CN101539521A - Constant-temperature fluorescence detector with optical fiber reference light paths - Google Patents
Constant-temperature fluorescence detector with optical fiber reference light paths Download PDFInfo
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- CN101539521A CN101539521A CN200910135726A CN200910135726A CN101539521A CN 101539521 A CN101539521 A CN 101539521A CN 200910135726 A CN200910135726 A CN 200910135726A CN 200910135726 A CN200910135726 A CN 200910135726A CN 101539521 A CN101539521 A CN 101539521A
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 28
- 230000003287 optical effect Effects 0.000 claims abstract description 30
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- 239000000523 sample Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
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Abstract
A constant-temperature fluorescence detector with optical fiber reference light paths relates to an optical monitoring instrument in chemical analysis. Aside from an optical system and a signal detecting and treating system, the constant-temperature fluorescence detector also comprises an auto water-inlet constant-temperature device comprising a temperature controller, a digital temperature probe and a constant-temperature cabinet; the digital temperature probe detects water temperature inside a water inlet tube, and according to the detected water temperature, the temperature controller controls a cooling device and a heating device inside the constant-temperature cabinet so as to realize the constant temperature of inlet water inside a sample cell. The detector adopts optical fibers as reference light paths and is internally provided with the auto water-inlet constant-temperature device simultaneously, therefore not only has high sensitivity, simple method, good reproducibility and easy realization of automation, but also avoids the interferences to detection result caused by environment temperature, instantaneous vibration of light source and light intensity attenuation. The detector has small host volume, thus being convenient to carry and place.
Description
Technical field
The present invention relates to a kind of fluorescence detector, belong to the optical inspection techniques field in the chemical analysis.
Background technology
The fluorescence spectrum technology is nearly 20 years new chemical analytical approachs of rising, and its relies on measures some organic substances that contain special chemical structure such as conjugated launch the qualitative or quantitative test that the light of specific wavelength is finished these organic compounds under the exciting of visible light or ultraviolet light.Nowadays, fluorometry has developed into a kind of very important and effective spectrochemical analysis means, introducing along with some new technologies of aspect such as laser, microprocessor, optoelectronics, light transmitting fiber and nano materials, promoted fluorometry greatly in development theoretical and that use fermentation, made fluorometry constantly towards efficient, trace, real-time and robotization aspect development.
Fluorescent material except that excitation wavelength with emission wavelength is different, fluorescent characteristic parameters such as quantum yield, fluorescence lifetime and fluorescence polarization are difference to some extent also, can realize the qualitative analysis of material by the mensuration of these characterisitic parameters.Quantitative test is according to Beer-Lambert law, when ε bc＜＜0.05,
I
f＝2.303Y
jI
oεbc (1)
I in the formula
fBe fluorescence intensity, Y
fThe fluorescence quantum yield of material, I
0Be excitating light strength, ε material molar absorptivity, b are the solution light path, and c is a solution concentration.
Fluorometry has following advantage: fluorometry is highly sensitive, than taller 2～3 orders of magnitude of beam split photometry sensitivity.Another advantage of fluorometry is the selectivity height, because the fluorescent characteristic parameter of fluorescent material is many, as: excitation wavelength, emission wavelength, quantum yield, fluorescence lifetime and fluorescence polarization etc., add emerging synchronous scanning, 3-D scanning, derivative spectrum, time resolution and some fluorimetric new technologies such as resolution mutually, can realize selective determination well.In addition, fluorometry is easy, favorable reproducibility, and sampling amount is few, easily is automated, and instrument and equipment is simple.
The major defect of fluorescence method is that the spectrum that measures is influenced greatly by temperature, the instantaneous shake of light source and incident intensity.But fluorescence detector self does not have the sample introduction automatic thermostatic device at present, and measurement result is subject to temperature disturbance.Most of fluoroscopic examination instrument does not have reference light paths, and measurement result is disturbed by instantaneous shake of light source and light intensity attenuation, so the comparability of the testing result of different time is relatively poor.Though some is provided with reference light paths, adopted complicated beam-splitting structure and negative feedback correcting unit, cause the detector complex structure.
Summary of the invention
At the deficiencies in the prior art and defective, the invention provides a kind of constant-temperature fluorescence detector that has optical fiber reference light paths, make it not only simple in structure, and avoided the interference of environment temperature, the instantaneous shake of light source and light intensity attenuation testing result.
Technical scheme of the present invention is as follows:
A kind of constant-temperature fluorescence detector that has optical fiber reference light paths contains optical system and input and disposal system; Described optical system comprises light source 1, condenser 2, exciting light interference filter 3, the first optical slot 4a, light beam beam-splitting board 5, emission optical interference filter 11 and the second optical slot 4b successively, on light beam beam-splitting board 5, connect reference light paths 6, reference light paths connects the first photomultiplier 7a, and the second optical slot 4b connects the second photomultiplier 7b; Sample cell is placed between light beam beam-splitting board 5 and the emission optical interference filter 11; Described input and disposal system comprise filtering circuit 12, amplifying circuit 13, A/D converter 14, central processing unit 15 and storer 16, the electric signal that the described first photomultiplier 7a and the second photomultiplier 7b produce is through filtering circuit 12 filtering, after amplifying circuit 13 signals amplify, be transformed into digital signal through A/D converter 14, the program that central processing unit 15 calls in the storer 16 is analyzed and is handled digital signal, it is characterized in that: described constant-temperature fluorescence detector also comprises into water automatic thermostatic device, and this water inlet automatic thermostatic device comprises temperature controller 24, digital temperature probe 20 and constant temperature oven 8; The water temperature that described digital temperature probe 20 detects in the water inlet pipe 9, temperature controller 24 are according to detected water temperature, and refrigerating plant 18 in the control constant temperature oven and heating arrangement 19 are realized the water inlet constant temperature of sample cell 10; Described reference light paths 6 adopts reference optical fiber.
In the technique scheme, the temperature of described automatic thermostatic device control is at 25 ℃ ± 0.01 ℃.
Reference light paths 6 of the present invention adopts reference optical fiber, and described reference optical fiber is made up of the fixed chuck 26 at fibre bundle 27, the metal hose 25 that is arranged on fibre bundle 27 outsides and two ends.Described refrigerating plant 18 adopts semiconductor chilling plate; Described heating arrangement 19 adopts the electrical heating bar.
The present invention is comparing with existing luminoscope technical scheme, and have the following advantages and the high-lighting effect: the present invention adopts optical fiber as reference light paths, simultaneously built-in water inlet automatic thermostatic device, not only highly sensitive, method is easy, and favorable reproducibility easily is automated; And it is simple in structure; And avoided environment temperature, the instantaneous shake of light source and light intensity attenuation to the interference of testing result, and simplified correcting unit simultaneously, realized real-time monitoring to light source, eliminated the interference of the intensity of light source to measuring.The instrument host volume is little, and 450 * 400 * 160mm only is easy to carry and lays.When light source ages, prompting is changed automatically.Detector actual measurement signal to noise ratio (S/N ratio) is greater than 108, and the response time only is 100ms.
Description of drawings
Fig. 1 is the theory structure synoptic diagram that has the constant-temperature fluorescence detector of optical fiber reference light paths.
Fig. 2 is the thermostat fundamental diagram.
Fig. 3 is the structural representation of optical fiber.
Among the figure: the 1-light source; The 2-condenser; 3-exciting light interference filter; 4a-first optical slot; 4b-second optical slot; 5-light beam beam-splitting board; The 6-optical fiber reference light paths; 7a-first photomultiplier; 7b-second photomultiplier; The 8-constant temperature oven; The 9-water inlet pipe; The 10-sample cell; 11-launches optical interference filter; The 12-filtering circuit; The 13-amplifying circuit; The 14-A/D converter; The 15-central processing unit; The 16-storer; The 18-semiconductor chilling plate; The 19-fire-bar; 20-digital temperature probe; The 21-dc solid-state relay; The 22-ac solid relay; The 23-power module; The 24-temperature controller; The 25-metal hose; The 26-fixed chuck; The 27-fibre bundle.
Embodiment
Below in conjunction with accompanying drawing concrete structure of the present invention, principle of work and the course of work are further described.
A kind of constant-temperature fluorescence detector that has optical fiber reference light paths contains optical system and input and disposal system; Described optical system comprises light source 1, condenser 2, exciting light interference filter 3, the first optical slot 4a, light beam beam-splitting board 5, emission optical interference filter 11 and the second optical slot 4b successively, on light beam beam-splitting board 5, connect reference light paths 6, reference light paths connects the first photomultiplier 7a, and the second optical slot 4b connects the second photomultiplier 7b; Sample cell is placed between light beam beam-splitting board 5 and the emission optical interference filter 11; The light that light source 1 sends becomes directional light behind condenser 2, directional light has only required exciting light to pass through after filtering through exciting light interference filter 3, required exciting light by the first optical slot 4a after by light beam beam-splitting board 5 be divided into two the bundle directional lights, a branch of first photomultiplier 7a that incides is as reference, a branch ofly incide excited sample on the sample cell 10, the fluorescence of generation filters after the second optical slot 4b incides the second photomultiplier 7b through emission optical interference filter 11; Described input and disposal system comprise filtering circuit 12, amplifying circuit 13, A/D converter 14, central processing unit 15 and storer 16, the electric signal that the described first photomultiplier 7a and the second photomultiplier 7b produce is through filtering circuit 12 filtering, after amplifying circuit 13 signals amplify, be transformed into digital signal through A/D converter 14, the program that central processing unit 15 calls in the storer 16 is analyzed and is handled digital signal, it is characterized in that: described constant-temperature fluorescence detector also comprises into water automatic thermostatic device, and this water inlet automatic thermostatic device comprises temperature controller 24, digital temperature probe 20 and constant temperature oven 8; The water temperature that described digital temperature probe 20 detects in the water inlet pipe 9, temperature controller 24 are according to detected water temperature, and refrigerating plant 18 in the control constant temperature oven and heating arrangement 19 are realized the water inlet constant temperature of sample cell 10; Described reference light paths 6 adopts reference optical fiber.In the technique scheme, the temperature of described automatic thermostatic device control is at 25 ℃ ± 0.01 ℃.Described fine reference light paths 6 adopts reference optical fiber, and described reference optical fiber is made up of the fixed chuck 26 at fibre bundle 24, the metal hose 25 that is arranged on fibre bundle 24 outsides and two ends.Described refrigerating plant 18 adopts semiconductor chilling plate; Described heating arrangement 19 adopts the electrical heating bar.
Water inlet thermostat proposed by the invention as shown in Figure 2.Water inlet pipe 9, semiconductor chilling plate 18 and fire-bar 19 are sealed in the constant temperature oven of being made by thermal insulation material 17, the constant temperature oven water outlet is flowed through behind digital temperature probe 20 (precision ± 0.1%), water temperature signal reaches artificial intelligence temperature controller 24 (precision ± 0.3%) and shows in real time, can set detected temperatures by temperature controller.Temperature controller is controlled the break-make of dc solid-state relay 21 and ac solid relay 22 by judging the difference of inflow temperature and design temperature, thereby decision triggers refrigeration or heating arrangement is realized the constant temperature of intaking.Water inlet enters sample cell 10 by water inlet pipe 9 and carries out fluoroscopic examination behind constant temperature.
Reference light paths adopts silica fibre, optical fiber designs as shown in Figure 3, fibre bundle 27 is made up of the superfine optical fiber of 15～25 softnesses, this design can guarantee to see through light intensity can make whole fibre bundle arbitrarily crooked again, satisfy the needs of assembly layout, (depend on that fibre bundle comprises the quantity and the machining precision of optical fiber) about whole optical fiber beam diameter 1mm, outside cover metal hose 25, the fibre bundle two ends are fixing by fixed chuck 26, and dop band external thread is realized being connected with light beam beam-splitting board 5.Instrument relies on the real-time monitoring that has realized light source that is provided with of optical fiber, with the gained fluorescence intensity divided by excitating light strength, multiply by again and excite light intensity when light source is just adorned, with the normalization of gained fluorescence intensity, fluorescence intensity and excitating light strength are irrelevant after the normalization, and be only relevant with the self attributes and the solution light path of fluorescent material.
Claims (4)
1. the constant-temperature fluorescence detector with optical fiber reference light paths contains optical system and input and disposal system; Described optical system comprises light source (1), condenser (2), exciting light interference filter (3), first optical slot (4a), light beam beam-splitting board (5), emission optical interference filter (11) and second optical slot (4b) successively, on light beam beam-splitting board (5), connect fine reference light paths (6), reference light paths connects first photomultiplier (7a), and second optical slot (4b) connects second photomultiplier (7b); Sample cell is placed between light beam beam-splitting board (5) and the emission optical interference filter (11); Described input and disposal system comprise filtering circuit (12), amplifying circuit (13), A/D converter (14), central processing unit (15) and storer (16), the electric signal that described first photomultiplier (7a) and second photomultiplier (7b) produce is through filtering circuit (12) filtering, after amplifying circuit (13) amplifies electric signal, be transformed into digital signal through A/D converter (14), the program that central processing unit (15) calls in the storer (16) is analyzed and is handled digital signal, it is characterized in that: described constant-temperature fluorescence detector also comprises into water automatic thermostatic device, and this water inlet automatic thermostatic device comprises temperature controller (24), digital temperature probe (20) and constant temperature oven (8); Described digital temperature probe (20) detects the water temperature in the water inlet pipe (9), and temperature controller (24) is according to detected water temperature, and refrigerating plant (18) in the control constant temperature oven and heating arrangement (19) are realized the water inlet constant temperature of sample cell (10); Described reference light paths (6) adopts optical fiber.
2. according to the constant-temperature fluorescence detector of the described band optical fiber reference light paths of claim 1, it is characterized in that: the temperature of described automatic thermostatic device control is at 25 ℃ ± 0.01 ℃.
3. according to the constant-temperature fluorescence detector of claim 1 or 2 described band optical fiber reference light paths, it is characterized in that: described reference optical fiber is made up of fibre bundle (24), the metal hose (25) that is arranged on fibre bundle (24) outside and the fixed chuck (26) at two ends.
4. according to the constant-temperature fluorescence detector of the described band optical fiber reference light paths of claim 1, it is characterized in that: described refrigerating plant (18) adopts semiconductor chilling plate; Described heating arrangement (19) adopts the electrical heating bar.
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| CN200910135726A CN101539521A (en) | 2009-04-27 | 2009-04-27 | Constant-temperature fluorescence detector with optical fiber reference light paths |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111175236A (en) * | 2020-01-09 | 2020-05-19 | 中国原子能科学研究院 | Light path correction method and device for baseline drift in glove box type online spectral analysis |
| CN112835190A (en) * | 2021-01-04 | 2021-05-25 | 桂林电子科技大学 | Double-core optical fiber light control and dynamic speckle illumination microscopic imaging method and system |
-
2009
- 2009-04-27 CN CN200910135726A patent/CN101539521A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111175236A (en) * | 2020-01-09 | 2020-05-19 | 中国原子能科学研究院 | Light path correction method and device for baseline drift in glove box type online spectral analysis |
| CN112835190A (en) * | 2021-01-04 | 2021-05-25 | 桂林电子科技大学 | Double-core optical fiber light control and dynamic speckle illumination microscopic imaging method and system |
| CN112835190B (en) * | 2021-01-04 | 2022-08-09 | 桂林电子科技大学 | Based on two core optic fibre light manipulation and dynamic speckle illumination microscopic imaging system |
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