WO2020079800A1 - Appareil de détection - Google Patents

Appareil de détection Download PDF

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Publication number
WO2020079800A1
WO2020079800A1 PCT/JP2018/038826 JP2018038826W WO2020079800A1 WO 2020079800 A1 WO2020079800 A1 WO 2020079800A1 JP 2018038826 W JP2018038826 W JP 2018038826W WO 2020079800 A1 WO2020079800 A1 WO 2020079800A1
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WO
WIPO (PCT)
Prior art keywords
flow cell
threshold value
light
detection device
holding unit
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Application number
PCT/JP2018/038826
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English (en)
Japanese (ja)
Inventor
真二 辻
Original Assignee
株式会社島津製作所
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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 PCT/JP2018/038826 priority Critical patent/WO2020079800A1/fr
Publication of WO2020079800A1 publication Critical patent/WO2020079800A1/fr

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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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03—Cuvette constructions
    • G01N21/05—Flow-through cuvettes
    • 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
    • G01N21/01—Arrangements or apparatus for facilitating the optical investigation
    • G01N21/15—Preventing contamination of the components of the optical system or obstruction of the light path

Definitions

  • the present invention relates to a detection device that includes a flow cell for circulating a sample solution and is configured to detect a sample in a sample solution based on a change in the amount of light passing through the flow cell.
  • Absorbance detectors are known as detection devices for liquid chromatographs.
  • the absorbance detector irradiates the flow cell in which the sample solution flows with light from a light source, detects the intensity of the light that has passed through the flow cell with an optical sensor, and obtains the absorbance at a specific wavelength to obtain a sample solution in the sample solution flowing in the flow cell. It quantifies or qualifies the components (see, for example, Patent Document 1).
  • the ratio of noise contained in the measured data such as absorbance may increase due to some factors.
  • the magnitude of the noise in the measurement data changes due to various factors such as deterioration of the light source and optical system, insufficient degassing of the mobile phase solvent, and contamination of the flow cell and piping.Therefore, it is not possible to identify the cause of the large noise. It's not easy.
  • an object of the present invention is to make it possible to easily determine whether or not a flow cell is dirty.
  • the detection device has a light source, an optical system that generates measurement light and reference light based on the light emitted from the light source, and a flow cell for circulating a sample solution, and the flow cell is the measurement.
  • a flow cell device provided so as to be arranged on the optical path of light, a measurement light that has passed through the flow cell and a reference light that does not pass through the flow cell (no flow cell is provided on the optical path)
  • a light amount detection unit for detecting the light amount, the light amount of the measurement light and the reference light obtained based on the output signal of the light amount detection unit when the flow cell is in a blank state in which the sample solution does not flow
  • a dirt determination unit configured to determine the presence or absence of dirt on the flow cell by comparing the ratio of the amount of light with a threshold value.
  • a blank state in which the sample solution is not flown into the flow cell includes not only a state in which no liquid is flown into the flow cell but also a state in which a blank liquid containing no sample component is flown into the flow cell.
  • the "threshold value" used to determine the presence or absence of stains on the flow cell is obtained based on the ratio of the light amount of the measurement light and the reference light measured in the "initial state” where the flow cell is clean and in the "blank state”. Is.
  • the values when the light quantity of the measurement light and the light quantity of the reference light are measured in the "initial state” and the “blank state” of the flow cell are defined as the “initial values" of the measurement light and the reference light, respectively.
  • the ratio of the amount of measuring light to the amount of reference light when the flow cell is in a blank state is most affected by the contamination of the flow cell and is hardly affected by the emission intensity of the light source.
  • the ratio of the light quantity of the measurement light and the reference light when the flow cell is in the "initial state” and "blank state” is a unique value when the flow cell is clean, and is a standard that indicates that the flow cell is clean. It is a value. If the ratio of the light amount of the measurement light and the reference light measured with the flow cell in the blank state is different from this reference value, it is considered that the flow cell is contaminated. Therefore, a value obtained by adding an allowable range such as a measurement error to the reference value obtained by the initial values of the measurement light and the reference light can be used as the threshold value for determining the presence or absence of the stain.
  • the detection device made based on the above knowledge, measuring the light quantity of the measurement light and the reference light with the flow cell in a blank state, obtain the ratio of the light quantity, the ratio and a predetermined threshold value.
  • the comparison is provided with a function of determining whether or not the flow cell is dirty.
  • the above threshold may be set in advance.
  • the detection device is provided with a threshold value holding unit that holds a preset threshold value.
  • the flow cell is provided with a holding unit that holds the initial values of the light amounts of the measurement light and the reference light measured in the initial state and in the blank state, each time when determining whether the flow cell is dirty or not.
  • the threshold value may be set based on the ratio of those initial values.
  • the threshold configured to set the threshold value. It is preferable to further include a value setting unit. Then, when the user installs the flow cell device in the detection device, the user can set the unique threshold value of the flow cell device by using the function of the threshold value setting unit. In this case, the threshold value set by the threshold value setting unit is held in the threshold value holding unit.
  • different flow cell devices may be used depending on the application (for example, the type of sample) or each user who uses the detection apparatus.
  • the threshold value for determining whether or not the flow cell is contaminated is a unique value that differs for each flow cell device.
  • the flow cell device has unique cell identification information
  • the threshold value holding unit sets the unique threshold value of the flow cell device to the cell identification information. Is configured to be held in association with.
  • the dirt determination unit holds the flow cell of the flow cell device based on the threshold value held in the threshold value holding unit and associated with the cell identification information of the flow cell device currently in use. It is configured to determine the presence or absence of dirt. As a result, even if the flow cell device is replaced with another one, it is possible to determine whether the flow cell is dirty or not by using the threshold value specific to the flow cell device and associated with the cell identification information of the flow cell device. You can
  • the threshold holding unit itself may be mounted on the flow cell device and hold the threshold specific to the flow cell device. This means that the flow cell device itself holds its own threshold. Then, when the flow cell device is replaced with another one, it is possible to determine whether or not the flow cell is contaminated by using the unique threshold value held by the flow cell device itself.
  • the flow cell device may be used across multiple detectors.
  • the ratio of the amount of light of the measurement light and the reference light varies depending on the detection device, it is necessary to determine the presence or absence of contamination of the flow cell depending on which detection device has measured the initial value of the measurement light and the reference light.
  • the threshold can change. Therefore, if the threshold value set by a certain detection device is used, it may not be possible to correctly determine whether or not the flow cell is dirty. Therefore, when determining whether or not the flow cell is contaminated, it is preferable that the flow cell device is prepared not only for each flow cell device but also for each detection device in which the flow cell device is installed.
  • the detection apparatus has unique detection apparatus identification information
  • the threshold value holding unit is unique when the flow cell device is used in the detection apparatus.
  • the threshold value is configured to be held in association with the detection device identification information
  • the dirt determination unit is associated with the detection device identification information of the detection device held in the threshold value holding unit. It is configured to determine whether or not the flow cell is contaminated based on the threshold value obtained. By doing so, it is possible to determine the presence or absence of contamination of the flow cell by using a unique threshold that can vary depending on the combination of the flow cell device and the detection device, and to determine the presence or absence of contamination of the flow cell with higher accuracy. You can
  • the flow cell may further include an initial value holding unit that holds the initial values of the amounts of the measurement light and the reference light when the measurement is performed in the initial state and the blank state. If the information about the initial values of the light amounts of the measurement light and the reference light is held, it is possible to further limit the cause of noise in the measurement data. For example, since contamination of the flow cell does not contribute to the change in the light amount of the reference light, when the light amount of the reference light is lower than the initial value, the emission intensity of the light source is reduced, the light transmittance is reduced due to the deterioration of the lens, It is conceivable that the mirror may be clouded or deteriorated, resulting in a decrease in reflectance.
  • the dirt determination unit determines that the flow cell is dirty, it is configured to notify the user to that effect. Any method may be used to notify the user. For example, a method of displaying such on a display unit such as a liquid crystal display provided in the detection device or connected to the detection device, a method of lighting a lamp indicating an error, a method of issuing a warning sound, and the like can be mentioned.
  • the flow cell is in a blank state, the light quantities of the measurement light and the reference light are measured, the ratio of the light quantities thereof is determined, and the ratio is compared with a predetermined threshold value, whereby the flow cell is contaminated. Since it has a function of determining whether or not there is any, it is possible to easily determine whether or not the flow cell is dirty.
  • Fig. 1 shows an embodiment of the detection device.
  • the detection device 1 of this embodiment includes a measurement unit 2 and an arithmetic processing unit 4.
  • the measurement unit 2 includes a light source 6, a slit 8, a mirror 10, a spectroscope 12, a beam splitter 14, a flow cell device 16, and photodetection elements 20 and 22.
  • the arithmetic processing unit 4 includes a stain determination unit 26, a threshold value setting unit 28, a threshold value holding unit 30, and an initial value holding unit 32.
  • a display unit 34 is connected to the arithmetic processing unit 4.
  • the light emitted from the light source 6 passes through the slit 8 and is reflected by the mirror 10 and guided to the spectroscope 12 realized by a diffraction grating or the like.
  • the spectroscope 12 is adjusted so as to disperse the light from the mirror 10 for each wavelength component and guide only the light of the measurement wavelength to the beam splitter 14 side.
  • Part of the light of the measurement wavelength guided to the beam splitter 14 by the spectroscope 12 is reflected by the beam splitter 14 and enters the photodetector 22 as reference light, and the remaining light passes through the beam splitter 14. And becomes measuring light.
  • the beam splitter 14 realizes an optical system that generates measurement light and reference light based on the light from the light source 6.
  • the optical system that generates the measurement light and the reference light based on the light from the light source 6 is not limited to the beam splitter 14, and is measured by changing the reflection angle of the light from the light source 6 with time. It may be configured to generate the light and the reference light, or may be a light-shielding plate having a hole for measuring light generation and a hole for generating reference light.
  • the flow cell device 16 has a flow cell 18 for circulating a sample solution therein, and the flow cell 18 is provided so as to be arranged on the optical path of the measurement light that has passed through the beam splitter 14.
  • the measurement light that has passed through the flow cell 18 enters the photodetection element 20.
  • the light detection elements 20 and 22 form a light amount detection unit that detects the light amounts of the measurement light and the reference light.
  • the detection signals obtained by the photodetectors 20 and 22 are taken into the arithmetic processing unit 4.
  • the flow cell device 16 also includes a storage medium 24 realized by a flash memory or the like.
  • the storage medium 24 stores unique cell identification information for identifying the flow cell device 16 from other flow cell devices.
  • the information stored in the storage medium 24 is also fetched by the arithmetic processing unit 4.
  • the arithmetic processing unit 4 is realized by a dedicated computer or a general-purpose personal computer.
  • the dirt determination unit 26 and the threshold value setting unit 28 of the arithmetic processing unit 4 are functions obtained by the arithmetic elements such as the CPU executing the programs stored in the arithmetic processing unit 4.
  • the threshold value holding unit 30 and the initial value holding unit 32 are functions realized by a partial area of the storage medium provided in the arithmetic processing unit 4.
  • the contamination determination unit 26 determines a ratio (for example, reference light / measurement light) of a light amount of the measurement light and the reference light detected by the photodetection elements 20 and 22 when the flow cell 18 is in a blank state in which the sample solution does not flow. It is configured to determine whether or not the flow cell 18 of the flow cell device 16 is contaminated by comparing it with the threshold value of. Whether or not the flow cell 18 is contaminated can be determined, for example, when the amount of light emitted from the light source 6 at the time of validation performed when the detection device 1 is activated is checked.
  • a ratio for example, reference light / measurement light
  • the soiling determination unit 26 displays a message to that effect on the display unit 34, turns on a predetermined lamp, or emits a warning sound to notify the user.
  • the flow cell 18 is configured to be washed.
  • the threshold value holding unit 30 holds a preset threshold value for determining whether or not the flow cell 18 is dirty.
  • the threshold value held in the threshold value holding unit 30 may be set by the threshold value setting unit 28.
  • the threshold value setting unit 28 determines the presence or absence of contamination of the flow cell 18 of the flow cell device 16 automatically or based on a command from the user when the flow cell device 16 is first installed in the detection apparatus 1. Configured to set a threshold for.
  • the threshold value is obtained by measuring the light amounts of the measurement light and the reference light as respective initial values with the flow cell 18 in the initial state in which no dirt is generated being in a blank state, and calculating the ratio of those initial values, and calculating the ratio. Can be set as a value in which the allowable range is added.
  • the threshold value set by the threshold value setting unit 28 is held in the threshold value holding unit 30.
  • the initial values of the measurement light and the reference light used for setting the threshold value are held in the initial value holding unit 32.
  • the initial values of the measurement light and the reference light held in the initial value holding unit 32 are factors of noise in the measurement data other than contamination of the flow cell 18 (for example, decrease in light emission intensity of the light source 6, deterioration of the mirror 10, clouding, etc.). Can be used to identify
  • both the threshold value holding unit 30 and the initial value holding unit 32 do not necessarily have to be provided.
  • the initial value holding unit 32 may not be provided.
  • the threshold value can be calculated each time using the initial values of the measurement light and the reference light held in the initial value holding unit 32.
  • the threshold value holding unit 30 may not be provided.
  • a plurality of flow cell devices 16 may be prepared, and measurement may be performed by exchanging the flow cell device 16 with a different flow cell device 16 depending on the application (type of sample, etc.) or each user.
  • the initial values of the measurement light and the reference light are measured for each flow cell device 16, and a unique value set based on the ratio is measured. Is preferably used.
  • the threshold value holding unit 30 of the arithmetic processing unit 4 sets the threshold value set for each flow cell device 16 to the threshold value. It is preferably configured to be held in association with the unique cell identification information of each flow cell device 16.
  • the dirt determination unit 26 reads the cell identification information of the flow cell device 16 installed in the detection device 1, reads the threshold value associated with the cell identification information from the threshold value holding unit 30, and detects the flow cell 18 of the flow cell 18. The threshold value is used to determine whether or not there is a stain.
  • the threshold holding unit 30 may be provided on the flow cell device 16 itself.
  • the threshold value holding unit 30 can be realized by a partial area of the storage medium 24 provided in each flow cell device 16.
  • the threshold value set by the threshold value setting unit 28 is held in the threshold value holding unit 30 of the flow cell device 16. Then, when the dirt determination unit 26 determines the presence or absence of dirt on the flow cell 18, the threshold value holding unit 30 of the flow cell device 18 reads the unique threshold value of the flow cell device 18, and the judgment is performed using the threshold value. Do.
  • each flow cell device 16 may be provided with an initial value holding unit 32 instead of the threshold holding unit 30 or in addition to the threshold holding unit 30.
  • the dirt holding unit 26 holds the initial value holding unit 32 when it judges whether or not the flow cell 18 is dirty. Based on the initial values of the measurement light and the reference light, a threshold value is obtained each time, and the presence or absence of dirt is determined using the threshold value.
  • a specific flow cell device 16 may be used across a plurality of detection devices 1.
  • the threshold value for determining the presence / absence of contamination of the flow cell 18 varies depending on which detector 1 measures the initial values of the measurement light and the reference light. Therefore, the threshold holding unit 30 of the flow cell device 16 may hold the threshold set by each detection device 1 in association with the detection device identification information assigned to each detection device 1. preferable.
  • the dirt determination unit 26 of each detection device 1 has a threshold value associated with the detection device identification information of the detection device 1 among the threshold values held in the threshold value holding unit 30 of the flow cell device 16. The value is used to determine whether the flow cell 18 is dirty.
  • the initial value holding unit 32 may be provided in each flow cell device 16 instead of the threshold value holding unit 30.
  • the threshold value for determining whether or not the flow cell 18 is contaminated can vary for each individual flow cell device 16 and for each detection device 1 for which the threshold value is set. In other words, there is a unique threshold value for each combination of the detection device 1 and the flow cell device 16. Therefore, the threshold value holding unit 16 that holds the threshold value associated with each combination of the detection device identification information and the cell identification information may be provided on either the detection device 1 side or the flow cell device 16 side. desirable.
  • the threshold value is set automatically, for example, when the flow cell device 16 is installed in the detection device 1 for the first time, or based on a command from the user.
  • the threshold value is set by making the emission intensity of the light source 6 stable and leaving the flow cell 18 in a blank state (step S1).
  • the blank state means a state in which no liquid is flowing or a blank liquid containing no sample component is flowing.
  • the threshold value setting unit 28 reads the output signals of the photodetection elements 20 and 22 and measures the amounts of the measurement light and the reference light (step S2). The measured value becomes the initial value of the measurement light and the reference light.
  • the threshold setting unit 28 calculates the ratio of the measured measurement light and the initial value of the reference light (for example, reference light / measurement light) (step S3). Then, a value obtained by adding a certain allowable range to the ratio of the measurement light and the reference light obtained by calculation is set as a threshold value (step S4).
  • the threshold value set by the threshold value setting unit 28 is held (stored) in the threshold value holding unit 30, and the initial values of the measurement light and the reference light are held (stored) in the initial value holding unit 32.
  • the threshold value varies depending on the required S / N, the ratio between the measurement light and the reference light may be set to a constant value (for example, 0.5).
  • the determination as to whether or not the flow cell 18 is contaminated is performed, for example, at the time of validation when the detection device 1 is started up.
  • the dirt determination unit 26 reads out the unique threshold value of the flow cell device 16 from the threshold value holding unit 30 (step S11).
  • the flow cell 18 is set in a blank state (step S12), and the light amounts of the measurement light and the reference light in the state where the emission intensity of the light source 6 is stable are measured (step S13).
  • the stain determination unit 26 obtains the ratio of the measured light amount of the measured light and the reference light (for example, reference light / measured light) by calculation (step S14), and the ratio is the threshold value read from the threshold value holding unit 30. (Step S15). If the calculated ratio is equal to or greater than the threshold value, it is determined that the flow cell 18 is soiled (step S16), and the fact is displayed on the display unit 34 or a predetermined lamp is lit. The user is prompted to wash the flow cell 18 by issuing a warning sound (step S17). On the other hand, if the calculated ratio is smaller than the threshold value, it is determined that the flow cell 18 is not contaminated (step S18).

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Optical Measuring Cells (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

Le présent appareil de détection comporte : une source de lumière ; un système optique pour générer une lumière de mesure et une lumière de référence sur la base de la lumière émise par la source de lumière ; un dispositif de cellule d'écoulement ayant une cellule d'écoulement à travers laquelle une solution d'échantillon est amenée à s'écouler, la cellule d'écoulement étant disposée de façon à être disposée sur le trajet optique de la lumière de mesure ; une unité de détection de quantité de lumière pour détecter la quantité de chacune de la lumière de mesure traversant la cellule d'écoulement et la lumière de référence ne passant pas à travers la cellule d'écoulement (la cellule d'écoulement n'étant pas disposée sur le trajet optique de la lumière de référence) ; et une unité de détermination de contamination configurée de façon à déterminer la présence / l'absence de contamination de la cellule d'écoulement par comparaison, avec une valeur de seuil, du rapport de la quantité de la lumière de mesure obtenue sur la base du signal de sortie de l'unité de détection de quantité de lumière dans un état d'ébauche dans lequel il n'y a pas de solution d'échantillon s'écoulant dans la cellule d'écoulement et la quantité de la lumière de référence.
PCT/JP2018/038826 2018-10-18 2018-10-18 Appareil de détection WO2020079800A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023218672A1 (fr) * 2022-05-13 2023-11-16 富士電機株式会社 Dispositif d'analyse de la qualité de l'eau

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Publication number Priority date Publication date Assignee Title
JPS57101742A (en) * 1980-12-17 1982-06-24 Mitsubishi Electric Corp Optical concentration meter
JPH02276927A (ja) * 1988-08-30 1990-11-13 Shimadzu Corp 一体型分光器とオンライン用分光計測装置
JPH07301630A (ja) * 1994-03-07 1995-11-14 Kyoto Daiichi Kagaku:Kk 尿中成分測定装置を備えた便器
JPH09171022A (ja) * 1995-10-31 1997-06-30 Hewlett Packard Co <Hp> 分析測定装置における交換可能な部品を識別する装置
JPH09218152A (ja) * 1996-02-13 1997-08-19 Horiba Ltd ダブルビーム型の測定系における異常検知方法
JP2000131310A (ja) * 1998-10-28 2000-05-12 Hitachi Ltd 水質計の自己診断機能
JP2001194302A (ja) * 2000-01-14 2001-07-19 Otsuka Denshi Co Ltd 光学測定装置
WO2006009251A1 (fr) * 2004-07-22 2006-01-26 Wako Pure Chemical Industries, Ltd. Procédé d'assistance d'analyse, analyseur, ordinateur distant, procédé d'analyse de données, programme et conteneur de réactif
JP2007057283A (ja) * 2005-08-23 2007-03-08 Horiba Ltd 薬液濃度モニタ
JP2011149831A (ja) * 2010-01-22 2011-08-04 Hitachi High-Technologies Corp 自動分析装置
JP2017058382A (ja) * 2016-12-27 2017-03-23 株式会社島津製作所 液体クロマトグラフ用検出器
JP2017156093A (ja) * 2016-02-29 2017-09-07 株式会社島津製作所 分析測定装置システム

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57101742A (en) * 1980-12-17 1982-06-24 Mitsubishi Electric Corp Optical concentration meter
JPH02276927A (ja) * 1988-08-30 1990-11-13 Shimadzu Corp 一体型分光器とオンライン用分光計測装置
JPH07301630A (ja) * 1994-03-07 1995-11-14 Kyoto Daiichi Kagaku:Kk 尿中成分測定装置を備えた便器
JPH09171022A (ja) * 1995-10-31 1997-06-30 Hewlett Packard Co <Hp> 分析測定装置における交換可能な部品を識別する装置
JPH09218152A (ja) * 1996-02-13 1997-08-19 Horiba Ltd ダブルビーム型の測定系における異常検知方法
JP2000131310A (ja) * 1998-10-28 2000-05-12 Hitachi Ltd 水質計の自己診断機能
JP2001194302A (ja) * 2000-01-14 2001-07-19 Otsuka Denshi Co Ltd 光学測定装置
WO2006009251A1 (fr) * 2004-07-22 2006-01-26 Wako Pure Chemical Industries, Ltd. Procédé d'assistance d'analyse, analyseur, ordinateur distant, procédé d'analyse de données, programme et conteneur de réactif
JP2007057283A (ja) * 2005-08-23 2007-03-08 Horiba Ltd 薬液濃度モニタ
JP2011149831A (ja) * 2010-01-22 2011-08-04 Hitachi High-Technologies Corp 自動分析装置
JP2017156093A (ja) * 2016-02-29 2017-09-07 株式会社島津製作所 分析測定装置システム
JP2017058382A (ja) * 2016-12-27 2017-03-23 株式会社島津製作所 液体クロマトグラフ用検出器

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023218672A1 (fr) * 2022-05-13 2023-11-16 富士電機株式会社 Dispositif d'analyse de la qualité de l'eau

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