WO2021044704A1 - クロマトグラフ用分光光度計および基準位置検出方法 - Google Patents

クロマトグラフ用分光光度計および基準位置検出方法 Download PDF

Info

Publication number
WO2021044704A1
WO2021044704A1 PCT/JP2020/023847 JP2020023847W WO2021044704A1 WO 2021044704 A1 WO2021044704 A1 WO 2021044704A1 JP 2020023847 W JP2020023847 W JP 2020023847W WO 2021044704 A1 WO2021044704 A1 WO 2021044704A1
Authority
WO
WIPO (PCT)
Prior art keywords
light
angle
diffraction grating
reference position
motor
Prior art date
Application number
PCT/JP2020/023847
Other languages
English (en)
French (fr)
Japanese (ja)
Inventor
優子 重里
真二 辻
Original Assignee
株式会社島津製作所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to JP2021543964A priority Critical patent/JP7616054B2/ja
Publication of WO2021044704A1 publication Critical patent/WO2021044704A1/ja

Links

Images

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/02—Details
    • G01J3/06—Scanning arrangements arrangements for order-selection
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/12—Generating the spectrum; Monochromators
    • G01J3/18—Generating the spectrum; Monochromators using diffraction elements, e.g. grating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/28—Investigating the spectrum
    • G01J3/30—Measuring the intensity of spectral lines directly on the spectrum itself
    • G01J3/32—Investigating bands of a spectrum in sequence by a single detector
    • 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

Definitions

  • the present invention relates to a spectrophotometer for a chromatograph and a reference position detection method.
  • a spectrophotometer is used, for example, in a liquid chromatograph to detect the components of a sample separated by an analytical column.
  • the spectrophotometer includes a light source, a diffraction grating, a flow cell and a photodetector.
  • the light generated by the light source is dispersed by a diffraction grating into a plurality of lights having different wavelengths.
  • a diffraction grating into a plurality of lights having different wavelengths.
  • light having a specific wavelength is guided to the flow cell.
  • the light transmitted through the flow cell is detected by a photodetector.
  • the appropriate wavelength differs depending on the sample to be analyzed. Therefore, the angle of the diffraction grating is adjusted by the motor, so that light having a wavelength suitable for sample analysis is incident on the flow cell.
  • the wavelength of light guided to the flow cell by the diffraction grating when the diffraction grating is at a predetermined reference angle (hereinafter referred to as a reference position) is known.
  • the relationship between the rotation angle of the diffraction grating from the reference position and the wavelength of the light incident on the flow cell is also known. Therefore, by adjusting the rotation angle of the diffraction grating from the reference position, light of a desired wavelength can be guided to the flow cell.
  • the rotation axis of the motor stops at an arbitrary angle. Therefore, the diffraction grating does not always stop at the reference position.
  • a home position sensor for detecting that the diffraction grating is in the home position is provided in the vicinity of the diffraction grating (grating).
  • the home position sensor is, for example, a microswitch.
  • the motor rotates the grating by a constant pulse until the home position sensor detects that the grating is in the home position. After that, the motor rotates the diffraction grating in the opposite direction by a predetermined pulse.
  • the motor rotates the grating by one pulse until the home position sensor detects that the grating is in the home position. JP-A-2018-13412
  • the spectrophotometer described in Patent Document 1 requires a home position sensor in order to position the diffraction grating at the home position.
  • a protrusion is provided on the mounting member of the diffraction grating, and a photo interrupter for detecting the protrusion may be used as the home position sensor. In these cases, the cost of parts for the home position sensor is required, and the manufacturing cost for mounting the home position sensor is required.
  • An object of the present invention is to provide a spectrophotometer and a reference position detection method capable of reducing the cost for detecting a reference position of a diffraction grating.
  • the spectrophotometer for chromatograph includes a light source, a diffraction grid that disperses the light generated by the light source into light having a plurality of different wavelengths, a motor that changes the angle of the diffraction grid, and the above.
  • a sample cell that receives light of one of a plurality of wavelengths dispersed by a diffraction grid, a light detector that detects light transmitted through the sample cell, and a light receiving amount of the light detector are predetermined.
  • the motor is rotated in the first direction by a first angle until the threshold value is exceeded, and after the amount of light received by the light detector is equal to or higher than the threshold value, the motor is moved to the first position.
  • the rotation angle of the motor in which the peak of the light receiving amount of the light detector appears by rotating by a second angle smaller than the angle is detected, and the rotation angle corresponds to the reference angle of the diffraction grid based on the detected rotation angle. It is provided with a reference position detecting unit for detecting a reference position to be used.
  • the reference position detection method is a reference position detection method for detecting a reference position corresponding to a reference angle of a diffraction grating in a spectrophotometer, and the spectrophotometer generates light by a light source.
  • the light generated by the light source is dispersed by a diffraction grating into light having a plurality of different wavelengths, and the light having one of the dispersed wavelengths is guided to the light detector through the sample cell.
  • the step, the step of rotating the diffraction grating in the first direction by a first angle until the light receiving amount of the light detector becomes equal to or higher than a predetermined threshold value, and the light receiving amount of the light detector are described.
  • the diffraction grating is rotated by a second angle smaller than the first angle to detect the rotation angle of the diffraction grating at which the peak of the light receiving amount of the light detector appears.
  • the step includes a step of detecting the reference position based on the detected rotation angle.
  • the present invention it is possible to reduce the cost for detecting the reference position of the diffraction grating in the spectrophotometer.
  • FIG. 1 is a block diagram showing a configuration of a spectrophotometer for a chromatograph according to an embodiment.
  • FIG. 2 is a schematic view showing the configuration of a diffraction grating.
  • FIG. 3 is a block diagram showing a functional configuration of the detector control unit of FIG.
  • FIG. 4 is a flowchart showing a reference position detection method according to the embodiment.
  • FIG. 5 is a diagram showing an example of a change in the amount of light received by the photodetector depending on the number of control pulses given to the motor.
  • FIG. 6 is an enlarged view of part A in FIG.
  • FIG. 7 is a block diagram showing the configuration of a liquid chromatograph including the spectrophotometer of FIG.
  • FIG. 1 is a block diagram showing a configuration of a spectrophotometer for a chromatograph according to an embodiment.
  • the spectrophotometer according to this embodiment is used, for example, in a liquid chromatograph.
  • the spectrophotometer 10 of FIG. 1 includes a light source 11, a dimming filter 12, a diffraction grating 13, a flow cell 14, a photodetector 15, a motor 16, and a detector control unit 30.
  • the light source 11 is, for example, a deuterium lamp.
  • the motor 16 rotates the diffraction grating 13.
  • the spectrophotometer 10 performs a reference position detection operation and a normal operation.
  • the reference position refers to the angle of the diffraction grating 13 such that light having a predetermined wavelength is guided to the photodetector 15 through the flow cell 14.
  • the reference position of the diffraction grating 13 is defined as the angle of the diffraction grating 13 when the 0th-order light reflected by the diffraction grating 13 enters the photodetector 15 through the flow cell 14.
  • the light generated by the light source 11 is attenuated by passing through the dimming filter 12.
  • the attenuated light is guided to the diffraction grating 13 by an optical system (not shown) such as a mirror.
  • the mechanism for attenuating light is not limited to the dimming filter 12, and other members or devices may be used.
  • the dimming filter 12 may not be provided.
  • the light generated by the light source 11 is guided to the diffraction grating 13 by the optical system without passing through the dimming filter 12.
  • the diffraction grating 13 reflects the incident light so as to disperse it into light having a plurality of wavelengths.
  • the light of a plurality of wavelengths reflected by the diffraction grating 13 is reflected at different angles.
  • the 0th order light from the diffraction grating 13 includes light having a plurality of wavelengths. Therefore, the intensity of the 0th-order light is higher than the intensity of light of any wavelength.
  • the flow cell 14 is an example of a sample cell.
  • the wavelength of the light guided to the flow cell 14 changes according to the angle of the diffraction grating 13.
  • the light transmitted through the flow cell 14 is guided to the photodetector 15.
  • the photodetector 15 includes, for example, a photodiode and detects the intensity of incident light. The intensity of light detected by the photodetector 15 is equivalent to the amount of light received by the photodetector 15.
  • the wavelength of light suitable for analysis differs depending on the type of sample. Therefore, it is necessary to adjust the angle of the diffraction grating 13 so that light having a wavelength suitable for sample analysis enters the photodetector 15 through the flow cell 14.
  • the detector control unit 30 includes an input / output I / F (interface) 31, a CPU (central processing unit) 32, a RAM (random access memory) 33, a ROM (read-only memory) 34, and a storage device 35.
  • the input / output I / F 31, CPU 32, RAM 33, ROM 34, and storage device 35 are connected to the bus 38.
  • the storage device 35 includes a storage medium such as a semiconductor memory or a memory card, and stores a detector control program.
  • the RAM 33 is used as a work area of the CPU 32.
  • the system program is stored in the ROM 34.
  • the CPU 32 controls the light source 11, the dimming filter 12, and the motor 16 through the input / output I / F 31 by executing the detector control program stored in the storage device 35 on the RAM 33, and outputs the output signal of the photodetector 15. Received through input / output I / F31.
  • the detector control program also includes a reference position detection program. The reference position detection method described later is implemented by the CPU 32 executing the reference position detection program stored in the storage device 35 on the RAM 33.
  • the input / output I / F 31 is connected to, for example, the analysis control unit 50 (FIG. 7) of the liquid chromatograph.
  • FIG. 2 is a schematic diagram showing the configuration of the diffraction grating.
  • the diffraction grating 13 has a diffraction grating reflecting surface 13a.
  • the diffraction grating 13 is attached to the rotating shaft 16a of the motor 16 by the attachment member 13b.
  • the motor 16 is a stepping motor.
  • the detector control unit 30 of FIG. 1 gives a pulse signal including a control pulse and a rotation direction instruction signal indicating a rotation direction to the motor 16. Each time a control pulse is given to the motor 16, the rotation shaft 16a rotates by a constant angle in the direction indicated by the rotation direction instruction signal.
  • one control pulse corresponds to a constant rotation angle of the motor 16.
  • the rotation angle of the motor 16 per one control pulse is 0.009 degrees.
  • the angle of the diffraction grating 13 usually does not match the reference position. In this case, it is necessary to detect the angle of the diffraction grating 13 with respect to the reference position when the power of the spectrophotometer 10 is turned off. For that purpose, it is necessary to detect the reference position with respect to the initial state of the diffraction grating 13 when the power is turned on.
  • the relationship between the angle of the diffraction grating 13 with respect to the reference position and the wavelength of the light incident on the photodetector 15 is known.
  • the angle of the diffraction grating 13 can be set so as to guide the light having a desired wavelength according to the sample to the photodetector 15 through the flow cell 14.
  • the reference position of the diffraction grating 13 is detected by the reference position detection operation before the normal operation.
  • FIG. 3 is a block diagram showing a functional configuration of the detector control unit of FIG.
  • the detector control unit 30 includes a light source drive unit 301, a motor drive unit 302, a light receiving amount acquisition unit 303, a storage unit 304, a reference position detection unit 305, an operation switching unit 306, and a normal operation control unit 307. including.
  • the functions of the above components (301 to 307) are realized by the CPU 32 of FIG. 1 executing a detector control program which is a computer program stored in a storage medium (recording medium) such as a storage device.
  • a part or all the components of the detector control unit 30 may be realized by hardware such as an electronic circuit.
  • the light source driving unit 301 turns the light source 11 on and off.
  • the motor drive unit 302 gives the motor 16 a pulse signal including a control pulse and a direction indicating signal instructing the rotation direction in order to rotate the motor 16 in the forward direction or the reverse direction.
  • the light receiving amount acquisition unit 303 acquires the light receiving amount of the photodetector 15 based on the output signal of the photodetector 15, and also acquires the pulse signal and the direction indicating signal from the motor drive unit 302. Further, the light receiving amount acquisition unit 303 integrates the number of control pulses included in the pulse signal. In this case, the light receiving amount acquisition unit 303 adds the number of control pulses included in the pulse signal when the rotation direction indicated by the direction indicating signal is the positive direction.
  • the number of control pulses included in the pulse signal is subtracted.
  • the relationship between the number of control pulses and the amount of received light can be obtained.
  • the change in the amount of received light according to the change in the number of control pulses is sequentially stored in the storage unit 304.
  • the reference position detection unit 305 controls the motor drive unit 302 and detects the reference position of the diffraction grating 13 based on the change in the amount of light received stored in the storage unit 304. The details of the reference position detection method will be described later.
  • the operation switching unit 306 switches between the reference position detection operation and the normal operation. Further, the operation switching unit 306 inserts the dimming filter 12 into the optical path between the light source 11 and the diffraction grating 13 during the reference position detection operation, and inserts the dimming filter 12 between the light source 11 and the diffraction grating 13 during normal operation. Exclude from the optical path of. When the amount of light of the light source 11 is small, the dimming filter 12 may not be provided.
  • the normal operation control unit 307 adjusts the angle of the diffraction grating 13 from the reference position by controlling the motor 16 based on the reference position stored in the storage unit 304. In this case, the normal operation control unit 307 adjusts the angle of the diffraction grating 13 so that the light having the wavelength corresponding to the sample is guided to the photodetector 15 through the flow cell 14.
  • FIG. 4 is a flowchart showing a reference position detection method according to the embodiment.
  • FIG. 5 is a diagram showing an example of a change in the amount of light received by the photodetector 15 depending on the number of control pulses given to the motor 16.
  • FIG. 6 is an enlarged view of part A in FIG.
  • the vertical axis of FIGS. 5 and 6 shows the amount of light received by the photodetector 15, and the horizontal axis shows the number of control pulses given to the motor 16.
  • the number of control pulses in FIGS. 5 and 6 is added when the motor 16 rotates in the forward direction and subtracted when the motor 16 rotates in the opposite direction. As shown in FIGS.
  • the threshold value Th for detecting the peak of the 0th order light is set in advance.
  • the threshold value Th is smaller than the peak value (maximum value) of the received amount of the 0th-order light guided from the diffraction grating 13 to the photodetector 15 through the flow cell 14, and the threshold value Th is of light other than the 0th-order light. It is set larger than the amount of light received.
  • the reference position detection method of FIG. 4 is carried out by executing the reference position detection program.
  • the operation switching unit 306 determines whether or not the power of the spectrophotometer 10 is turned on (step S1). When the power is turned on, the light source driving unit 301 turns on the light source 11 (step S2). In this state, the operation switching unit 306 instructs the reference position detection unit 305 to perform the reference position detection operation, and inserts the dimming filter 12 into the optical path in the optical path between the light source 11 and the diffraction grating 13 (Ste S3).
  • the motor drive unit 302 applies M control pulses to the motor 16 to rotate the diffraction grating 13 in the positive direction by a first angle (step S4).
  • M is, for example, 20.
  • the control pulse number M is set so that the first angle is smaller than the width of the peak of the 0th-order light at the intersection of the peak of the 0th-order light and the threshold value Th.
  • the light receiving amount acquisition unit 303 acquires the light receiving amount of the photodetector 15 based on the output signal of the photodetector 15 (step S5).
  • the light-receiving amount acquired by the light-receiving amount acquisition unit 303 is stored in the storage unit 304.
  • the reference position detection unit 305 determines whether or not the amount of light received stored in the storage unit 304 is equal to or greater than a preset threshold value Th (step S6).
  • Th the motor drive unit 302 returns to step S4 and applies M control pulses to the motor 16 to make the diffraction grating 13 a first angle in the positive direction. Rotate.
  • steps S4 to S6 are repeated until the amount of received light becomes equal to or higher than the threshold value Th.
  • the coarse adjustment of the diffraction grating 13 is performed so that the angle of the diffraction grating 13 approaches the reference position.
  • the motor drive unit 302 applies K control pulses to the motor 16 to rotate the diffraction grating 13 by a third angle in the opposite direction (Ste S7).
  • the number of K is, for example, half of M, and 10 in this example.
  • the amount of light received when the diffraction grating 13 is rotated in the positive direction by an angle corresponding to the control pulse number P1 from the initial state is the threshold value Th or more.
  • the rotation angle of the diffraction grating 13 exceeds the angle at which the light receiving amount reaches the peak value.
  • the diffraction grating 13 returns from the angle corresponding to the control pulse number P1 in the opposite direction by the angle corresponding to the control pulse number K.
  • the angle of the diffraction grating 13 becomes an angle corresponding to the control pulse number P2 from the initial state.
  • the rotation angle of the diffraction grating 13 is smaller than the angle at which the light receiving amount reaches the peak value.
  • N is smaller than M and K, for example 1.
  • the light receiving amount acquisition unit 303 acquires the light receiving amount of the photodetector 15 based on the output signal of the photodetector 15 (step S9).
  • the light-receiving amount acquired by the light-receiving amount acquisition unit 303 is stored in the storage unit 304.
  • the reference position detection unit 305 determines whether or not the peak value of the received light amount stored in the storage unit 304 has been detected (step S10).
  • the motor driving unit 302 returns to step S8 and applies N control pulses to the motor 16 to further rotate the diffraction grating 13 in the positive direction by a second angle.
  • the processes of steps S8 to S10 are repeated until the peak value of the received light amount is detected.
  • control pulses are given to the motor 16 one by one from a state where the angle of the diffraction grating 13 is an angle corresponding to the number of control pulses P2, and the diffraction grating 13 rotates by a third angle.
  • the amount of light received gradually increases, and when the angle of the diffraction grating 13 is an angle corresponding to the number of control pulses P3, the amount of light received becomes the peak value (maximum value) Pe.
  • the amount of light received decreases when the angle of the diffraction grating 13 is rotated to an angle corresponding to the number of control pulses P4.
  • the received light amount reaches the peak value Pe at the angle corresponding to the control pulse number P3 before the angle corresponding to the control pulse number P4.
  • the method for determining whether or not the peak value Pe of the received light amount is detected is not limited to the above method, and other methods may be used.
  • the reference position detection unit 305 stores the number of control pulses corresponding to the peak value of the received light amount in the storage unit 304 as the reference position (step S11).
  • the control pulse number P3 is stored in the storage unit 304 as a reference position. The control pulse corresponding to the reference position is accurately detected by the processing of steps S8 to S10.
  • the operation switching unit 306 instructs the normal operation control unit 307 to perform the normal operation.
  • the storage unit 304 stores in advance the relationship between the rotation angle of the diffraction grating 13 from the reference position and the wavelength.
  • the number of control pulses given to the motor 16 after the power of the spectrophotometer is turned on is normally given to the operation control unit 307.
  • the normal operation control unit 307 calculates, for example, the difference between the number of control pulses given to the motor 16 and the number of control pulses corresponding to the reference position, and the difference in the number of control pulses corresponds to the wavelength specified according to the sample.
  • the motor 16 is rotated by the motor drive unit 302 so as to do so. As a result, among the light generated by the light source 11, light having a specified wavelength is guided to the photodetector 15 through the flow cell 14.
  • FIG. 7 is a block diagram showing the configuration of a liquid chromatograph including the spectrophotometer 10 of FIG.
  • the liquid chromatograph 100 of FIG. 7 includes a pump 110 for a mobile phase, a sample introduction unit 120, an introduction port 130, an analysis column 140, a column oven 150, and a spectrophotometer 10.
  • the analysis column 140 is provided in the column oven 150.
  • the column oven 150 maintains the analytical column 140 at a set temperature.
  • the pump 110 sucks the mobile phase (eluent) in the mobile phase container 111 and supplies it to the analysis column 140.
  • the sample introduction unit 120 includes, for example, an autosampler or an injector, and introduces the sample to be analyzed into the mobile phase at the introduction port 130.
  • the mobile phase and the sample that have passed through the analysis column 140 flow through the flow cell 14 (see FIG. 1) of the spectrophotometer 10, and are discharged to the waste liquid container 112.
  • the liquid chromatograph 100 includes an analysis control unit 50, an operation unit 51, and a display unit 52.
  • the operation unit 51 is used by the user to give various commands to the analysis control unit 50.
  • the analysis control unit 50 controls the pump 110, the sample introduction unit 120, the column oven 150, and the spectrophotometer 10. Further, the analysis control unit 50 generates a chromatogram based on the output signal of the spectrophotometer 10. The generated chromatogram is displayed on the display unit 52.
  • the motor 16 when the light receiving amount of the photodetector 15 becomes the threshold value Th or more, the motor 16 is rotated in the opposite direction by a third angle. Therefore, even when the first angle is set to be relatively large, it is possible to detect the rotation angle of the motor 16 in which the peak value of the light receiving amount of the photodetector 15 appears. As a result, the reference position of the diffraction grating 13 can be detected in a short time.
  • the reference position of the diffraction grating 13 can be detected more accurately based on the amount of received 0th-order light having the highest intensity.
  • the first angle is set to be smaller than the angle corresponding to the peak width at the intersection of the peak of the 0th-order light guided from the diffraction grating 13 to the photodetector 15 through the flow cell 14 and the threshold value Th.
  • the angle at which the received light amount is equal to or higher than the threshold value Th is not detected, it is not necessary to perform processing such as resetting the first angle to a small value. As a result, the reference position of the diffraction grating 13 can be reliably detected in a short time.
  • the angle of the diffraction grating 13 corresponding to the number of control pulses in which the peak of the 0th order light from the diffraction grating 13 appears is detected as the reference position, but this is the reference position. Not limited to.
  • the angle of the diffraction grating 13 at which the peak of a specific wavelength obtained when the diffraction grating 13 is rotated may appear may be detected as the reference position.
  • the motor 16 is rotated in the reverse direction of the third angle when the light receiving amount of the photodetector 15 becomes equal to or higher than the threshold value Th due to the rotation of the motor 16 in the forward direction by the first angle.
  • the motor 16 it is not always necessary for the motor 16 to be rotated in the opposite direction by a third angle.
  • the angle of the diffraction grating 13 may not exceed the angle corresponding to the peak value due to the rotation of the motor 16 in the positive direction of the first angle.
  • the motor 16 may not be rotated in the reverse direction and the diffraction grating 13 may be finely adjusted.
  • the threshold value Th is set to be smaller than the maximum value of the received amount of the 0th-order light and larger than the received amount of the 0th-order light, but the threshold value Th is not limited to this.
  • the threshold value Th is larger than the peak value of the received amount of light having a specific wavelength. It may be set to be smaller and larger than the amount of received light having other wavelengths.
  • the number of control pulses M corresponding to the first angle is set to be smaller than the number of control pulses corresponding to the peak width at the intersection of the peak of the amount of received light of the 0th order light and the threshold value Th.
  • the control pulse number M is not limited to this.
  • the control pulse number M is initially set large, and when the diffraction grating 13 is rotating within a certain angle range, the control pulse number M is reduced when the received light amount does not exceed the threshold value Th. Processing may be performed.
  • the motor 16 may be rotated once during the reference position detection operation, or may be rotated within a predetermined angle range. Further, a mechanism using a motor, a belt and a pulley may be used to rotate the diffraction grating 13.
  • the spectrophotometer 10 is used for the liquid chromatograph 100, but the spectrophotometer 10 may be used for other chromatographs such as a supercritical chromatograph.
  • the light source 11 is a deuterium lamp, but the light source 11 may be another lamp such as a tungsten lamp or another light emitting element such as a light emitting diode.
  • the spectrophotometer for chromatograph is Light source and A diffraction grating that disperses the light generated by the light source into light of a plurality of different wavelengths, A motor that changes the angle of the diffraction grating and A sample cell that receives light of one of a plurality of wavelengths dispersed by the diffraction grating, and A photodetector that detects the light that passes through the sample cell, The motor is rotated in the first direction by a first angle until the light receiving amount of the light detector becomes equal to or higher than a predetermined threshold value, and the light receiving amount of the light detector becomes equal to or higher than the threshold value.
  • a reference position detecting unit for detecting a reference position corresponding to the reference angle of the diffraction grid may be provided.
  • the motor is rotated in the first direction by a first angle until the amount of light received by the photodetector exceeds a predetermined threshold value.
  • the diffraction grating is adjusted close to the reference position in a short time.
  • the motor is rotated by a second angle smaller than the first angle, so that the rotation angle of the motor at which the peak of the light receiving amount of the photodetector appears is detected.
  • the reference position of the diffraction grating is accurately detected.
  • the reference position detection unit makes the motor smaller than the first angle and larger than the second angle by a third angle when the amount of light received by the photodetector exceeds the threshold value. After rotating in the second direction opposite to the first direction, the motor may be rotated by the second angle.
  • the spectrophotometer for chromatograph described in the second item, it is possible to detect the rotation angle of the motor in which the peak of the received light amount of the photodetector appears even when the first angle is set relatively large. It becomes. Thereby, the reference position can be detected in a shorter time.
  • the reference position of the diffraction grating can be detected more accurately based on the intensity of the 0th-order light having the highest intensity.
  • the first angle is the 0th order light guided from the diffraction grating to the photodetector through the sample cell. It may be smaller than the angle corresponding to the peak width at the intersection of the peak of the received light amount and the threshold value.
  • the amount of light received is limited between the time point before the rotation of the first angle of the diffraction grating and the time point after the rotation of the first angle of the diffraction grating.
  • the situation that exceeds the value does not occur.
  • the reference position detection method is a reference position detection method for detecting a reference position corresponding to a reference angle of a diffraction grating in a spectrophotometer.
  • the step of detecting the rotation angle of the diffraction grating and It may include a step of detecting the reference position based on the detected rotation angle.
  • the diffraction grating is rotated in the first direction by a first angle until the amount of light received by the photodetector becomes equal to or higher than a predetermined threshold value.
  • the diffraction grating is adjusted close to the reference position in a short time.
  • the diffraction grating is rotated by a second angle smaller than the first angle, so that the rotation angle of the diffraction grating at which the peak of the light receiving amount of the photodetector appears is detected.
  • the reference position of the diffraction grating is accurately detected.

Landscapes

  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Spectrometry And Color Measurement (AREA)
PCT/JP2020/023847 2019-09-02 2020-06-17 クロマトグラフ用分光光度計および基準位置検出方法 WO2021044704A1 (ja)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2021543964A JP7616054B2 (ja) 2019-09-02 2020-06-17 クロマトグラフ用分光光度計および基準位置検出方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2019-159791 2019-09-02
JP2019159791 2019-09-02

Publications (1)

Publication Number Publication Date
WO2021044704A1 true WO2021044704A1 (ja) 2021-03-11

Family

ID=74853158

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2020/023847 WO2021044704A1 (ja) 2019-09-02 2020-06-17 クロマトグラフ用分光光度計および基準位置検出方法

Country Status (2)

Country Link
JP (1) JP7616054B2 (enrdf_load_stackoverflow)
WO (1) WO2021044704A1 (enrdf_load_stackoverflow)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57142524A (en) * 1981-02-27 1982-09-03 Hitachi Ltd Measuring method and device for spectral luminous intensity
JPH02201124A (ja) * 1989-01-28 1990-08-09 Shimadzu Corp 分光光度計
JPH04290933A (ja) * 1991-03-19 1992-10-15 Hitachi Ltd 回折格子駆動装置
JPH10104068A (ja) * 1996-09-30 1998-04-24 Shimadzu Corp 分光分析装置
JP2000065641A (ja) * 1998-08-24 2000-03-03 Shimadzu Corp 分光光度計

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS56108923A (en) * 1980-01-31 1981-08-28 Norito Suzuki Sweep control method of luminous analyzing spectroscope using microcomputer
US4916645A (en) * 1988-06-02 1990-04-10 The Perkin-Elmer Corporation Continuous monochrometer drift compensation of a spectral monochromator
JPH08114538A (ja) * 1994-10-15 1996-05-07 Horiba Ltd 吸光度計
JP4533527B2 (ja) * 2000-12-05 2010-09-01 アンリツ株式会社 光スペクトラムアナライザおよびその波長校正方法
JP2008292249A (ja) * 2007-05-23 2008-12-04 Hitachi High-Tech Manufacturing & Service Corp 分光光度計

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57142524A (en) * 1981-02-27 1982-09-03 Hitachi Ltd Measuring method and device for spectral luminous intensity
JPH02201124A (ja) * 1989-01-28 1990-08-09 Shimadzu Corp 分光光度計
JPH04290933A (ja) * 1991-03-19 1992-10-15 Hitachi Ltd 回折格子駆動装置
JPH10104068A (ja) * 1996-09-30 1998-04-24 Shimadzu Corp 分光分析装置
JP2000065641A (ja) * 1998-08-24 2000-03-03 Shimadzu Corp 分光光度計

Also Published As

Publication number Publication date
JP7616054B2 (ja) 2025-01-17
JPWO2021044704A1 (enrdf_load_stackoverflow) 2021-03-11

Similar Documents

Publication Publication Date Title
JP6549832B2 (ja) ダイクロイック・ビームコンバイナおよびスプリッタを含む光学吸収分光システム
US20090153855A1 (en) Spectrophotometer
EP1380329B1 (en) Preparative liquid chromatograph using plural detectors
US10816398B2 (en) Spectrometer and spectrum measurement method thereof
US8094302B2 (en) Spectrophotometer
JPWO2014136184A1 (ja) 分取クロマトグラフ装置
CN110824080B (zh) 分光检测器
US7746468B2 (en) Analysis system
WO2021044704A1 (ja) クロマトグラフ用分光光度計および基準位置検出方法
US10782186B2 (en) Monochromator
JP7168917B2 (ja) クロマトグラフ用吸光度検出器および基準位置検出方法
JP4872863B2 (ja) 分光光度計
CN113348345A (zh) 分光光度计
JP2008292249A (ja) 分光光度計
JP5378307B2 (ja) 液体クロマトグラフ用検出器
EP0837326A1 (en) Absorptivity detecting apparatus, chromatographic apparatus, method of detecting absorptivity and method of chromatography
US10648902B2 (en) Analyzer and warm-up determination method
JP2024101182A (ja) 光学的測定装置及び液体クロマトグラフシステム
JP6614056B2 (ja) 分光光度計
KR100555731B1 (ko) 분광광도계
JPWO2006025104A1 (ja) 光学的検出方法および光学的検出器
US5424534A (en) Retail checkstand device with removable controller
JPH05113369A (ja) 分光光度計
JPH0331726A (ja) 分光装置の光源補償機構
JP2002168772A (ja) 分光分析装置

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20861010

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2021543964

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20861010

Country of ref document: EP

Kind code of ref document: A1