract
The present invention relates to a kind of thermal power measurement devices with Visible imaging simulation measurement function, including between thermal measurement system, spectral measurement system, acquisition and control system and constant temperature and humidity, thermal measurement system is used to measure the thermal power of solution reaction system；Spectral measurement system is used to measure the Visible imaging simulation of solution；Acquisition and control system includes data acquisition device, computer and nanovolt meter, and calorimetric module, spectroscopic module and calorimetric-spectrum combination module are provided in computer；Data acquisition device is for acquiring the constant temperature bath temperature of thermal measurement system and the electric current and voltage signal of programme-controlled dc power and being sent to calorimetric module, nanovolt meter is used to acquire the heat flow signal of solution reaction system and sends it to calorimetric module, calibration and thermal power measurement of the calorimetric module for thermal measurement system；Spectroscopic module is used to acquire spectrometer signal and carries out the spectral signal measurement that solution is realized in processing；Calorimetric-spectrum combination module controls for realizing the measurement of thermal power and spectral signal.
Description
Technical field
The present invention relates to a kind of thermal power measurement devices, have the function of Visible imaging simulation measurement especially with regard to one kind
Thermal power measurement device.
Background technique
Thermal power measurement device (i.e. calorimeter) is widely used in the scientific domains such as physics, chemistry and biology and petroleum
The technical fields such as work, secondary cell, food processing, pharmacy.Wherein, isothermal titration calorimeter is particularly suitable for biosystem and divides
Weak interaction research between son.Due to the complexity of such system, it can generally be aided with spectral measurement to obtain microscopic information.Isothermal
Concentration scanning can be had the characteristics that with multiple spot Continuous Titration by titrating calorimetric.And spectrum etc. is used for the instrument of Study on Microstructure at present
Device does not have this scanning function in design, can only test respectively point by point.So in face of calorimetric curve complicated and changeable with
And the limited spectral that can not continuously measure as a result, usually make one can not determine the corresponding structure in different calorimetric curvilinear motions section and
Phase.For large biological molecule and molecular self-assembly, the conversion of interaction, structure and phase has very
Strong dynamics dependence, the fine differences such as temperature even 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 stringent right between microstructure
It should be related to.
Once someone is put into optical fiber probe the variation that solution turbidity is directly measured in the reaction tank of titration calorimeter in the world
(P.Johansson, I.Wadso, Thermochimica Acta 1999,342,19), but its optical measurement section is with bright
Aobvious limitation is that can not provide detailed spectral information first, and followed by optical fiber probe is immersed directly in solution, and structure is multiple
It is miscellaneous, limit its use.Hereafter the energy of solution system and the synchro measure of microstructure be can be realized without instrument again.
Summary of the invention
In view of the above-mentioned problems, to provide a kind of energy that can be achieved at the same time solution system synchronous with microstructure by the present invention
The instrument of measurement, the i.e. thermal power measurement device with Visible imaging simulation measurement function.
To achieve the above object, the present invention takes following technical scheme: a kind of with Visible imaging simulation measurement function
Thermal power measurement device, which is characterized in that the thermal power measurement device includes that thermal measurement system, spectral measurement system, data are 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
It sets in the constant temperature and humidity；The thermal measurement system is used to measure the thermal power of solution reaction system；The spectral measurement
System is used to measure the Visible imaging simulation of solution, and the spectral measurement system includes light source, and the light that the light source issues is through Y
Type bifurcation fiber is divided into two-way light, and two-way light passes through fibre optic attenuator respectively and optical fiber enters the solution reaction system and bottom
Liquid, the light being emitted after the solution reaction system and bottom liquid enter spectrometer through fiber coupling lens and optical fiber respectively；It is described
Acquisition and control system includes data acquisition device, computer and nanovolt meter, be provided in the computer calorimetric module,
Spectroscopic module and calorimetric-spectrum are combined module；The data acquisition device is used to acquire the constant temperature bath temperature of 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 described molten for acquiring
The heat flow signal of liquid reaction system simultaneously sends it to the calorimetric module, and the calorimetric module is for the thermal measurement system
Calibration and thermal power measurement；The spectroscopic module is for after acquiring the spectrometer signal and carrying out the solution spectrum signal
Processing；The calorimetric-spectrum combination module controls for realizing the measurement of 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
Placement is described heat sink in warm bath, and the heat sink interior placement calorimetric pond, the calorimetric pond is using the design of Shuangzi pond i.e. including greatly
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
Reaction tank places the reaction tank for holding the solution reaction system or bottom liquid in each heat-conducting block, 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-controlled 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
Stating thermal resistance makes the temperature difference heat pile in the case of different input thermal powers have different output voltage signals, the sample cell
It is reversely connected with the temperature difference heat pile output end of reference cell, i.e., the described sample cell thermoelectric pile output head anode connects the reference cell thermoelectricity
Heap output head anode, the two external nanovolt meters of temperature difference heat pile negative pole of output end are as output signal.
Further, require temperature control at 20 to 25 DEG C between the constant temperature and humidity, temperature-controlled precision ± 0.5 DEG C, relative humidity (45~
70) %RH.
Further, the thermal measurement system uses isothermal titration formula weight thermal method.
Further, each reaction tank is all made of 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 all made of highly heat-conductive material and is made.
Further, the light source adds deuterium lamp using halogen lamp.
Further, the temperature difference heat pile after spectral measurement by the programme-controlled dc power in the calorimetric pond
The directly cooling reaction tank of upper application electric current and reference cell enable it be rapidly achieved thermal balance, realize rapid survey.
The invention adopts the above technical scheme, which has the following advantages: 1, light-path is placed in reaction tank by the present invention
Outside, the complication of reaction system caused by reaction tank built-in fiber probe is avoided, it is quick that the operation is more convenient.2, the present invention uses
Sample cell and reference cell carry out thermal measurement and spectral measurement simultaneously, while realizing double pond thermal measurements and two-way light measurement, offset
The heat generated in spectral measurement does not interfere with each other two kinds of measurements, improves flash ranging amount efficiency.3, the present invention is imitated by peltier
It should actively cool down and further speed up thermal balance, to reduce influence of the light measurement to thermal measurement, improve measurement efficiency.To sum up institute
State, the present invention can both measure thermal power and spectrum simultaneously, can also independent measurement thermal power and spectrum, can be widely applied to biological big
The research and application field of the intermolecular weak interactions such as molecule and molecular self-assembling and other solution reaction systems.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of thermal power measurement device of the present invention；
Fig. 2 is the structural schematic diagram of spectral measurement system of the present invention；
Fig. 3 is the structural schematic diagram of heat-conducting block of the invention；
Fig. 4 is that lauryl sodium sulfate in the embodiment of the present invention (SDS) is instilled in bovine serum albumin (BSA) reaction process
Heat and ultraviolet spectra measurement result, wherein figure (a) be in reaction process thermal measurement as a result, scheme (b) be ultraviolet light in reaction process
Spectrometry result.
Specific embodiment
Come to carry out detailed description to the present invention below in conjunction with attached drawing.It should be appreciated, however, that attached drawing has been provided only more
Understand the present invention well, they should not be interpreted as limitation of the present invention.
Solution reaction system of the invention includes solution and bottom liquid, in the reaction tank of sample cell and reference cell before general experiment
Inside place bottom liquid (such as 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 light measurement；It to be instilled in the reaction tank of sample cell solution (such as SDS in embodiment), in the reaction tank of sample cell
It bottom liquid and instills solution and reacts and release heat simultaneously, spectrum also corresponding change.
As shown in Figures 1 to 3, the thermal power measurement device provided by the invention with Visible imaging simulation measurement function, packet
It includes 4 between thermal measurement system 1, spectral measurement system 2, acquisition and control system 3 and constant temperature and humidity；Wherein, thermal measurement system
1, spectral measurement system 2 and acquisition and control system 3 are both placed in 4 between constant temperature and humidity.
Thermal measurement system 1 of the 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 to further increase 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 pond 13 and a reference cell 14, and sample cell 13 is identical with structure with the size of reference cell 14, and sample
Pond 13 and reference cell 14 are symmetrically placed to guarantee that thermal environment is identical in heat sink 12.Sample cell 13 and reference cell 14 are led including one
Heat block 141, a temperature difference heat pile and a reaction tank.Each 141 center of heat-conducting block place for hold solution reaction system or
The reaction tank of bottom liquid, is respectively provided with that there are two optical measurement holes 142 on each heat-conducting block 141.Hot calibration system is for establishing output
Corresponding relationship (usually linear relationship) between voltage signal and thermal power comprising programme-controlled dc power 15 and be attached thereto
The thermal resistance being fixed in heat-conducting block 141, programme-controlled dc power 15 make different input heat using different electric currents heating thermal resistance
Temperature difference heat pile has different output voltage signals, the temperature difference heat pile output end of sample cell 13 and reference cell 14 under power situation
Reversal connection, i.e. the temperature difference heat pile output head anode of the temperature difference heat pile output head anode connection reference cell 14 of sample cell 13, two temperature
The external nanovolt meter of differential thermoelectric pile negative pole of output end can offset disturbing for heat sink temperature as entire calorimetric pond output signal, such connection
The dynamic influence to temperature difference heat pile output signal.In addition, the present invention also utilizes peltier effect to exist 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
The heat affecting of border and optical signal.
Spectral measurement system 2 of the 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 to obtain the Visible imaging simulation variation of solution.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 has
The spectrometer 26 of grating.The light that light source 21 issues is divided into two-way light by Y type bifurcation fiber 22, and two-way light, which is taken up in order of priority, passes through 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 being emitted after solution reaction system and bottom liquid is again respectively by opposite optics
Fiber coupling lens 25 and optical fiber 24 in measured hole 142 enter spectrometer 26；Light source 21 of the invention is arranged outside reaction tank
Portion, while double-optical path is realized using sample cell 13 and reference cell 14；Fibre optic attenuator 23 keeps two ways of optical signals intensity consistent,
Adjusting optical signal relative intensity makes thermal signal offset minimum, to eliminate as much as influence of the light measurement to thermal measurement.Two
Road spectral signal can be measured simultaneously by the different channels of same spectrometer, or be measured respectively with same spectrometer.
Acquisition and control system 3 includes data collecting card 31 or digital multimeter, 32 and of nanovolt meter with scanning card
Computer is provided with calorimetric module, spectroscopic module and calorimetric-spectrum combination module in computer.Wherein, calorimetric module is used for
The calibration of thermal measurement system 1 and thermal power measurement, data collecting card 31 or the digital multimeter with scanning card are for acquiring constant temperature
The electric current and voltage signal of bath temperature and programme-controlled dc power 15 simultaneously send calorimetric module for acquisition data, and nanovolt meter is for adopting
Collect the heat flow signal that temperature difference heat pile generates and send it to calorimetric module and is processed and displayed；Spectroscopic module is for acquiring
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
In the measurement control for realizing thermal power and spectral signal, since spectral measurement optical signal can heat sample cell 13 and reference cell
14, severe jamming thermal measurement controls thermoelectricity of the programme-controlled dc power 15 to two ponds so needing to be combined module by calorimetric-spectrum
Heap applies cooling two reaction tanks of electric current and arrives set temperature, just can be carried out next step thermal measurement and spectrum survey after force revert thermal balance
Amount, this process need to be combined module by calorimetric-spectrum and measure thermal signal and apply cooling electric current appropriate to complete.
In a preferred embodiment, 4 require temperature control at 20 to 25 DEG C between constant temperature and humidity, temperature-controlled precision ± 0.5 DEG C, phase
To humidity (45~70) %RH.
In a preferred embodiment, thermal measurement system 1 can use isothermal titration formula weight thermal method, but be not limited to titrate
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 used Commercial semiconductors electrothermal module and assemble, according to
Thermal measurement specific requirement selects different model, it is not limited here.
In a preferred embodiment, light source 21 can add deuterium lamp using halogen lamp.
Below with the thermal power and purple of lauryl sodium sulfate (SDS) and 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 invention
Process.
It measures the ultraviolet spectra of the BSA water solution system of the 5mg/ml of 0.6ml first before drop reaction, then drips every time
Enter 10 microlitres of SDS, measurement titration heat measures ultraviolet spectra, alternately thermal measurement and spectral measurement after titrating thermal measurement.
Such as Fig. 4 (a) and (b) are shown respectively for totally 33 titration results and 34 UV adsorption results for the present embodiment, top song in Fig. 4 (b)
Line sequence number 0 indicates 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 component, connection type and manufacture craft etc. are all
It can be varied, all equivalents and improvement carried out based on the technical solution of the present invention should not exclude
Except protection scope of the present invention.
Claims (8)
1. a kind of thermal power measurement device with Visible imaging simulation measurement function, which is characterized in that thermal power measurement dress
It sets 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 to measure the thermal power of solution reaction system, the thermal measurement system include constant temperature bath, it is heat sink,
Calorimetric pond, reaction tank and hot calibration system, the constant temperature bath is interior to place described heat sink, the heat sink interior placement calorimetric pond,
The calorimetric pond using the design of Shuangzi pond i.e. including size and completely identical in structure sample cell and reference cell, the sample cell and
Reference cell includes heat-conducting block, temperature difference heat pile and reaction tank, is placed for holding the solution in each heat-conducting block
The reaction tank of reaction system or bottom liquid, each heat-conducting block are provided with the optical measurement for placing fiber coupling lens
Hole, the hot calibration system include programme-controlled dc power and the thermal resistance being fixed in the heat-conducting block being attached thereto, described
Programme-controlled dc power heats the thermal resistance using different electric currents and makes the temperature difference heat pile in the case of different input thermal powers
There are different output voltage signals, the temperature difference heat pile output end reversal connection of the sample cell and reference cell, i.e., the described sample cell heat
Pile output head anode connects the reference cell thermoelectric pile output head anode, receives outside the two temperature difference heat pile negative pole of output end
Volt is counted as output signal；
The spectral measurement system is used to measure the Visible imaging simulation of solution, and the spectral measurement system includes light source, described
The light that light source issues is divided into two-way light through Y type bifurcation fiber, and it is saturating that two-way light passes through fibre optic attenuator, optical fiber and fiber coupling respectively
Mirror enters the solution reaction system and bottom liquid, and the light being emitted through the solution reaction system and bottom liquid is respectively through the optical fiber coupling
It closes lens and optical fiber enters spectrometer；
The acquisition and control system includes data acquisition device, computer and nanovolt meter, is provided in the computer
Calorimetric module, spectroscopic module and calorimetric-spectrum are combined module；The data acquisition device is for acquiring 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 for adopting
Collect the heat flow signal of the solution reaction system and send it to the calorimetric module, the calorimetric module is surveyed for the heat
The calibration of amount system and thermal power measurement；The spectroscopic module is for acquiring the spectrometer signal and carrying out the solution spectrum
The post-processing of signal；The calorimetric-spectrum combination module controls for realizing the measurement of thermal power and spectral signal.
2. the thermal power measurement device as described in claim 1 with Visible imaging simulation measurement function, which is characterized in that
Require temperature control at 20 to 25 DEG C between the constant temperature and humidity, temperature-controlled precision ± 0.5 DEG C, relative humidity (45~70) %RH.
3. such as the described in any item thermal power measurement devices with Visible imaging simulation measurement function of claims 1 to 2,
It is characterized in that, the thermal measurement system uses isothermal titration formula weight thermal method.
4. the thermal power measurement device as described in claim 1 with Visible imaging simulation measurement function, which is characterized in that
Each reaction tank is all made of quartz glass tube.
5. the thermal power measurement device as described in claim 1 with Visible imaging simulation measurement function, which is characterized 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.
6. the thermal power measurement device as described in claim 1 with Visible imaging simulation measurement function, which is characterized in that
Each heat-conducting block is all made of highly heat-conductive material and is made.
7. the thermal power measurement device as claimed in claim 1 or 2 with Visible imaging simulation measurement function, feature exist
In the light source adds deuterium lamp using halogen lamp.
8. the thermal power measurement device with Visible imaging simulation measurement function as described in claim 2 or 4 or 5 or 6,
It is characterized in that, is applied on the temperature difference heat pile in the calorimetric pond after spectral measurement by the programme-controlled dc power
The directly cooling reaction tank of electric current and reference cell enable it be rapidly achieved thermal balance, realize rapid survey.
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| CN108061726B (en) * | 2017-12-04 | 2020-07-14 | 中国科学院化学研究所 | Isothermal thermal power measuring device with fluorescence spectrum measuring function |
| CN107748178B (en) * | 2017-12-04 | 2019-09-27 | 中国科学院化学研究所 | Thermal power measurement device with visible-ultraviolet, fluorescence and raman spectroscopy measurement |
| CN107976467B (en) * | 2017-12-04 | 2019-12-10 | 中国科学院化学研究所 | Thermal power measuring device with Raman spectrum measuring function |
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