Analysis System

Abstract

An analysis system (1) comprises an analysis device (100) that analyzes samples. At least one of the constituent elements of the analysis device (100) is a temperature adjustment constituent element (106; 108) that includes a temperature adjustment element (112; 116) and a temperature sensor (112; 116). The temperature adjustment constituent element (106; 108) must perform temperature control by using the temperature adjustment element (112, 116) and the temperature sensor (112, 116) and stabilize the temperature at a set target temperature at the time of starting the analysis. The analysis device (100) enters an analysis-enabled state in which analysis can be started when the temperatures of all the temperature adjustment constituent elements (106; 108) stabilize at the temperature set for each. The analysis system (1) comprises: a time measurement unit (202) that is configured to measure, as stabilization times, the time required from the start of the temperature control until output of the temperature sensor (112; 116) stabilizes, every time the temperature control is executed; a data accumulation unit (204) that is configured to store and accumulate the stabilization times, which are measured by the time measurement unit (202) each time the temperature control is executed, in association with conditions that affect the stabilization times when the temperature control is executed; and a time prediction unit (206) that is configured to calculate a predicted value of the time required for the analysis device (100) to enter the analysis-enabled state, by using a large number of compatible stabilization times, from among the stabilization times accumulated by the data accumulation unit (204), in which the associated conditions are compatible with the conditions at the time of the setting, when the settings for the analysis are made.

Description

[Technical Field]

[0001] The present invention relates to analytical systems, such as chromatographic analytical systems. [Background technology]

[0002] The temperature of some analytical instrument components affects the reproducibility and stability of analytical results. For example, in a chromatograph, the temperature of the column oven affects the separation performance of the separation column (see Patent Document 1). Therefore, after starting up the analytical instrument and starting temperature control using the column oven or other device, analysis cannot begin until the temperature stabilizes. In addition, absorbance detectors used in liquid chromatographs cannot begin analysis until the temperature of the light source stabilizes, because the intensity of light emitted from the light source is temperature-dependent. In the case of an electrical conductivity detector, the temperature of the cell through which the eluate from the separation column flows affects the measured electrical conductivity, so analysis cannot begin until the temperature of the cell stabilizes. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Application Laid-Open No. 2015-045532 Summary of the Invention [Problem to be solved by the invention]

[0004] The stabilization time required for the temperature of components such as a column oven to stabilize varies depending on the temperature of the environment in which the analytical instrument is located and the target temperature for temperature control set by the user, making it difficult for the user to grasp, at the stage of configuring the analytical instrument, how long it will take for the analytical instrument to be ready for analysis. Therefore, after configuring the analytical instrument, the user may have to repeatedly check whether the analytical instrument is ready for analysis until it is. This cumbersome checking process could be reduced if the user could grasp, at the stage of configuring the analytical instrument, an estimate of the time required for the analytical instrument to be ready for analysis.

[0005] The present invention has been made in consideration of the above-mentioned problems, and aims to provide an analysis system that makes it possible to know in advance an estimate of the time required for the analysis device to become ready for analysis. [Means for solving the problem]

[0006] The analytical system according to the present invention is an analytical system including an analytical device for analyzing a sample, wherein at least one of the components of the analytical device has a temperature control element and a temperature sensor, and is a temperature control component that needs to control the temperature using the temperature control element and the temperature sensor to stabilize the temperature at a set target temperature at the start of the analysis; the analytical device is in an analysis-ready state where it can start analysis when the temperatures of all the temperature control components have stabilized at the temperatures set for each of them; The analysis system comprises: a time measurement unit configured to measure, for each of the temperature control components, a time required for an output of the temperature sensor to stabilize from when the temperature control is started, as a stabilization time, each time the temperature control is executed; a data storage unit configured to store and store the stabilization time measured by the time measurement unit each time the temperature control is executed, in association with conditions that affect the stabilization time when the temperature control is executed; and and a time prediction unit configured to calculate a predicted value of the time required for the analysis device to reach the analysis-ready state by using a large number of compatible stable times, among the stable times stored by the data storage unit, whose associated conditions are compatible with the conditions at the time of setting when the analysis is set. [Effects of the Invention]

[0007] The analysis system of the present invention comprises a time measurement unit that measures, for each of the temperature control components, the time required for the output of the temperature sensor to stabilize after the temperature control is started as a stabilization time each time the temperature control is performed; a data storage unit that stores and accumulates the stabilization time measured by the time measurement unit each time the temperature control is performed, in association with conditions that affect the stabilization time when the temperature control is performed; and a time prediction unit that, when analysis settings are made, calculates a predicted value of the time required for the analysis device to reach a state where it is ready for analysis by using a large number of compatible stabilization times, among the stabilization times accumulated by the data storage unit, whose associated conditions are compatible with the conditions at the time of the settings, thereby making it possible to grasp an estimate of the time required for the analysis device to reach a state where it is ready for analysis. [Brief explanation of the drawings]

[0008] [Figure 1] FIG. 1 is a schematic configuration diagram illustrating an example of an analysis system. [Figure 2] 10 is a flowchart showing an example of the operation until the analysis system of the embodiment reaches a state where analysis is possible. [Figure 3] 10 is an example of stable time data stored in a data storage unit. DETAILED DESCRIPTION OF THE INVENTION

[0009] An embodiment of an analytical system according to the present invention will be described below with reference to the drawings. Although the following description will be given using a liquid chromatography analytical system as an example, the present invention can also be applied to analytical systems such as a gas chromatography analytical system that includes an analytical device having a temperature-controlled component (temperature control component).

[0010] The analysis system 1 includes a liquid chromatograph 100, which is an analysis device, and a management device 200 for managing the operation of the liquid chromatograph 100 and performing various calculation processes.

[0011] The liquid chromatograph 100 includes, as components, a liquid pump 102, an autosampler 104, a column oven 106, a detector 108, and a system controller 110.

[0012] The liquid delivery pump 102 is a device that delivers a mobile phase. The autosampler 104 is a device that injects a sample into the mobile phase delivered by the liquid delivery pump 102. The column oven 106 is a device that houses a separation column for separating components in the sample injected into the mobile phase by the autosampler 104 and adjusts the temperature of the separation column to a preset temperature. The detector 108 is a device that detects each component separated by the separation column. The system controller 110 is provided to be able to communicate with the liquid delivery pump 102, the autosampler 104, the column oven 106, and the detector 108, and is a device that manages the operations of these components 102, 104, 106, and 108.

[0013] Among the components of the liquid chromatograph 100, the column oven 106 and the detector 108 are examples of temperature-controlled components whose respective temperatures are controlled to reach preset target temperatures. The column oven 106 and the detector 108 are equipped with temperature control elements 112 and 116, such as heaters, and temperature sensors 114 and 118, respectively, and the outputs of the temperature control elements 112 and 116 are controlled so that the oven temperature detected by the temperature sensor 114 and the detector temperature detected by the temperature sensor 118 reach the preset target temperatures. The detector 108 is, for example, an absorbance detector or an electrical conductivity detector.

[0014] The management device 200 is a computer device in which software for managing the operation of the analytical device 100 is installed, and is communicably connected to the system controller 100. A user sets analysis conditions and an analysis schedule in the management device 200. The management device 200 transmits necessary information to the system controller 110 based on the analysis conditions and analysis schedule set by the user. Based on the information transmitted from the system controller 110, the system controller 110 controls the operations of the liquid delivery pump 102, autosampler 104, column oven 106, and detector 108 by providing control signals to these components 102, 104, 106, and 108.

[0015] The oven temperature affects the resolution of the separation column, and the detector temperature affects the intensity of the detector signal. In other words, the temperatures of temperature-controlling components such as the column oven 106 and the detector 108 affect the analytical results. Therefore, the analytical instrument 100 is ready for analysis only when the temperatures of all temperature-controlling components have stabilized and are in a standby state. Therefore, when the analytical instrument 100 starts up and temperature control is initiated for the column oven 106 and the detector 108, the system controller 110 reads the temperatures detected by the temperature sensors 114 and 118 and monitors whether the column oven 106 and the detector 108 have entered a standby state. Whether the column oven 106 and the detector 108 have entered a standby state can be determined, for example, by determining whether the temperatures detected by the temperature sensors 114 and 118 remain within a temperature range (target temperature ±α) set based on the target temperatures of the column oven 106 and the detector 108 for a certain period of time.

[0016] The management device 200 reads the status of each of the components 102, 104, 106, and 108 through the system controller 110. The management device 200 not only monitors whether the analysis device 100 is ready for analysis and notifies the user, but also predicts the time required for the analysis device 100 to reach an analysis-ready state after startup and notifies the user. To perform such operations, the management device 200 has the following functions: a time measurement unit 202, a data accumulation unit 204, a time prediction unit 206, an information presentation unit 208, a time management unit 210, and a warning unit 212.

[0017] The time measurement unit 202 has a function of measuring the stabilization time required for the column oven 106 and the detector 108 to enter a standby state after the column oven 106 and the detector 108 start temperature control, respectively.

[0018] The data accumulation unit 204 has a function of storing and accumulating the stabilization times of the column oven 106 and the detector 108 measured by the time measurement unit 202 each time the column oven 106 and the detector 108 perform temperature control, in association with conditions that affect the stabilization times. The conditions that affect the stabilization times include at least the room temperature (ambient temperature of the analytical device 100) at the time of temperature control and the target temperatures set for the column oven 106 and the detector 108. The room temperature is acquired by a room temperature sensor (not shown) provided in one of the components of the analytical device 100 (e.g., the system controller 110). The data accumulation unit 204 is realized by a partial storage area of ​​an information storage device provided in the management device 200. The conditions may be any factor that affects the temperature change of each component device.

[0019] The data accumulation unit 204 accumulates data on stabilization times in a histogram format, such as that shown in FIG. 3, in association with room temperature and target temperature. FIG. 3 shows an example of accumulated data on stabilization times for the column oven 106 when the room temperature is set to 20 to 25°C and the target temperature is set to 70 to 80°C. Each time temperature control of the column oven 106 is performed, the stabilization times measured by the time measurement unit 202 are classified into time ranges (bins) in 500-second increments, such as 250 to 750 seconds, 750 to 1250 seconds, 1250 to 1750 seconds, 1750 to 2250 seconds, 2250 to 2750 seconds, 2750 to 3250 seconds, and 3250 to 3750 seconds, and the number of temperature control attempts for the bin to which the measured stabilization time belongs is incremented. For example, if the stabilization time measured by the time measurement unit 202 is 2640 seconds, the number of temperature control attempts for the bin of 2250 to 2750 seconds is incremented by one. In this way, the data accumulation unit 204 accumulates data on the stabilization time for each temperature range to which the room temperature and target temperature belong when temperature control is executed, as shown in FIG. 3, for each of the column oven 106 and the detector 108.

[0020] Note that FIG. 3 is an example, and the data accumulation unit 204 may be configured to accumulate the stable time data in a format other than a histogram, such as a simple moving average value.

[0021] The time prediction unit 206 is a function that, when analysis conditions such as the target temperatures of the column oven 106 and the detector 108 during analysis are set, calculates a predicted value of the time required for the analyzer 100 to reach an analysis-ready state after startup, using stabilization time (suitable stabilization time) data that matches the room temperature and the set target temperature at that time. The suitable stabilization time data is the stabilization time data for the temperature range that includes the room temperature and target temperature when the analysis conditions were set, among the stabilization time data for each temperature range stored in the data storage unit 204. For example, if the room temperature and target temperature when the analysis conditions were set for the column oven 106 are 28°C and 80°C, respectively, the stabilization time data is the stabilization time data measured under conditions of a room temperature of 25 to 30°C and a target temperature of 70 to 80°C.

[0022] If the number of accumulated data points for the suitable stable time (total number of temperature control times) is equal to or greater than a certain number (e.g., 100), the time prediction unit 206 calculates a predicted value for the time required for the analysis device 100 to reach a state where it can perform analysis, using the remaining suitable stable time data after excluding data points for outliers from the accumulated suitable stable time data.

[0023] The predicted value can be the median or average of the adaptive stabilization time used. The deviant time data can be defined as adaptive stabilization time data that deviates from the median or average of all adaptive stabilization time data by a predetermined time (e.g., 1000 seconds) or more. Furthermore, if the stabilization time data accumulated by the data accumulation unit 204 is a histogram as shown in FIG. 3, the deviant time data can be any stable time data that belongs to a bin (time range) that is a certain number of times (e.g., 2) or more away from the bin to which the median or average of all adaptive stabilization time data belongs. In the example of FIG. 3, the deviant time data can be any data for 12 temperature control runs that falls within a time range of 250 to 750 seconds.

[0024] If the number of accumulated data points for the adapted stabilization time for a temperature control component does not reach a certain number, the predicted value of the time required for that temperature control component to reach a standby state is not calculated. In other words, if the number of accumulated data points for the adapted stabilization time for either the column oven 106 or the detector 108 does not reach a certain number, the prediction of the time required for the analyzer 100 to reach an analysis-ready state is not performed.

[0025] The information presentation unit 208 has a function of presenting to the user, for example, on a display, the predicted value of the time required for the analysis device 100 to become ready for analysis, calculated by the time prediction unit 206.

[0026] The time management unit 210 has a function that allows a user to set an analysis start time, calculates the start-up time of the analysis device 100 so that the analysis device 100 will be ready for analysis at the time set by the user, and starts up the analysis device 100 at the calculated time. The start-up time of the analysis device 100 is calculated using the predicted value of the time required for the analysis device 100 to be ready for analysis, calculated by the time prediction unit 206. Note that the user can arbitrarily set either the start-up time or the analysis start time of the analysis device 100. However, the function of the time management unit 210 is based on the premise that the prediction function of the time prediction unit 206 is enabled.

[0027] The warning unit 212 has a function of determining whether the room temperature at the time of startup of the analyzer 100 has changed significantly from the room temperature when the analysis conditions were set, and if so, issuing a warning to the user by, for example, displaying a predetermined message on the display. If the room temperature at the time of startup of the analyzer 100 has changed significantly from the room temperature when the analysis conditions were set, the time required for the analyzer 100 to actually reach an analysis-ready state is likely to differ significantly from the predicted value calculated by the time prediction unit 206. Therefore, the warning unit 212 notifies the user that the time required for the analyzer 100 to reach an analysis-ready state may differ from the predicted value by, for example, displaying a message such as "The controlled temperature will be difficult to stabilize. Please check whether the room temperature has not fluctuated significantly." Whether the room temperature at the time of startup of the analyzer 100 has changed significantly from the room temperature when the analysis conditions were set can be determined by whether the difference between the two is equal to or greater than a predetermined temperature (e.g., 5°C).

[0028] An example of the operation of the analysis system 1 realized by the above-described functions will be described with reference to the flowchart of FIG. 2 together with FIG.

[0029] When a user sets analytical conditions in the management device 200, the time prediction unit 206 acquires the room temperature at that time from the room temperature sensor (step 101) and extracts suitable stabilization time data for each of the column oven 106 and the detector 108 using the acquired room temperature and the set analytical conditions (step 102). If the number of pieces of suitable stabilization time data for each of the column oven 106 and the detector 108 is equal to or greater than a certain number, the time prediction unit 206 determines that it is possible to predict the time required for the analytical device 100 to reach an analytically ready state after startup (step 103: Yes) and calculates a predicted value (step 104). The information presentation unit 208 displays the predicted value calculated by the time prediction unit 206 on a display (step 105). On the other hand, if the number of pieces of suitable stabilization time data for at least one of the column oven 106 and the detector 108 is less than the certain number, the time prediction unit 206 does not execute steps 104 and 105.

[0030] Thereafter, when the start-up time of the analytical device 100, set by the user or calculated by the time management unit 210, arrives, the management device 200 sends a signal to the system controller 110 to start up the components 102, 104, 106, and 108, and the system controller 110 starts up the components 102, 104, 106, and 108 (step 109). At this time, temperature control is started in the column oven 106 and the detector 108. The warning unit 212 acquires the room temperature when the analytical device 100 is started up (step 107), determines whether the room temperature has changed significantly since the analysis conditions were set (step 108), and if it has changed significantly, displays a warning on the display (step 110).

[0031] After the analytical device 100 starts up, the time measurement unit 202 measures the stabilization time of each temperature control component (column oven 106 and detector 108), and the stabilization times measured by the time measurement unit 202 are stored in the data storage unit 204 (step 111). Then, when the temperatures of all the temperature control components are stabilized at the target temperatures, the analytical device 100 becomes ready for analysis (step 112).

[0032] It should be noted that the functions of the time measurement unit 202, data accumulation unit 204, time prediction unit 206, information presentation unit 208, time management unit 210, and warning unit 212 do not necessarily have to be installed in the management device 200, and some or all of these functions may be installed in the system controller 110.

[0033] The embodiment described above is merely one example of an embodiment of the analysis system according to the present invention. The embodiment of the analysis system according to the present invention is as follows.

[0034] One embodiment of the analysis system according to the present invention is an analysis system including an analysis device that analyzes a sample, At least one of the components of the analytical device is a temperature control component that has a temperature control element and a temperature sensor, and is required to control the temperature using the temperature control element and the temperature sensor to stabilize the temperature at a set target temperature at the start of the analysis; the analytical device is in an analysis-ready state where it can start analysis when the temperatures of all the temperature control components have stabilized at the temperatures set for each of them; The analysis system comprises: a time measurement unit configured to measure, for each of the temperature control components, a time required for an output of the temperature sensor to stabilize from when the temperature control is started, as a stabilization time, each time the temperature control is executed; a data storage unit configured to store and store the stabilization time measured by the time measurement unit each time the temperature control is executed, in association with conditions that affect the stabilization time when the temperature control is executed; and and a time prediction unit configured to calculate a predicted value of the time required for the analysis device to reach the analysis-ready state by using a large number of compatible stable times, among the stable times stored by the data storage unit, whose associated conditions are compatible with the conditions at the time of setting when the analysis is set.

[0035] In the aspect [1] of the above embodiment, the conditions include an ambient temperature of the analytical device and the target temperature set for the temperature control component.

[0036] In the above aspect [1], the temperature control device may further include a warning unit configured to issue a warning to a user when the environmental temperature when the temperature control of the temperature adjustment component is executed differs by a predetermined temperature or more from the environmental temperature at the time of setting, thereby notifying the user that the time required for the analyzer to actually reach the analysis ready time may significantly deviate from the value predicted by the time prediction unit.

[0037] In a second aspect of the embodiment, the time prediction unit is configured to set the predicted value to the average or median of the adaptive settling times used. This second aspect can be combined with the first aspect.

[0038] In aspect [3] of the above embodiment, the time prediction unit is configured to calculate the average of the adaptation stable times as a provisional average value or the median of the adaptation stable times as a provisional median value, determine the adaptation stable times that deviate from the provisional average value or the provisional median value by a predetermined time or more as deviation times, and use the adaptation stable times excluding the deviation times in calculating the predicted value. By calculating the predicted value excluding the deviation times, a more accurate predicted value can be obtained. This aspect [3] can be combined with the above aspect [1] and / or aspect [2].

[0039] In aspect [4] of the above embodiment, the apparatus further includes an information presentation unit configured to present the predicted value calculated by the time prediction unit to a user. This allows the user to understand the approximate time required for the analytical device to reach a state where it is ready for analysis. This aspect [4] can be combined with the above aspect [1], and / or aspect [2], and / or aspect [3].

[0040] In aspect [5] of the above embodiment, the analyzer further includes a time management unit configured to allow a user to set a time at which the analyzer should be in the analysis-ready state, calculate a start time for the temperature control of the temperature control components using the predicted value calculated by the time prediction unit so that the analyzer will be in the analysis-ready state at the time set by the user, and automatically start the temperature control of the temperature control components at the calculated time. This aspect [5] can be combined with the above aspect [1], and / or aspect [2], and / or aspect [3], and / or aspect [4].

[0041] In aspect [6] of the above embodiment, the analytical device is a chromatograph, and the temperature control components include a column oven and a detector. This aspect [6] can be combined with the above aspects [1], [2], [3], [4], and [5]. [Explanation of symbols]

[0042] 1. Analysis System 100 Analytical equipment (liquid chromatograph) 102 Liquid transfer pump 104 Autosampler 106 Column Oven 108 detectors 110 System Controller 112,116 Temperature control element 114,118 Temperature Sensors 200 Management device 202 Time Measurement Section 204 Data Storage Unit 206 Time Prediction Section 208 Information Presentation Department 210 Time Management Department 212 Warning section

Claims

1. An analytical system including an analytical device for analyzing a sample, At least one of the components of the analytical device is a temperature control component that has a temperature control element and a temperature sensor, and is required to control the temperature using the temperature control element and the temperature sensor to stabilize the temperature at a set target temperature at the start of the analysis; the analytical device is in an analysis-ready state where it can start analysis when the temperatures of all the temperature control components have stabilized at the temperatures set for each of them; The analysis system comprises: a time measurement unit configured to measure, for each of the temperature control components, a time required for an output of the temperature sensor to stabilize from when the temperature control is started, as a stabilization time, each time the temperature control is executed; a data storage unit configured to store and store the stabilization time measured by the time measurement unit each time the temperature control is performed, in association with the environmental temperature of the analytical device and the target temperature set for the temperature control component, which are conditions that affect the stabilization time when the temperature control is performed; an analysis system comprising: a time prediction unit configured, when the analysis is set up, to calculate a predicted value of the time required for the analysis device to reach the analysis-ready state by using a suitable stabilization time, among the stabilization times stored by the data storage unit, whose associated conditions are suitable for the conditions at the time of setting up.

2. The analysis system of claim 1, further comprising a warning unit configured to issue a warning to a user when the environmental temperature when the temperature control of the temperature control component is performed is different from the environmental temperature at the time of setting by more than a predetermined temperature.

3. The analysis system according to claim 1 , wherein the time prediction unit is configured to set the predicted value to an average or median value of the adapted settling times used.

4. 2. The analysis system according to claim 1, wherein the time prediction unit is configured to determine the average value of the adaptation stable times as a provisional average value or the median value of the adaptation stable times as a provisional median value, to determine the adaptation stable times that deviate from the provisional average value or the provisional median value by a predetermined time or more as deviant times, and to use the adaptation stable times excluding the deviant times in calculating the predicted value.

5. The analysis system according to claim 1 , further comprising an information presentation unit configured to present the predicted value calculated by the time prediction unit to a user.

6. The analysis system of claim 1 further comprises a time management unit configured to allow a user to set the time at which the analysis device should be in the analysis-ready state, calculate the start time of the temperature control of the temperature control components using the predicted value calculated by the time prediction unit so that the analysis device will be in the analysis-ready state at the time set by the user, and automatically start the temperature control of the temperature control components at the calculated time.

7. the analytical device is a chromatograph; The analytical system of claim 1 , wherein the temperature control components include a column oven and a detector.

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