CN107576622A - A kind of micro hot systems of monochromatic light - Google Patents
A kind of micro hot systems of monochromatic light Download PDFInfo
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- CN107576622A CN107576622A CN201710013543.0A CN201710013543A CN107576622A CN 107576622 A CN107576622 A CN 107576622A CN 201710013543 A CN201710013543 A CN 201710013543A CN 107576622 A CN107576622 A CN 107576622A
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- monochromatic light
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Abstract
The present invention relates to a kind of development of monochromatic light low-grade fever amount system.Whole combined system is made up of micro- calorimeter, monochromatic light source, optical fiber and computer.When system works, monochromatic light caused by light source is incorporated into the sample cell and reference cell of micro- calorimeter through optical fiber, the system is a kind of new light low-grade fever amount system, it is suitable for photoinduction and the detection of light-initiated chemistry and physical process, the particularly thermodynamics in situ to photochemical reaction process and dynamic (dynamical) Simultaneous Determination, process thermodynamics, process kineticses and mechanism is interrelated, Microcalorimetric method is promoted in spectroscopy and photochemical development, the technology is expected to have widely application prospect in the science such as chemistry, biology, medicine and high polymer material.
Description
Technical field
The present invention relates to a kind of development of monochromatic light-low-grade fever amount system.Whole combined system is by micro- calorimeter, monochromatic light ray
Source, optical fiber and computer composition.System work when, monochromatic light caused by light source through optical fiber be incorporated into micro- calorimeter sample cell and
Reference cell, the system are a kind of new light-low-grade fever amount systems, are suitable for photoinduction and the inspection of light-initiated chemistry and physical process
Survey, particularly the thermodynamics in situ to photochemical reaction process and dynamic (dynamical) Simultaneous Determination, by process thermodynamics, process power
Learn and mechanism it is interrelated, promote Microcalorimetric method in spectroscopy and photochemical development, the technology be expected to chemistry, biology,
There is widely application prospect in the science such as medicine and high polymer material.
Background technology
Be developed in succession in a variety of photochemical catalysts of the past few decades using titanium dioxide as representative, but to its catalytic mechanism and
The research of catalytic theory relatively lags behind, it is difficult to clearly recognizes the Fundamental Aspects such as catalytic nature, the complicated catalytic process
Often likened to a flight data recorder for having no way of opening.Therefore, develop new technological means in-situ synchronization research chemistry thermodynamics,
Dynamics and the mechanism problem in molecular level change, are to crack the most effective approach of this flight data recorder；
Either chemical process, or life process or physical process, there is the machine of thermodynamics, dynamics and process occurrence and development
The Fundamental Aspects such as reason or mechanism, chemistry and its correlated process scientific research seek to solve chemical thermodynamics, chemomotive force
The mechanism problem learned and changed on a molecular scale.Light-low-grade fever amount system undoubtedly provides research photochemical reaction original position mistake
The new science method of journey, this method in real time, not damaged and intuitively obtain its thermokinetics fine information, synchronously by reaction
Situ process, degradation rate and Thermodynamic Correlation in situ.Domestic First LED- white lights-low-grade fever amount system is built by this seminar,
And it is used for the thermodynamics and kineticses in situ for studying photocatalytic process first, by the situ process of reaction, degradation rate and original position
Thermodynamic Correlation.[a) Li Xingxing, model is superb, Ma Zhao, Tan Xuecai, yellow anti-in the visible optical drive Ag AgCl catalysis of silver-colored
Micro heat research [J] the Chinese sciences in situ answered:Chemistry, 2014 (10): 1576-1584. b) X. X. Li, Z.
Y. Huang, Z. J. Liu, K. S. Diao, G. C. Fan, Z. Huang, X. C. Tan. In situ
photocalorimetry: An alternative approach to study photocatalysis by tracing
heat changes and kinetics[J]. Applied Catalysis B: Environmental, 2016, 181,
79 ]；
Compared to LED- light-low-grade fever amount system, monochromatic light-low-grade fever amount system has more advantage, with the laser of different wave length (such as 405,
432 and 532 nm etc.) be light source, available for research temperature, light intensity and incident wavelength etc. to the thermodynamics in situ of photochemistry,
The influence of kinetics and mechanism；Temperature programming simultaneously, determines system optimal reaction temperature；The different monochromatic light quantum effects of measure
Rate, such as determine bio-light combined coefficient.Promoting Microcalorimetric method, the technology is expected to changing in spectroscopy and photochemical development
There is widely application prospect in the science such as, biology, medicine and high polymer material.
The content of the invention
It is an object of the invention to provide a kind of monochromatic light-low-grade fever amount system, its property indices meets quantitative analysis will
Ask.
The present invention is realized by following proposal.It, which includes it, includes monochromatic light source (1), optical fiber (2), micro- calorimeter
And computer (9) (3).Its connected mode is：Light caused by monochromatic light source (1) is respectively connecting to the sample in micro- calorimeter (3)
Product pond (4) and reference cell (5), micro- calorimeter (3) are connected with computer (9).Sample cell passage (6) is by sample cell passage (4) by 1
A diameter of 10 μm, long 1.5 m of root glass optical fiber, for light caused by light source (1) to be introduced into sample cell (4).Reference cell leads to
Road (7) is by 1 a diameter of 10 μm, long 1.5 m glass optical fiber, for light caused by light source (1) to be introduced into reference cell (5).
It is an advantage of the invention that novel in design, connection is ingenious, and the high temperature control of detection sensitivity is accurate, at the same obtain photochemistry and
Photocatalytic process original position thermodynamics and kineticses, process thermodynamics, process kineticses and mechanism is interrelated, it can be used for simultaneously
Study the influence to the thermodynamics in situ, kinetics and mechanism of photochemistry such as temperature, light intensity and lambda1-wavelength；Program liter
Temperature, determine system optimal reaction temperature；The different monochromatic photo-quantum efficiencies of measure；Microcalorimetric method is promoted in spectroscopy and light
The development of chemistry, the technology are expected to have widely application prospect in the science such as chemistry, biology, medicine and high polymer material.
Brief description of the drawings
Accompanying drawing 1 is monochromatic light-low-grade fever amount system structure diagram；
Accompanying drawing 2 is 405 nm laser respectively in the light intensity (a) of sample cell and reference cell and baseline zero adjustment (b)；
Accompanying drawing 3 is caused divalence Fe after embodiment mesoxalic acid ferripotassium illumination different time decomposes2+Match somebody with somebody with 1,10- Phens
Compound (Fe2+(oph)3) ultraviolet visible absorption spectra figure (a) and potassium ferric oxalate min of illumination 5 in monochromatic light-low-grade fever amount system
(b) and the min (c) of illumination 10 heat flow curve.
Embodiment
The technical characteristic of the present invention is described in detail in conjunction with accompanying drawing.The invention mainly comprises monochromatic light source (1), optical fiber
(2), micro- calorimeter (3) and computer (9).When system works, 2 mL (V are added in sample cell1) 0.006 M potassium ferric oxalate
([Fe(C2O4)3]3-) solution, 2 mL deionized waters are added in reference cell.Then under the conditions of 25 DEG C, arrange parameter and in baseline
Light source is opened after steady, light caused by light source (1) is respectively connecting to sample cell (4) and reference cell (5) in micro- calorimeter (3),
The incident interface of optical fiber (8) the connection fiber spectrometer (9) of sample cell (4), by determining photodissociation of the potassium ferric oxalate in visible ray
Enthalpy is evaluated to instrument performance index.
After illumination certain time, 1 mL (V2) 10 mL (V of illumination solution injection3) in volumetric flask, add 0.5 mL HAc-
NaAc cushioning liquid and 4 mL 1,10- o-phenanthrolines (0.1%) mixed solution, and it is diluted to graduation mark with deionized water.Lucifuge
Place at least 30 min and form complex.When being 25 min for light application time, it is contemplated that the applicable bar of Lambert-Beer's law
Part, avoid concentration is excessive from causing UV-vis absorption spectrum not meet Lambert-Beer's law, take 0.5 mL (V2) illumination solution
Inject 10 mL (V3) in volumetric flask, adding 0.25 mL HAc-NaAc cushioning liquid and 2 mL 1,10- o-phenanthrolines
(0.1%) mixed solution, and graduation mark is diluted to deionized water, avoid light place at least 30 min are fully coordinated colour developing.Reference cell
In under the conditions of not illumination repeat aforesaid operations.The Fe of generation2+Mole can be calculated as follows：
,
Wherein A：Difference of the complex in 510nm absorbance in sample cell and reference cell；ε is ferrous ion complex compound in 510nm
Absorption constant (11100 Lmol at place-1·cm-1)；bFor light path, the i.e. photometric printing opacity thickness of ultraviolet-visible
(1.0cm)。
At 25 DEG C, potassium ferric oxalate ([Fe (C2O4)3]3-) photodissociation when standard molar reaction enthalpy be calculated as follows formula：
WhereinQFor the potassium ferric oxalate ([Fe (C shown in monochromatic light-low-grade fever amount system2O4)3]3-) photodissociation heat；n(Fe2+) be
Fe2+The amount of material.
Before experiment, the regulation of monochromatic light-low-grade fever amount system incident light source is divided to following two steps：First, pass through outside instrument
Light power meter determines two-beam intensity.As shown in Figure 2 a, sample cell and reference cell incident light source light intensity be respectively (19.53 ±
0.20) W m-2(19.15 ± 0.14) W m-2.Again by finely tuning 405 nm, as shown in Figure 2 b, although two-beam fiber
Intensity is more or less the same, but its heat affecting is not zero, and shows that the light intensity of sample cell is more than reference cell light intensity.In order to further reduce partially
Difference, need to be by the light intensity decreasing of sample cell, until fuel factor difference caused by two ponds substantially eliminates；
Fig. 3 is Fe caused by different light application time potassium ferric oxalate light decompose2+The purple of the complex compound formed with 1,10- o-phenanthrolines
Outside-visible absorption spectra figure, absorption peak position is 510 nm corresponding to it, and the absorption intensity of four groups of experiments is shown in Table 1.Fig. 3 (b),
Fig. 3 (c) be under the conditions of 25 DEG C of normal pressure potassium ferric oxalate in the in-situ heat moving curve of the photolysis reactionses of different light application times.In order to enter
One step reduces because of minor departures caused by sample cell and reference cell, and 2.0 mL deionized waters are filled in two ponds, and in identical bar
Part, identical light application time carry out the hot blank control experiment of light quantity.Only the heat score-curve in situ reacted is to determine grass by light calorimeter
Sour ferripotassium photodissociation heat score-curve deducts blank control and tests to obtain.It was found from figure, four curves occur absorbing heat first again gradual
Into exothermic phase.
It is anti-that its normalized molar can be obtained according to the heat flow curve of potassium ferric oxalate light-catalyzed reaction and uv-vis spectra absorption figure
Ying Han, standard molar reaction enthalpy are (- 59.9425 ± 2.7298) kJmol-1, with document [Adamson, A. W.,
Vogler, A., Kunkely, H. Photocalorimetry enthalpies of photolysis of trans-
azobenzene, ferrioxalate and cobaltioxalate ions, chromium hexacarbonyl, and
dirhenium decarbonyl. Journal of The American Chemical Society, 1978, 100(4):
1298-1300] value it is close, illustrate combined system be scientific and reasonability.
The standard molar reaction enthalpy that 25 DEG C of potassium ferric oxalate light decomposes
Claims (3)
- A kind of 1. monochromatic light-low-grade fever amount system, it is characterised in that：It includes monochromatic light source (1), optical fiber (2), micro- calorimeter And computer (9) (3)；Its connected mode is：Light caused by monochromatic light source (1) is respectively connecting to the sample in micro- calorimeter (3) Product pond (4) and reference cell (5), micro- calorimeter (3) are connected with computer (9).
- 2. according to the monochromatic light described in right 1-low-grade fever amount system, it is characterised in that：Sample cell passage (6) is by sample cell passage (4) by 1 a diameter of 10 um, long 1.5 m glass optical fiber, for light caused by light source (1) to be introduced into sample cell (4).
- 3. according to the monochromatic light described in right 1-low-grade fever amount system, it is characterised in that：Reference cell passage (7) is by 1 a diameter of 10 Um, long 1.5 m glass optical fiber, for light caused by light source (1) to be introduced into reference cell (5).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2031530U (en) * | 1988-05-09 | 1989-01-25 | 张�杰 | Automatic photo controlled titration apparatus |
| US20090122317A1 (en) * | 2005-09-07 | 2009-05-14 | Masafumi Ito | Spectroscopy Method and Spectroscope |
| CN101592624A (en) * | 2009-06-19 | 2009-12-02 | 上海理工大学 | Be applicable to the microcalorimetric method of microbial count situation in the fast detecting food |
| CN201653885U (en) * | 2010-04-09 | 2010-11-24 | 苏州大学 | Micro-plate reader |
| CN102645448A (en) * | 2012-04-10 | 2012-08-22 | 西安科技大学 | Method for measuring growth cycle of puccinia striiformis by using microcalorimetric method |
-
2017
- 2017-01-09 CN CN201710013543.0A patent/CN107576622A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2031530U (en) * | 1988-05-09 | 1989-01-25 | 张�杰 | Automatic photo controlled titration apparatus |
| US20090122317A1 (en) * | 2005-09-07 | 2009-05-14 | Masafumi Ito | Spectroscopy Method and Spectroscope |
| CN101592624A (en) * | 2009-06-19 | 2009-12-02 | 上海理工大学 | Be applicable to the microcalorimetric method of microbial count situation in the fast detecting food |
| CN201653885U (en) * | 2010-04-09 | 2010-11-24 | 苏州大学 | Micro-plate reader |
| CN102645448A (en) * | 2012-04-10 | 2012-08-22 | 西安科技大学 | Method for measuring growth cycle of puccinia striiformis by using microcalorimetric method |
Non-Patent Citations (3)
| Title |
|---|
| XINGXING LI 等: "In situ photocalorimetry：An alternative approach to study photocatalysis by tracing heat changes and kinetics", 《APPLIED CATALYSIS B:ENVIRONMENTAL》 * |
| 唐晋发 等: "《现代光学薄膜技术》", 30 November 2006 * |
| 李星星 等: "可见光驱动Ag@AgCl催化反应的原位微量热研究", 《中国科学：化学》 * |
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