CN111796046A - Diode array detector for liquid chromatography - Google Patents
Diode array detector for liquid chromatography Download PDFInfo
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- CN111796046A CN111796046A CN202010766579.8A CN202010766579A CN111796046A CN 111796046 A CN111796046 A CN 111796046A CN 202010766579 A CN202010766579 A CN 202010766579A CN 111796046 A CN111796046 A CN 111796046A
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- slit
- speculum
- light source
- diode array
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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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
Abstract
The invention belongs to the technical field of liquid chromatogram analysis, and particularly relates to a diode array detector of a liquid chromatogram.A light path of a light source device sequentially passes through an M1 reflector, a flow cell, a first slit or a second slit, an M2 reflector, a grating and an M3 reflector and irradiates on a photodiode array. The light beam of the light source of the invention passes through the M1 reflector, the flow cell and the slit plate, is dispersed on the surface of the grating and is transmitted on the photodiode array, so as to obtain the spectrum of the component to be detected and various qualitative and quantitative data, and meet the requirements of holographic detection; in addition, the second slit is provided with a filter, and the slit plate is rotated by a motor, so that the position exchange of the combination of the first slit, the second slit and the filter is realized, and the wavelength calibration work of the detector is realized. Thus, the accuracy and integrity of the liquid chromatography system as a whole is improved.
Description
Technical Field
The invention belongs to the technical field of liquid chromatogram analysis, and particularly relates to a diode array detector for liquid chromatogram.
Background
The high performance liquid chromatography is also called high pressure liquid chromatography, high speed liquid chromatography, high resolution liquid chromatography, modern column chromatography and the like. High performance liquid chromatography is an important branch of chromatography, liquid is used as a mobile phase, a high-pressure infusion system is adopted, mobile phases such as single solvents with different polarities or mixed solvents, buffer solutions and the like with different proportions are pumped into a chromatographic column filled with a stationary phase, and after components in the column are separated, the mobile phases enter a detector for detection, so that analysis of a sample is realized. The method becomes an important separation and analysis technology in the subject fields of chemistry, medicine, industry, agriculture, commodity inspection, law inspection and the like.
Most common organic substances and part of inorganic substances have ultraviolet or visible light absorption groups and thus have stronger ultraviolet or visible light absorption capacity, and the ultraviolet-visible light detector of the liquid chromatograph is based on the principle, and the content of each component in the sample flowing through the flow cell is determined by measuring the absorption value of the sample to light with a specific wavelength. Since a common dispersive uv-vis detector can only detect light intensity at one wavelength at a time, only one species concentration in a sample can be detected at a time. The spectrum and various qualitative and quantitative data of the detected components cannot be provided, and the requirements of holographic detection cannot be met.
Disclosure of Invention
The invention aims to solve the problems, and provides a diode array detector for liquid chromatography, which aims to solve the technical problems that the common dispersive ultraviolet-visible light detector in the prior art can only detect the light intensity of one wavelength at a time, so that the concentration of only one substance in a sample can be detected at a time, the spectrum and various qualitative and quantitative data of a component to be detected cannot be given, and the requirement of holographic detection cannot be met.
The invention provides a diode array detector of liquid chromatogram, which has the following specific technical scheme:
liquid chromatogram's diode array detector, including the mainframe box, the mainframe box is the camera bellows, install light source device, M1 speculum, flow cell, slit board, M2 speculum, grating, M3 speculum, photodiode array in the mainframe box, the slit board passes through the motor and rotates the setting, first slit and second slit have been seted up on the slit board, the light filter is installed to second slit below, first slit or second slit are aimed at the focus of M1 speculum, M2 speculum focus, first slit or second slit are aimed at the focus of M1 speculum, M2 speculum focus, the grating is fixed to be set up, first slit or second slit are located the focus of M1 speculum and the straight line in place of M2 speculum focus, the light path of light source device passes through in proper order the M1 speculum, flow cell, light source device, M1 speculum, flow cell, light source, slit, light source, The first slit or the second slit, the M2 mirror, the grating, and the M3 mirror impinge on the photodiode array.
In some embodiments, the light source device includes a darkroom box, a light source outlet is arranged at one side of the darkroom box, a quartz lens is arranged on the light source outlet, a tungsten lamp, a lens and a deuterium lamp are fixedly arranged in the darkroom box, the lens is arranged between the tungsten lamp and the deuterium lamp, and the tungsten lamp, the optical center of the lens, the light through hole of the deuterium lamp and the light source outlet are all located on the same horizontal line.
In some embodiments, the system further comprises a heat dissipation fan disposed toward the dark room box.
In some embodiments, the refrigerator further comprises a controller and a temperature sensor, wherein the temperature sensor is installed in the darkroom box, and the heat dissipation fan and the temperature sensor are electrically connected with the controller.
In some embodiments, the slit plate further has a third slit and a fourth slit, the first slit, the second slit, the third slit and the fourth slit are uniformly distributed on the slit plate, the first slit and the second slit have the same width, and the second slit, the third slit and the fourth slit have different widths.
In certain embodiments, the sample channel of the flow cell is aligned with the focal point of the M1 mirror.
In some embodiments, the filter is a holmium glass filter.
In certain embodiments, the motor is a precision motor.
The invention has the following beneficial effects: in the diode array detector for liquid chromatography provided by the invention, the light path of the light source device sequentially passes through the M1 reflector, the flow cell, the first slit or the second slit, the M2 reflector, the grating and the M3 reflector to irradiate on the photodiode array. The light beam of the light source of the invention passes through the M1 reflector, the flow cell and the slit plate, is dispersed on the surface of the grating and is transmitted on the photodiode array, so as to obtain the spectrum of the component to be detected and various qualitative and quantitative data, and meet the requirements of holographic detection; in addition, the second slit is provided with a filter, and the slit plate is rotated by a motor, so that the position exchange of the combination of the first slit, the second slit and the filter is realized, and the wavelength calibration work of the detector is realized. Thus, the accuracy and integrity of the liquid chromatography system as a whole is improved.
Drawings
FIG. 1 is a schematic diagram of an optical path system of a diode array detector for liquid chromatography provided by the present invention;
FIG. 2 is a schematic plan view of the slit plate according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings 1-2 in conjunction with specific embodiments.
The invention provides a diode array detector of liquid chromatogram, which has the following specific technical scheme:
a liquid chromatogram diode array detector comprises a main case, wherein a light source device 1, an M1 reflector 2, a flow cell 3, a slit plate 4, an M2 reflector 5, a grating 6, an M3 reflector 7 and a photodiode array 8 are arranged in the main case, the slit plate 4 is rotationally arranged through a motor 9, a first slit 41 and a second slit 42 are arranged on the slit plate 4, an optical filter 43 is arranged below the second slit 42, the first slit 41 or the second slit 42 is aligned with a focus of the M1 reflector 2 and a focus of the M2 reflector 5, the first slit 41 or the second slit 42 is aligned with a focus of the M1 reflector 2 and a focus of the M2 reflector 5, the grating 6 is fixedly arranged, the first slit 41 or the second slit 42 is positioned on a straight line where the focus of the M1 reflector 2 and the focus of the M2 reflector 5 are positioned, and a light path of the light source device 1 sequentially passes through the M1 reflector 2, the flow cell 3, the first slit 41 or the second slit 42, The M2 mirror 5, grating 6, and M3 mirror 7 illuminate onto the photodiode array 8. The light source device 1 emits a light source to an M1 reflecting mirror 2, then the light source is imaged and converged to an M2 reflecting mirror 5 through a flow cell 3 and a first slit 41 on a slit plate 4, wherein the slit plate 4 is switched to a combination of a second slit 42 and holmium glass through rotation of a first motor 9, the combination of the second slit 42 and the holmium glass can be used for wavelength calibration, the transmitted light M2 reflecting mirror 5 is reflected to a grating 6, dispersion is carried out on the surface of the grating 6, and the obtained monochromatic light is irradiated to a photodiode array through an M3 reflecting mirror 7.
In some embodiments, the light source apparatus 1 includes a darkroom box 11, a light source outlet 111 is disposed at one side of the darkroom box 11, a quartz lens 112 is mounted on the light source outlet 111, a tungsten lamp 12, a lens 13 and a deuterium lamp 14 are fixedly mounted in the darkroom box 11, the lens 13 is disposed between the tungsten lamp 12 and the deuterium lamp 14, and the light centers of the tungsten lamp 12 and the lens 13, the light-passing hole of the deuterium lamp 14 and the light source outlet 111 are all located on the same horizontal line. The invention adopts the back-transparent deuterium lamp 14, the use wave band range of the tungsten lamp 12 is between 400-900nm, the use wavelength range of the deuterium lamp 14 is between 200-600nm, the light emitted by the tungsten lamp 12 is converged to the light through hole of the deuterium lamp 14 through the lens 13 of the tungsten lamp 12, and the tungsten lamp 12 and the deuterium lamp 14 are emitted to the M1 reflector 2 through the quartz lens 13112.
In some embodiments, a heat dissipation fan 15 is further included, the heat dissipation fan 15 being disposed toward the dark room box 11. The light source device 1 easily generates high heat, and the light source device 1 is cooled and reduced in heat by the aid of the cooling fan 15, so that the overall stability of the detector is guaranteed, and the stability of a liquid chromatography system is further maintained.
In some embodiments, the system further comprises a controller (the controller can adopt any type of existing single chip microcomputer) and a temperature sensor, the temperature sensor is installed in the darkroom box 11, and the cooling fan 15 and the temperature sensor are electrically connected with the controller. The deuterium lamp 14 needs to be preheated for a certain time to be stable, the heat dissipation fan 15 is not started when the deuterium lamp is started, when the temperature sensor detects that the temperature in the darkroom box 11 reaches a set value, the controller receives a signal transmitted by the temperature sensor to control the heat dissipation fan 15 to rotate, and the speed of the heat dissipation fan 15 can be regulated through the controller, so that the temperature of the darkroom box 11 provided with the deuterium lamp 14 can be controlled within a required range, the stability of a light source is further realized, and the stability of the signal is further ensured.
In some embodiments, the slit plate 4 further has a third slit and a fourth slit, the first slit 41, the second slit 42, the third slit and the fourth slit are uniformly distributed on the slit plate 4, the widths of the first slit 41 and the second slit 42 are the same, and the widths of the second slit 42, the third slit and the fourth slit are different from each other. In this way, the slit plate 4 can be rotated by the first motor 9, the first slit 41, the second slit 42, the third slit or the fourth slit can be freely switched to align with the M1 reflector 2, and the transmitted light path is received, so that the slit-adjustable effect can be realized, and the light resolution precision can be improved.
In some embodiments, the sample channel of the flow cell 3 is aligned with the focus of the M1 mirror 2.
In some embodiments, the filter 43 is a holmium glass filter 43. The characteristic signal of deuterium lamp 14 is found from the scanned data, and then calibration and correction of wavelength are performed to ensure wavelength accuracy. The detector can detect two characteristic spectra of the deuterium lamp 14 without using holmium glass, the wavelengths of the two characteristic spectra are known, and thus the positioning of the wavelengths further realizes the calibration of the wavelengths; filter 43 is holmium glass filter 43 can filter some stray light, and the detector can see the other two characteristic spectra of deuterium lamp 14, so that the four characteristic spectra are obtained by adding the two characteristic spectra in the absence of holmium glass, and the four characteristic spectra are more accurately positioned than the two characteristic spectra.
In some embodiments, the motor 9 is a precision motor 9. This can improve the rotational accuracy of the slit plate 4.
The above description is only for the purpose of illustrating preferred embodiments of the present invention and is not to be construed as limiting the invention, and the present invention is not limited to the above examples, and those skilled in the art should also be able to make various changes, modifications, additions or substitutions within the spirit and scope of the present invention.
Claims (8)
1. Diode array detector of liquid chromatogram, its characterized in that, including the mainframe box, the mainframe box is the camera bellows, install light source device, M1 speculum, flow-through cell, slit board, M2 speculum, grating, M3 speculum, photodiode array in the mainframe box, the slit board passes through the motor and rotates the setting, first slit and second slit have been seted up on the slit board, the light filter is installed to second slit below, first slit or second slit are aimed at the focus of M1 speculum, M2 speculum focus, first slit or second slit are aimed at the focus of M1 speculum the M2 speculum focus, the grating is fixed to be set up, first slit or second slit are located the focus of M1 speculum and the straight line of the place of M2 speculum focus, the light path of light source device passes through in proper order the M1 speculum, The flow cell, the first slit or the second slit, the M2 mirror, the grating, and the M3 mirror impinge on the photodiode array.
2. The diode array detector of liquid chromatogram of claim 1, wherein said light source device comprises a darkroom box, one side of said darkroom box is provided with a light source outlet, a quartz lens is installed on said light source outlet, a tungsten lamp, a lens and a deuterium lamp are fixedly installed in said darkroom box, said lens is arranged between said tungsten lamp and said deuterium lamp, and said tungsten lamp, the optical center of said lens, the light-passing hole of said deuterium lamp and said light source outlet are all located on the same horizontal line.
3. The diode array detector of liquid chromatography of claim 2, further comprising a heat sink fan disposed toward the dark room box.
4. The diode array detector of liquid chromatography of claim 3, further comprising a controller and a temperature sensor, wherein the temperature sensor is mounted in the darkroom box, and the cooling fan and the temperature sensor are both in electrical control connection with the controller.
5. The diode array detector of claim 1, wherein the slit plate further comprises a third slit and a fourth slit, the first slit, the second slit, the third slit and the fourth slit are uniformly distributed on the slit plate, the first slit and the second slit have the same width, and the second slit, the third slit and the fourth slit have different widths.
6. The diode array detector of claim 1, wherein the sample channel of the flow cell is aligned with the focal point of the M1 mirror.
7. The uv-vis detector of liquid chromatography according to claim 1, wherein the filter is a holmium glass filter.
8. The uv-vis detector of liquid chromatography as claimed in claim 1, wherein the motor is a precision motor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010766579.8A CN111796046A (en) | 2020-08-03 | 2020-08-03 | Diode array detector for liquid chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010766579.8A CN111796046A (en) | 2020-08-03 | 2020-08-03 | Diode array detector for liquid chromatography |
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| Publication Number | Publication Date |
|---|---|
| CN111796046A true CN111796046A (en) | 2020-10-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010766579.8A Pending CN111796046A (en) | 2020-08-03 | 2020-08-03 | Diode array detector for liquid chromatography |
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| CN (1) | CN111796046A (en) |
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2020
- 2020-08-03 CN CN202010766579.8A patent/CN111796046A/en active Pending
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