Multi-usage spectrophotometer
Technical field
The present invention relates to the spectrophotometer using in a kind of spectral analysis, particularly a kind of can be directly as the multi-usage spectrophotometer of liquid chromatography multichannel array detecting device and common transmission measurement.
Background technology
UV-visible detector is in liquid chromatography, to configure maximum detecting devices, along with technical development and application level promote, can measure the use of the hyperchannel UV-visible detector of multi-wavelength response simultaneously and also day by day popularize.Multichannel detector can detect chromatogram and flow out the spectrum change of process in liquid chromatography, realizes the functions such as qualitative, quantitative, peak purity check, finger-print expression by spectrum.Liquid chromatography photometric detector can be realized the spectrophotometer of continuous coverage from the principle exactly, but due to testing goal difference, spectrophotometer and liquid chromatogram detector are all to create two kinds of instruments according to not isostructure, complete different analysis task.
Spectrophotometer is conventional analysis instrument, and along with laboratory equipment level improves, liquid chromatography photometric detector also becomes conventional analysis instrument gradually, and in laboratory, spectrophotometric usage frequency is greater than liquid chromatography photometric detector conventionally.Spectrophotometer and liquid chromatography photometric detector, as the instrument of same principle, due to structural differences, caused function repeated configuration.Multi-wavelength scanning type photometer and hyperchannel chromatogram photometric detector, due to better function, configuration and use also day by day increase, but instrument cost is higher at present, has affected popularization.
Summary of the invention
The technical problem to be solved in the present invention is: have identical instrumental analysis principle for existing liquid chromatography photometric detector and spectrophotometer, but due to lack can be unified the means that realize, and manufacture respectively and purchase, the problem that causes instrument resource not distribute rationally, provide a kind of can be directly as the multi-usage spectrophotometer of liquid chromatography multichannel array detecting device and common transmission measurement.
The technical scheme solving the problems of the technologies described above is: collimation lens A, cuvette device, slit, collimating mirror, grating and linear array electrooptical device that this photometer comprises light source, on the output main optical path of light source, is arranged in order, described cuvette device comprises cuvette support and can realize the cuvette that the visible spectrophotometry of general ultraviolet, liquid chromatography hyperchannel luminosity detect, trace flows colorimetric measurement function, and this cuvette is arranged on cuvette support; Between described cuvette device and slit, connect by optical fiber.
Between described collimation lens A and cuvette device, be connected by optical fiber.
Further technical scheme of the present invention is: described cuvette comprises can be realized the conventional cuvette of the visible spectrophotometry function of general ultraviolet and can realize the floating cuvette that liquid chromatography hyperchannel luminosity detects, trace flows colorimetric measurement function.
Further technical scheme more of the present invention is: described floating cuvette comprises airtight cuvette body, is provided with and flows than chrominance channel in cuvette body, and this flows and increases gradually than the diameter streamwise of chrominance channel; The top of cuvette body be respectively equipped with flow the sample feeding pipe that is connected than chrominance channel and reclinate go out sample pipe, the caliber that goes out sample pipe is greater than the caliber of sample feeding pipe, sample feeding pipe is connected with liquid chromatography inflow pipe by pipe joint.
Sample feeding pipe in described floating cuvette, go out sample pipe and flow all to adopt the fine pore of diameter≤2mm than the caliber of chrominance channel, sample feeding pipe, go out sample pipe and flow more level and smooth than the inside of chrominance channel and junction is seamless.
Described pipe joint comprises joint body, this joint body is fixed on the porch of sample feeding pipe, joint body is provided with the connecting hole that diameter increases gradually between liquid chromatography inflow pipe and sample feeding pipe, joint body is also provided with stepped hole in upper end, and be provided with external thread at the outer wall of stepped hole, clamp ring for clamping liquid chromatography inflow pipe is installed on described stepped hole, and the pipe joint nut for compressing clamp ring and matching with the external thread of joint body is installed at clamp ring top.
Described joint body adopts Teflon or stainless steel material to make.
Described cuvette support comprises base, is fixed on the cylinder-shaped bracket wall on base, in cylinder-shaped bracket wall, be placed with described cuvette, described cylinder-shaped bracket wall is provided with fiber optic collimator access joint at light light incident side, at light emitting side, fiber optic collimator is installed and picks out joint, this fiber optic collimator access joint, fiber optic collimator pick out joint and are connected with the optical fiber that is positioned at cuvette device light light incident side and emitting side by coupling fiber joint respectively.
Described fiber optic collimator access joint comprises internal thread sleeve pipe, male-pipe A and male-pipe B, the endoporus middle part of described internal thread sleeve pipe is provided with collimation lens set, male-pipe A and male-pipe B are arranged on respectively the both sides of collimation lens set, male-pipe A is connected with the optical fiber that is positioned at cuvette device light light incident side by coupling fiber joint, and male-pipe B is connected with cylinder-shaped bracket wall; Described fiber optic collimator picks out joint and comprises internal thread sleeve pipe, male-pipe C and male-pipe D, the endoporus middle part of described internal thread sleeve pipe is provided with collimation lens B, male-pipe C and male-pipe D are arranged on respectively the both sides of collimation lens, male-pipe C is connected with the optical fiber that is positioned at cuvette device light emitting side by coupling fiber joint, and male-pipe D is connected with cylinder-shaped bracket wall.
Described coupling fiber joint comprises ferrule and the flexible optical fiber jacket of fibre-optical splice nut, fiber orientation snap ring, rigidity, described ferrule, optical fiber jacket are coated on respectively outside optical fiber, ferrule is inserted in the through hole of male-pipe A or male-pipe C, and spacing by fiber orientation snap ring, described fibre-optical splice nut is arranged on outside male-pipe A or male-pipe C and fiber orientation snap ring is compressed.
Owing to adopting technique scheme, multipurpose spectrophotometer of the present invention compared with prior art, has following beneficial effect:
1, can realize a tractor serves several purposes:
Because cuvette device of the present invention comprises cuvette support and can realize the cuvette of the visible spectrophotometry of general ultraviolet, the detection of liquid chromatography hyperchannel luminosity, the mobile colorimetric measurement function of trace, be in the time that described cuvette adopts conventional cuvette, can realize the function of the visible spectrophotometry of general ultraviolet, can make common spectrophotometer and use; In the time that described cuvette adopts floating cuvette, flow cell in the alternative traditional hyperchannel liquid chromatography photometric detector of this floating cuvette, can realize the function that liquid chromatography hyperchannel luminosity detects, can be used as liquid chromatography hyperchannel luminosity detecting device and use; In the time that described cuvette adopts floating cuvette and microsyringe sample introduction, can realize the function of the mobile colorimetric measurement of trace.Therefore, the present invention can realize the object of a tractor serves several purposes, thereby can lowering apparatus deployment cost, promotes the universal of multi-channel detection.
2, stability of instrument is high, and measuring speed is fast, and output data quantity is large:
Owing to the present invention includes light source, collimation lens A, collimation lens set, cuvette device, collimation lens B, slit, collimating mirror, grating and linear array electrooptical device, compared with traditional ultraviolet-visible spectrophotometer, machinery-free of the present invention moves and adjustment component, stability of instrument is high, measuring speed is fast, and output data quantity is large.
3, rational in infrastructure reliable:
Because the characteristic of mobile phase of high performance liquid chromatography is continuously, trace, be plunger flow, the floating cuvette that the present invention adopts substitutes multi-passage circulating pond and has fully taken into account these characteristics.The floating cuvette that the present invention adopts comprises airtight cuvette body, in cuvette body, being provided with flows compares chrominance channel, this flows and increases gradually than the diameter streamwise of chrominance channel, to maintain small pressure reduction, suppress mobile back-mixing and diffusion, while caliber increases gradually can also offset part diffusion length, is conducive to keep separating effect; The top of cuvette body be respectively equipped with flow the sample feeding pipe that is connected than chrominance channel and reclinate go out sample pipe, the caliber that goes out sample pipe is greater than the caliber of sample feeding pipe, suppress mobile back-mixing to form micro-pressure reduction, sample feeding pipe is connected with liquid chromatography inflow pipe by pipe joint; In addition, all calibers in floating cuvette all adopt fine pore, can guarantee the requirement of micro-flow; Sample feeding pipe, go out sample pipe and flow more smoothly and junction is seamless than the inside of chrominance channel, can prevent that mobile phase is resident or form eddy current.Therefore, structure of the present invention is very rationally reliable.
4, signal to noise ratio (S/N ratio) that can lowering apparatus:
The signal to noise ratio (S/N ratio) of luminous flux direct relation instrument of measuring due to absorbance, cuvette device of the present invention has proposed non-parallel light path transmission design and has improved luminous flux, be that incident light flows and enters than the outflow direction of chrominance channel from floating cuvette, in the fiber optic collimator access joint of cuvette support, adopt the combination of collimation lens set, focus is adjusted near mobile colorimetric feeder connection, can utilize so the larger area of colorimetric channel outlet that flows, import larger luminous flux; The collimated picking out in joint through fiber optic collimator again by the light of dispersing after focus is coupled into optical fiber, imports rearmounted light splitting and array electrooptical device.Therefore, the present invention is by improving the signal to noise ratio (S/N ratio) that luminous flux also can lowering apparatus.
5, easy to maintenance, be easy to clean and change instrument component:
The present invention is compared with multichannel detector, and it is simple in structure, and Instrument assembly is directly perceived, easy to maintenance, is easy to clean and change instrument component, and overall cost is low.
6, the present invention is directed to cuvette and the support Design that trace stream hydrodynamic bulk measurement proposes, can meet dynamic and static micro liquid and measure requirement, possess the function of micro-spectrophotometer.
7, adopt significantly lowering apparatus cost of the present invention, improve instrument utilization ratio, strengthen instrument integration degree, improve the rationality of middle-size and small-size Laboratory Instruments resource distribution.
Below, in conjunction with the accompanying drawings and embodiments the spectrophotometric technical characterictic of multipurpose of the present invention is further described.
Accompanying drawing explanation
Fig. 1: the spectrophotometric fundamental diagram of multi-usage described in the embodiment of the present invention one,
Fig. 2~Fig. 3: the structural representation of floating cuvette,
Fig. 2: the main cut-open view, Fig. 3 looked: stereographic map.
Fig. 4: the structural representation of pipe joint described in the embodiment of the present invention one,
Fig. 5: the structural representation of cuvette support described in the embodiment of the present invention one,
Fig. 6: flow than the logical schematic diagram of the light of chrominance channel,
Fig. 7: the structural representation of fiber optic collimator access joint described in the embodiment of the present invention one,
Fig. 8: described in the embodiment of the present invention one, fiber optic collimator picks out the structural representation of joint,
Fig. 9: the structural representation of coupling fiber joint described in the embodiment of the present invention one.
In above-mentioned accompanying drawing, the label of each element is as follows:
1-light source, 2-collimation lens A, 3-optical fiber, 4-cuvette device,
41-cuvette support, 411-base, 412-cylinder-shaped bracket wall, 413-fiber optic collimator access joint,
4131-internal thread sleeve pipe, 4132-male-pipe A, 4133-male-pipe B, 4134-collimation lens set,
414-fiber optic collimator picks out joint, 4141-internal thread sleeve pipe, and 4142-male-pipe C, 4143-male-pipe D,
4144-collimation lens B, 415-coupling fiber joint, 4151-fibre-optical splice nut, 4152-fiber orientation snap ring,
4153-ferrule, 4154-optical fiber jacket, 42-floating cuvette, 421-cuvette body,
422-flows than chrominance channel, 423-sample feeding pipe, and 424-goes out sample pipe, 425-pipe joint,
4251-joint body, 4252-connecting hole, 4253-stepped hole, 4254-clamp ring,
4255-pipe joint nut, 426-liquid chromatography inflow pipe, 5-optical fiber, 6-slit,
7-collimating mirror, 8-grating, 9-linear array electrooptical device,
The flow direction of arrow A-mobile phase, arrow B-light transmission direction, arrow C-cuvette placement direction,
O-colorimetric the channel outlet that flows cross section, the I-colorimetric feeder connection cross section of flowing.
Embodiment
Embodiment mono-:
A kind of multi-usage spectrophotometer, this photometer comprises light source 1, the collimation lens A2 being arranged in order on the output main optical path of light source 1, cuvette device 4, slit 6, collimating mirror 7, grating 8 and linear array electrooptical device 9(are referring to Fig. 1), between described collimation lens A2 and cuvette device 4, be connected by optical fiber 3, between cuvette device 4 and slit 6, connect by optical fiber 5, described cuvette device 4 comprises cuvette support 41 and is arranged on conventional cuvette and the floating cuvette 42 on cuvette support 41, by the switching of conventional cuvette and floating cuvette 42, can realize the visible spectrophotometry of general ultraviolet, liquid chromatography hyperchannel luminosity detects, the functions such as the mobile colorimetric measurement function of trace.
Described conventional cuvette is known structure, no longer its structure is described in detail here; Described floating cuvette 42 is used to form the ratio chrominance channel of tested mobile phase, as shown in Figure 2 to 3, this floating cuvette 42 comprises airtight cuvette body 421, in cuvette body 421, be provided with and flow than chrominance channel 422, flow and increase gradually than the diameter streamwise of chrominance channel 422, to maintain small pressure reduction, suppress mobile back-mixing and diffusion, while caliber increases gradually can also offset part diffusion length, is conducive to keep separating effect; The top of cuvette body 421 be respectively equipped with flow the sample feeding pipe 423 that is connected than chrominance channel 422 and reclinate go out sample pipe 424, the caliber that goes out sample pipe 424 is greater than the caliber of sample feeding pipe 423, sample feeding pipe 423 is connected with liquid chromatography inflow pipe 426 by pipe joint 425, go out sample pipe 424 be bent downwardly can avoid derive mobile phase form step in exit, cause liquid residue and backflow; Sample feeding pipe 423 in described floating cuvette 42, go out sample pipe 424 and flow all to adopt the fine pore of diameter≤2mm than the caliber of chrominance channel 422, sample feeding pipe 423, go out sample pipe 424 and flow more level and smooth and junction is seamless than the inside of chrominance channel 422, to prevent that mobile phase is resident or to form eddy current; Described pipe joint 425 comprises joint body 4251, and this joint body 4251 adopts Teflon material to make, and its material surface tension force is greater than mobile phase, makes mobile phase be not easy to adhere at wall; Joint body 4251 is fixed on the porch of sample feeding pipe 423, joint body 4251 is provided with the connecting hole 4252 that diameter increases gradually between liquid chromatography inflow pipe 426 and sample feeding pipe 423, joint body 4251 is also provided with stepped hole 4253 in upper end, and be provided with external thread at the outer wall of stepped hole 4253, clamp ring 4254 for clamping liquid chromatography inflow pipe 426 is installed on described stepped hole, and pipe joint nut 4255(for compressing clamp ring 4254 and match with the external thread of joint body is installed referring to Fig. 4 at clamp ring 4254 tops).
Described cuvette support 41 comprises base 411, be fixed on cylinder-shaped bracket wall 412(on base 411 referring to Fig. 5), in cylinder-shaped bracket wall 412, be placed with described conventional cuvette or floating cuvette 42, described cylinder-shaped bracket wall 412 is provided with fiber optic collimator access joint 413 at light light incident side, at light emitting side, fiber optic collimator is installed and picks out joint 414, this fiber optic collimator access joint 413, fiber optic collimator pick out joint 414 and are connected with the optical fiber that is positioned at cuvette device 4 light light incident sides and emitting side by coupling fiber joint 415 respectively.
Described fiber optic collimator access joint 413 comprises that internal thread sleeve pipe 4131, male-pipe A4132 and male-pipe B4133(are referring to Fig. 7), the endoporus middle part of described internal thread sleeve pipe 4131 is provided with collimation lens set 4134, this collimation lens set 4134 comprises two collimation lenses, male-pipe A4132 and male-pipe B4133 are arranged on respectively the both sides of collimation lens set 4134, male-pipe A4132 is connected with the optical fiber that is positioned at cuvette device light light incident side by coupling fiber joint 415, and male-pipe B4133 is connected with cylinder-shaped bracket wall 412; Described fiber optic collimator picks out joint 414 and comprises that internal thread sleeve pipe 4141, male-pipe C4142 and male-pipe D4143(are referring to Fig. 8), the endoporus middle part of described internal thread sleeve pipe 4141 is provided with collimation lens B4144, male-pipe C4142 and male-pipe D4143 are arranged on respectively the both sides of collimation lens 4144, male-pipe C4142 is connected with the optical fiber that is positioned at cuvette device light emitting side by coupling fiber joint 415, and male-pipe D4143 is connected with cylinder-shaped bracket wall 412.
Described coupling fiber joint 415 comprises that the ferrule 4153 of fibre-optical splice nut 4151, fiber orientation snap ring 4152, rigidity and the optical fiber jacket 4154(of flexibility are referring to Fig. 9), described ferrule 4153, optical fiber jacket 4154 are coated on respectively outside optical fiber, ferrule 4153 is inserted in the through hole of male-pipe A4132 or male-pipe C4142, and spacing by fiber orientation snap ring 4152, described fibre-optical splice nut 4151 is arranged on outside male-pipe A4132 or male-pipe C4142 and fiber orientation snap ring 4152 is compressed.
Cuvette device of the present invention has proposed non-parallel light path transmission design and has improved luminous flux, be that incident light flows and enters than the outflow direction of chrominance channel from floating cuvette, in the fiber optic collimator access joint of cuvette support, adopt the combination of collimation lens set, focus is adjusted near mobile colorimetric feeder connection cross section I, can utilize so the larger area of colorimetric channel outlet cross section O that flows, import larger luminous flux; The collimated picking out in joint through fiber optic collimator again by the light of dispersing after focus is coupled into optical fiber, imports rearmounted light splitting and array electrooptical device (referring to Fig. 6).
Principle of work of the present invention is as follows:
The present invention adopts rearmounted beam-splitting structure design, as shown in Figure 1, the complex light that light source 1 sends is coupled to optical fiber 3 by collimation lens A2 and transmits, after collimation lens set adjustment by cuvette device 4, expose to cuvette, when cuvette adopts conventional cuvette, can realize the function of the visible spectrophotometry of general ultraviolet, can make common spectrophotometer and use; In the time adopting floating cuvette, the flow cell in the alternative traditional hyperchannel liquid chromatography photometric detector of this floating cuvette, can realize the function that liquid chromatography hyperchannel luminosity detects, and can be used as liquid chromatography hyperchannel luminosity detecting device and uses; In the time adopting floating cuvette and microsyringe sample introduction, can realize the function of the mobile colorimetric measurement of trace.Incident ray is coupled to optical fiber 7 through collimation lens B6 again and transmits after cuvette device 4, see through after slit 8, adjust through collimating mirror 9, be projected to reflection grating 10 light splitting, the spectrum after light splitting is converted into digital signal output through linear array electrooptical device 11.In global design of the present invention, machinery-free switches and mobile device, and instrument control is transmitted by Computer signal, adopts rearmounted light splitting to make instrument have equally the performance that liquid chromatography multichannel detector is measured rapidly, continuously in conjunction with Array Design.
As converting with one of the present embodiment one, described collimation lens set 4134 can also comprise plural collimation lens, between described collimation lens A2 and cuvette device 4, also can not be connected by optical fiber 3.
As another conversion of embodiment mono-, described joint body 4251 can also adopt stainless steel material to make.