Wavelength correction method, control circuit and monitoring system of liquid chromatograph
By dynamically adjusting the wavelength calibration cycle of the liquid chromatograph and combining the use of intensity and zone calibration modes, the problem of wavelength calibration lag in liquid chromatographs has been solved, achieving more efficient and accurate wavelength calibration and data analysis.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- CHONGQING MASS SPECTROMETRY TECHNOLOGY CO LTD
- Filing Date
- 2026-02-06
- Publication Date
- 2026-05-08
AI Technical Summary
Current liquid chromatograph wavelength calibration relies on human experience, which leads to lag and inconsistency, making it difficult to detect subtle deviations in a timely manner and affecting data reliability.
It adopts a mechanism that dynamically adjusts the wavelength calibration cycle based on usage intensity. The usage intensity of the chromatograph is obtained through the Internet of Things, and the calibration cycle is dynamically adjusted. Combined with regional centralized and decentralized autonomous calibration modes, the calibration cycle is adjusted in a personalized manner.
It improves the timeliness and efficiency of wavelength correction, enhances the accuracy and automation of detection and analysis data, and reduces reliance on manual labor and operational complexity.
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Figure CN121994958A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of liquid chromatography technology, specifically to a wavelength correction method, control circuit, and monitoring system for a liquid chromatograph. Background Technology
[0002] Currently, the maintenance of wavelength accuracy in liquid chromatographs relies heavily on manual experience. Users or maintenance personnel need to judge whether a wavelength shift has occurred based on experience, and manually trigger the calibration process or contact a specialist after discovering a problem. On the one hand, traditional methods are highly dependent on the professional experience of personnel; on the other hand, subtle early shifts are difficult to detect in a timely manner, often only being discovered when they evolve into obvious deviations that may have already affected data reliability. Therefore, there is a certain lag between the occurrence of a shift and its detection.
[0003] In response, some methods for correcting the output values of liquid chromatograph detectors have been proposed in the existing technology.
[0004] For example, patent CN107490632A discloses a liquid chromatograph and a method for correcting fluctuations in the detector output value of the liquid chromatograph. The selection of the correction wavelength is influenced by the user's experience, and excessive correction can lead to the loss of information about trace components, particularly small peaks, on the chromatogram, resulting in incorrect analytical results. This method determines the minimum peak value based on the analytical results, sets the S / N ratio of the minimum peak value as the maximum correction wavelength, and uses this determined correction wavelength to perform correction for the minimum peak value. Multiple detector output value correction methods are registered within the computing unit, and the method is selected from the registered methods based on the initially set correction method or purpose to perform the correction.
[0005] However, this technical solution focuses on processing the output data after the sample analysis is completed.
[0006] Therefore, there is an urgent need for a more efficient method for wavelength correction in liquid chromatography. Summary of the Invention
[0007] The purpose of this invention is to provide a wavelength correction method, control circuit and monitoring system for a liquid chromatograph, which partially solves or alleviates the above-mentioned deficiencies in the prior art and can improve the efficiency of wavelength correction of liquid chromatograph equipment.
[0008] To solve the aforementioned technical problems, the present invention specifically adopts the following technical solution: A first aspect of the present invention is to provide a wavelength calibration method for a liquid chromatograph, comprising the steps of: S101, performs wavelength correction periodically according to a preset correction cycle; S102, Obtain the usage intensity of the liquid chromatograph during the most recent calibration period; the usage intensity = K1 * standardized number of uses + K2 * standardized total running time; S103, determine whether the usage intensity within the most recent correction period is greater than or equal to a second preset threshold and less than a first preset threshold; the second preset threshold is less than the first preset threshold; S104, if the intensity of use is greater than or equal to the first preset threshold, shorten the correction period according to the first preset reduction, and perform periodic wavelength correction according to the adjusted correction period; S105, if the intensity of use is less than the second preset threshold, extend the correction period by the first preset increment, and perform periodic wavelength correction according to the adjusted correction period; S106, if the intensity of use is greater than or equal to the second preset threshold and less than the first preset threshold, maintain the current correction cycle.
[0009] In some embodiments, a plurality of spatially adjacent liquid chromatographs are divided into a region, and accordingly, the method further includes the step of: S201, The host computer obtains the usage intensity of each liquid chromatograph in each region during the most recent calibration period via the Internet of Things; S202, the host computer determines whether the difference between the usage intensity and the mean of each liquid chromatograph in each region is less than or equal to a preset difference threshold. If the host computer determines that the difference between the usage intensity and the mean of each liquid chromatograph in any region is less than or equal to a preset difference threshold, a regional centralized correction mode is adopted. The regional centralized correction mode is as follows: if the minimum usage intensity is greater than or equal to a first preset intensity threshold, the correction cycle of the chromatograph corresponding to the maximum usage intensity is shortened by a first preset reduction, and the correction cycle is used as the correction cycle of all chromatographs in any region; if the maximum usage intensity is less than a second preset threshold, the correction cycle of the chromatograph corresponding to the middle usage intensity is extended by a first preset increment, and the correction cycle is used as the correction cycle of all chromatographs in the same region. If the host computer determines that the difference between the usage intensity and the mean of at least N liquid chromatographs in any region is greater than the preset difference threshold, and N is greater than or equal to the preset quantity threshold, then a dispersed autonomous correction mode is adopted for the N liquid chromatographs; the dispersed autonomous correction mode includes: each liquid chromatograph in any region shortens the correction cycle by reducing its usage intensity according to a first preset reduction, or extends the correction cycle by increasing its usage intensity according to a first preset increment.
[0010] In some embodiments, employing the regional centralized correction mode specifically includes the following steps: Based on the historical data of each liquid chromatograph in any region, calculate its personalized periodic offset coefficient; specifically, it includes: performing linear fitting based on the wavelength deviation value of each chromatograph in the historical calibration period to obtain the slope characterizing the wavelength drift rate, and using the reciprocal of the slope as the personalized periodic offset coefficient. The calibration period obtained after adjusting the liquid chromatograph with the highest usage intensity in any of the regions is taken as the regional reference period; The final calibration cycle for each of the remaining liquid chromatographs in any given region is equal to the regional baseline cycle multiplied by the personalized cycle offset coefficient.
[0011] In some embodiments, the method further includes the step of: if, within a calibration period, the user manually triggers or receives a wavelength calibration task from a remote terminal, the user executes the wavelength calibration task and records this calibration as an aperiodic calibration task. Obtain the time interval between the non-periodic correction task and the previous periodic correction task; Calculate the ratio R of the time interval to the current correction period. If R < the first proportional threshold, the correction period is shortened according to the second preset reduction. If R ≥ the second proportional threshold, the correction period is extended according to the second preset increment. If the first proportional threshold ≤ R < the second proportional threshold, keep the current correction period unchanged; The adjusted period will be used as the new correction period, and the end time of this non-periodic correction task will be used as the start time of the next correction period.
[0012] In some embodiments, the steps further include: Receive remote tasks sent by the host computer and add the remote tasks to the task queue; Determine whether the priority of the remote task is higher than the priority of the currently executing task; If the value is high, interrupt the currently executing task to execute the remote task; The task queue includes data acquisition tasks, data reporting tasks, parameter configuration tasks, and periodic detection tasks, with priority decreasing in descending order. The parameter configuration task includes the remote task; the periodic detection task includes the wavelength correction task.
[0013] A second aspect of the present invention is to provide a control circuit for an ultraviolet-visible detector in a liquid chromatograph, comprising: a photoelectric sensor, a first amplifier, an ADC, three monochromator drive circuits, and a controller; The output of the photoelectric sensor is connected to the controller via a first amplifier and an ADC. The input terminals of the three monochromator drive circuits are all connected to the controller; The controller is configured to generate a PWM signal to drive the monochromator through three monochromator drive circuits, and to periodically perform wavelength correction according to a preset correction period; and to obtain the usage intensity in the most recent correction period; the usage intensity = K1 * normalized usage count + K2 * normalized total running time; and to determine whether the usage intensity in the most recent correction period is greater than or equal to a second preset threshold and less than a first preset threshold; if the usage intensity is greater than or equal to the first preset threshold, the correction period is shortened by a first preset reduction, and periodic wavelength correction is performed according to the adjusted correction period; if the usage intensity is less than the second preset threshold, the correction period is extended by a first preset increment, and periodic wavelength correction is performed according to the adjusted correction period; the second preset threshold is less than the first preset threshold; if the usage intensity is greater than or equal to the second preset threshold and less than the first preset threshold, the current correction period is maintained.
[0014] In some embodiments, the circuit further includes an Ethernet communication module electrically connected to the controller. The controller is also configured to perform periodic calibration based on control commands issued by the host computer according to the Ethernet communication module; the control commands are issued by the host computer when it starts the regional centralized calibration mode or the decentralized autonomous calibration mode after obtaining the usage intensity of each liquid chromatograph in each region in the most recent calibration period through the Internet of Things and identifying the distribution of the usage intensity of all liquid chromatographs in each region. If the distribution meets a first preset condition, a regional centralized correction mode is adopted. The first preset condition is that the difference between the usage intensity and the mean of each liquid chromatograph in the current region is less than or equal to a preset difference threshold. The regional centralized correction mode includes: if the minimum usage intensity is greater than or equal to the first preset threshold, shortening the correction cycle of the chromatograph corresponding to the maximum usage intensity by a first preset reduction, and using the correction cycle as the correction cycle of all chromatographs in the current region; if the maximum usage intensity is less than a second preset threshold, extending the correction cycle of the chromatograph corresponding to the middle usage intensity by a first preset increment, and using the correction cycle as the correction cycle of all chromatographs in the same region. If the distribution meets the second preset condition, and N is greater than or equal to a preset quantity threshold, then a dispersed autonomous correction mode is adopted for the N liquid chromatographs; the second preset condition is: the difference between the usage intensity and the mean of at least N liquid chromatographs in the current area is greater than a preset difference threshold; the dispersed autonomous correction mode includes: each liquid chromatograph in the current area shortens the correction cycle according to a first preset reduction in its usage intensity, or increases the correction cycle according to a first preset increment.
[0015] In some embodiments, the circuit further includes: a temperature sensor, a second amplifier, a leakage detection module, a third amplifier, a monochromator position detection module, and a deuterium lamp driving circuit, a tungsten lamp driving circuit, and an RS-485 communication interface electrically connected to the controller. The output of the temperature sensor is connected to the controller via a second amplifier; The output of the leakage detection module is connected to the controller via a third amplifier; The monochromator position detection module is electrically connected to the controller.
[0016] In some embodiments, the circuit further includes: a power management module electrically connected to the controller; the power management module includes: two sets of isolated DC / DC modules that supply power to the analog circuit and the microcontroller circuit respectively; and a set of non-isolated DC / DC circuits that supply power to the external I / O interface circuit.
[0017] A third aspect of the present invention is to provide a centralized monitoring system for a liquid chromatograph, comprising: Multiple liquid chromatographs, each including the control circuit described in any embodiment of the present invention; the liquid chromatographs are configured to periodically perform wavelength calibration at a preset calibration cycle; and the calibration cycle is dynamically adjusted according to the usage intensity within the most recent calibration cycle; the usage intensity = K1 * standardized number of uses + K2 * standardized total running time; The host computer is configured to acquire the usage intensity of each liquid chromatograph in each region during the most recent calibration period via the Internet of Things; and identify the distribution of usage intensity of all liquid chromatographs in each region; if the distribution meets a first preset condition, a regional centralized calibration mode is adopted; the first preset condition is: the difference between the usage intensity of each liquid chromatograph in the current region and the mean is less than or equal to a preset difference threshold; the regional centralized calibration mode includes: if the minimum usage intensity is greater than or equal to the first preset threshold, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period as the calibration period of all chromatographs in the current region; ... of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period of the chromatograph corresponding to the maximum usage intensity according to If the usage intensity is less than the second preset threshold, the calibration cycle of the corresponding chromatograph with the middle usage intensity is extended by the first preset increment, and the calibration cycle is used as the calibration cycle of all chromatographs in the same area; if the distribution meets the second preset condition, and N is greater than or equal to the preset quantity threshold, then a dispersed autonomous calibration mode is adopted for the N liquid chromatographs; the second preset condition is: the difference between the usage intensity and the mean of at least N liquid chromatographs in the current area is greater than the preset difference threshold; the dispersed autonomous calibration mode includes: each liquid chromatograph in the current area shortens the calibration cycle by reducing its usage intensity by the first preset amount, or increases the calibration cycle by the first preset increment.
[0018] Beneficial technical effects: Firstly, this invention proposes a mechanism for dynamically adjusting the wavelength calibration cycle based on usage intensity. This mechanism can fully consider the dynamic load of the instrument's actual operation (for example, the usage intensity of the chromatograph varies greatly at different times, under different tasks, and in different environments, which has a drastically different impact on the wear and tear of key components (such as deuterium lamps) and wavelength stability). This ensures the timeliness and efficiency of wavelength calibration to a certain extent, thereby helping to improve the accuracy of chromatograph detection and analysis data.
[0019] Secondly, the present invention determines the applicable regional centralized calibration mode or decentralized autonomous calibration mode by using the intensity distribution (e.g., the regional centralized calibration mode is applied to multiple liquid chromatographs that meet the first preset conditions, and the decentralized autonomous calibration mode is applied to some liquid chromatographs that meet the second preset conditions), and then applies the same or different calibration cycles to multiple liquid chromatographs in the same region, thereby achieving a better balance between the efficiency of unified management and the accuracy of individual differences.
[0020] Furthermore, under the regional centralized calibration mode, the regional reference cycle (i.e., the uniformly applicable calibration cycle) is also finely adjusted by a personalized cycle offset coefficient to make the calibration cycle more suitable for the individual conditions of the liquid chromatograph, thereby further improving the efficiency of wavelength calibration.
[0021] Thirdly, this invention proposes a periodic dynamic adjustment mechanism that utilizes feedback from non-periodic calibration tasks to adjust the calibration cycle. This mechanism allows for earlier monitoring of abnormal wavelength fluctuations in the chromatograph and adaptive adjustments to the wavelength calibration cycle. Furthermore, using non-periodic calibration tasks as a reference characterization of the chromatograph's operating status further enhances the timeliness and effectiveness of wavelength calibration. Attached Figure Description
[0022] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. In all the drawings, similar elements or parts are generally identified by similar reference numerals. The elements or parts in the drawings are not necessarily drawn to scale. Obviously, the drawings described below are some embodiments of the present invention, and those skilled in the art can obtain other drawings based on these drawings without any creative effort.
[0023] Figure 1 A schematic flowchart of a wavelength calibration method for a liquid chromatograph provided by the present invention; Figure 2 This invention provides a schematic diagram of the structure of a centralized monitoring system for a liquid chromatograph. Figure 3 A structural example diagram of the liquid chromatograph provided by the present invention; Figure 4 A structural example diagram of the ultraviolet-visible light detector control circuit provided by the present invention; Figure 5 This is a schematic block diagram of the structure of a computer device provided by the present invention. Detailed Implementation
[0024] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.
[0025] In this document, suffixes such as "module," "part," or "unit" used to denote elements are used only for the purpose of illustrative purposes and have no specific meaning in themselves. Therefore, "module," "part," or "unit" may be used interchangeably.
[0026] In this document, the terms "upper," "lower," "inner," "outer," "front," "rear," "one end," and "the other end," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the present invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.
[0027] In this document, unless otherwise explicitly specified and limited, the terms "installed," "equipped with," "connected," etc., should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, a direct connection, or an indirect connection through an intermediate medium; it can be a connection within two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.
[0028] In this document, "and / or" includes any and all combinations of one or more of the listed related items.
[0029] In this article, "multiple" means two or more, that is, it includes two, three, four, five, etc.
[0030] As used in this specification, the term "about" typically means + / -5% of the value, more typically + / -4% of the value, more typically + / -3% of the value, more typically + / -2% of the value, even more typically + / -1% of the value, and even more typically + / -0.5% of the value.
[0031] In this specification, certain embodiments may be disclosed in a range-bound format. It should be understood that this "range-bound" description is merely for convenience and brevity and should not be construed as a rigid limitation on the disclosed range. Therefore, the description of a range should be considered as having specifically disclosed all possible subranges and the individual numerical values within those ranges. For example, a description of the range 1-6 should be considered as having specifically disclosed subranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., and the individual numbers within those ranges, such as 1, 2, 3, 4, 5, and 6. This rule applies regardless of the breadth of the range.
[0032] Definition of noun: The host computer is used to centrally manage all the chromatographs that communicate with it. For example, it can acquire various parameters of each chromatograph, such as temperature and wavelength, through the Internet of Things, and perform data analysis and issue control commands (such as controlling the heating module to heat, or adjusting the wavelength calibration cycle).
[0033] A liquid chromatograph (or, as referred to in this text, a chromatograph, device, or instrument) can be an instrument that uses the difference in the distribution ratio of a mixture between a liquid and a solid or between two immiscible liquids to first separate the mixture and then analyze and identify it.
[0034] In other words, a liquid chromatograph is an instrument that uses the difference in the distribution ratio of a mixture between a mobile phase and a stationary phase to first separate the mixture, and then analyze and identify it. Please see [link to relevant documentation]. Figure 3 A liquid chromatograph mainly consists of an injector, a pump, a column oven, and a detector, all connected by pipelines.
[0035] Example 1: The applicant noted that maintaining wavelength accuracy during the use of a liquid chromatograph relies heavily on manual verification. Users or maintenance personnel need to judge whether a wavelength shift has occurred based on experience, and manually trigger the chromatograph's built-in calibration process or contact a specialist after discovering a problem. On the one hand, this method is highly dependent on human intervention, and differences in experience or negligence may lead to inconsistent judgments or omissions; on the other hand, subtle early shifts are difficult to detect immediately, often only being discovered when they evolve into significant deviations that may have already affected data reliability. Therefore, there is a certain lag between the occurrence of a shift and its detection.
[0036] In response, this invention proposes a mechanism for dynamically adjusting the wavelength calibration cycle based on usage intensity. This mechanism can fully consider the dynamic load of the instrument's actual operation (for example, the usage intensity of the chromatograph varies greatly at different times, under different tasks, and in different environments, which has a significant impact on the wear and tear of key components (such as deuterium lamps) and wavelength stability). This ensures the timeliness and efficiency of wavelength calibration to a certain extent, thereby helping to improve the accuracy of chromatograph detection and analysis data.
[0037] Specifically, when the chromatograph is used at a low intensity, the calibration cycle can be appropriately lengthened to reduce the number of wavelength calibrations and avoid or reduce unnecessary waste of resources and wear and tear on components. When the instrument is running under continuous high load, the calibration cycle can be appropriately shortened to increase the number of wavelength calibrations. This helps to cope with accelerated wavelength drift and thus improve the reliability of chromatograph data.
[0038] From another perspective, the dynamic adjustment mechanism of calibration cycle proposed in this invention can adjust the calibration cycle according to the actual usage (i.e., usage intensity). This helps to reduce the dependence on manual intervention (i.e., maintenance personnel do not need to formulate and adjust calibration plans for each chromatograph individually), thereby improving the automation level of chromatograph wavelength calibration.
[0039] Please see Figure 1 In some embodiments, the present invention provides a wavelength calibration method for a liquid chromatograph, comprising the steps of: S101, performs wavelength correction periodically according to a preset correction cycle; S102, Obtain the usage intensity of the liquid chromatograph during the most recent calibration period; the usage intensity = K1 * standardized number of uses + K2 * standardized total running time; S103, determine whether the usage intensity within the most recent correction period is greater than or equal to a second preset threshold and less than a first preset threshold; the second preset threshold is less than the first preset threshold; S104, if the intensity of use is greater than or equal to the first preset threshold, shorten the correction period according to the first preset reduction, and perform periodic wavelength correction according to the adjusted correction period; S105, if the intensity of use is less than the second preset threshold, extend the correction period by the first preset increment, and perform periodic wavelength correction according to the adjusted correction period; S106, if the intensity of use is greater than or equal to the second preset threshold, but less than the first preset threshold, maintain the current correction cycle.
[0040] In some embodiments, the preset calibration cycle (i.e., the initial calibration cycle) in step S101 can be set by the operator according to the actual use of each chromatograph or preset at the factory.
[0041] In some embodiments, in step S102, the preset calibration cycle of the chromatograph, i.e. the initial calibration cycle, is dynamically adjusted according to the usage intensity of the chromatograph in the most recent calibration cycle (e.g., in the previous calibration cycle or in the two most recent calibration cycles). This allows calibration to be flexibly triggered according to the actual wear and tear of the equipment, avoiding or reducing the situation of untimely or premature calibration caused by calibration based on a fixed calibration cycle.
[0042] For example, if the HPLC instrument has been used intensively in the most recent calibration period (e.g., greater than or equal to the first preset threshold), it may indicate heavy equipment usage and that its components have just undergone accelerated wear. In this case, shortening the calibration period allows for earlier identification and correction of wavelength drift, effectively avoiding calibration lag. Similarly, if the usage intensity in the most recent calibration period is low (e.g., less than or equal to the second preset threshold), it may indicate low equipment usage. Although its components may have experienced wear, it may be less than normal wear and tear. Therefore, the calibration period can be appropriately extended. Likewise, if the usage intensity in the most recent calibration period is within the normal range, i.e., greater than the second preset threshold and less than the first preset threshold, then periodic calibration can be performed according to the preset calibration period.
[0043] The number of uses can quantify the wavelength drift and lifespan degradation caused by the changes in current and temperature experienced by components such as the deuterium lamp during multiple power-on and power-off cycles. For example, each power-on and power-off cycle causes thermal expansion and contraction in the optical system (especially the light source and monochromator), which may result in minute mechanical deformation or lens position drift. In addition, frequent power-on of circuit components may also introduce minute parameter changes.
[0044] The total operating time quantifies the slow wavelength shift caused by the continuous consumption of filament luminescent material and the gradual aging of optical components. The total operating time is directly related to the cumulative aging of core optical components (such as deuterium lamps). The spectral output characteristics of deuterium lamps undergo a slow and irreversible drift with increasing illumination time, which is the primary source of wavelength deviation. In other words, the longer the operating time, the more significant the effects of lamp brightness decay and changes in internal gas composition, resulting in a greater wavelength drift. Therefore, the weight K2 corresponding to the total operating time is the dominant factor, meaning K2 is greater than the weight K1 of the number of uses.
[0045] For example, K2 can be set to K1 during initial parameter settings, with specific values being empirical, such as K1=0.4 and K2=0.6. The specific weights (K1, K2) can be determined before factory settings by performing regression analysis on a large amount of historical instrument data; this is existing technology and will not be described further here.
[0046] It should be understood that the calculated usage intensity is a dimensionless value. For example, the standardized number of uses = actual number of uses in the most recent period / reference number of uses; the standardized total running time = actual total running time in the period / reference total running time. The reference number of uses can be the average number of uses for all historical calibration periods of the chromatograph in the historical database; correspondingly, the reference total running time can be the average total running time for all historical calibration periods of the chromatograph in the historical database.
[0047] For example, use strength = K1*(N / N_ref) + K2*(T / T_ref).
[0048] Where: N is the actual number of uses within the most recent calibration period. N_ref is a preset reference number of uses (e.g., 10 times / cycle). T is the actual total running time within the most recent calibration period. T_ref is a preset reference running time (e.g., 40 hours / cycle).
[0049] In some embodiments, the first preset reduction and / or the first preset increment can be a specific time length (such as 1 hour or 1 week, which can be determined based on empirical values).
[0050] For example, the adjusted correction period = the preset correction period + the first preset increment, or the adjusted correction period = the preset correction period - the first preset decrement.
[0051] Furthermore, in other embodiments, different first preset reductions (or first preset increments) can be set based on the intensity difference that exceeds (or falls below) a first preset threshold (or a second preset threshold).
[0052] For example, intensity difference levels can be pre-defined, and a corresponding preset reduction can be preset for each intensity difference level. For instance, if the intensity exceeds a first preset threshold by 50% (i.e., the intensity difference reaches the highest level), a larger first preset reduction can be set (i.e., the maximum preset reduction corresponding to the highest intensity difference) to significantly shorten the correction cycle. If the intensity exceeds the first preset threshold by 10% (i.e., the intensity difference is the lowest level), a smaller first preset reduction can be set (i.e., the minimum preset reduction corresponding to the lowest intensity difference).
[0053] In some embodiments, periodic wavelength calibration refers to automatically and repeatedly performing wavelength accuracy checks and corrections at certain time intervals, with the specific calibration process built into the chromatograph.
[0054] In some embodiments, the most recent correction period may refer to at least one correction period prior to the current correction period. For example, the previous correction period.
[0055] In some embodiments, the first and second preset thresholds are typically set based on industry experience. Alternatively, they can be pre-determined based on historical data from a large number of chromatographs. If the usage intensity of a chromatograph is greater than or equal to the first preset threshold, it indicates that the chromatograph is under high usage intensity. In this case, equipment wear and tear is significant, and the resulting deviation may not be corrected by the preset calibration period. If the usage intensity of a chromatograph is less than or equal to the second preset threshold, it indicates that the chromatograph is under low usage intensity. In this case, equipment wear and tear is minimal, and the resulting deviation is very small. Correction according to the preset calibration period may result in over-calibration. If the usage intensity of a chromatograph is less than the first preset threshold but greater than or equal to the second preset threshold, the usage intensity is moderate, and the deviation caused by equipment wear and tear can be corrected by the preset calibration period.
[0056] Example 2: The applicant also noted that for a large number of chromatographs that need to be centrally managed in the same laboratory or testing center, all the detection and analysis data of the chromatographs will be continuously uploaded to the host computer via the Internet of Things. This will greatly increase the load on the communication link and the host system, and it will be difficult for monitoring personnel to quickly identify valid data or abnormal situations from the complex information. On the other hand, the large amount of calculation will also increase the overall energy consumption.
[0057] To address this, the present invention proposes another calibration method, which includes the steps described in Embodiment 1 above. The difference is that this embodiment no longer performs wavelength calibration individually for each liquid chromatograph, but instead proposes a zoned wavelength calibration mechanism based on the wavelength calibration of multiple liquid chromatographs. Specifically, in step S101, the initial calibration cycle for each liquid chromatograph is set, and in step S102, the usage intensity of each chromatograph is obtained. The usage intensity distribution of all liquid chromatographs belonging to the same region (dividing multiple spatially adjacent liquid chromatographs into one region) is statistically analyzed. Different calibration modes are selected based on different usage intensity distributions, thereby improving the overall equipment management efficiency and reducing the complexity of operation and maintenance to a certain extent. Simultaneously, adjusting the calibration cycle of equipment in the same region in batches or in a decentralized manner according to different calibration modes also helps to balance management efficiency and calibration accuracy. For example, when the usage intensity of each instrument in the same region is very similar and high, a centralized regional calibration mode is preferred to avoid the problems of high management difficulty and high computational cost that may occur when calibrating the wavelength of each instrument in a decentralized manner. When the usage intensity of each chromatograph in the same area is relatively dispersed, a decentralized self-calibration mode is adopted to avoid the introduction of large errors by ignoring individualization when using a centralized calibration mode.
[0058] Specifically, after executing step S102, the method further includes the following steps: S201, the host computer obtains the usage intensity of each liquid chromatograph in each region during the most recent calibration period through the Internet of Things; S202, the host computer determines whether the difference between the usage intensity and the mean of each liquid chromatograph in each region is less than or equal to a preset difference threshold (i.e., the host computer identifies the distribution of usage intensity of all liquid chromatographs in each region). If the distribution meets the first preset condition (i.e., the difference between the usage intensity of each liquid chromatograph in the same area and the average usage intensity is less than or equal to a preset difference threshold, i.e., the distribution is relatively uniform), and the minimum usage intensity is greater than or equal to the first preset threshold (i.e., all chromatographs in the same area are at high usage intensity), then proceed to step S203a. If the distribution meets the first preset condition, and the maximum usage intensity is less than the second preset threshold (i.e., all chromatographs in the same area are at low usage intensity), proceed to step S203b. If the distribution meets the first preset condition, and the usage intensity of some chromatographs is less than the first preset threshold, while the usage intensity of others is greater than or equal to the first preset threshold (i.e., some chromatographs in the same area are at high usage intensity, while others are at normal usage intensity and / or low usage intensity), or if the usage intensity of some chromatographs is greater than or equal to the second preset threshold (i.e., some chromatographs in the same area are at low usage intensity, while others are at high usage intensity and / or normal usage intensity), then proceed to step S203c. If the distribution meets the second preset condition (i.e., the difference between the usage intensity and the mean of at least N liquid chromatographs in the same area is greater than the preset difference threshold), proceed to step S204; S203a, adopting the first regional centralized calibration mode: shortening the calibration cycle of the chromatograph corresponding to the maximum usage intensity according to the first preset reduction, and using the calibration cycle as the calibration cycle of all chromatographs in the same region; S203b, adopting the second regional centralized calibration mode: shortening the calibration cycle of the chromatograph with the middle usage intensity (i.e., the chromatograph in the middle position when sorted by usage intensity from large to small or from small to large) according to the first preset reduction, and using the calibration cycle as the calibration cycle of all chromatographs in the same region. S203c, adopts the third region centralized calibration mode: shortens the calibration cycle of the chromatograph whose usage intensity is closest to the average usage intensity according to the first preset reduction (if multiple exist, one can be selected), and uses the calibration cycle as the calibration cycle of all chromatographs in the same region. S204 adopts a distributed autonomous correction mode; The decentralized autonomous calibration mode is as follows: each liquid chromatograph in the same area / group shortens the calibration cycle according to the first preset reduction based on its own usage intensity (for example, if the usage intensity of a liquid chromatograph is greater than or equal to the first preset threshold, its calibration cycle is shortened), or increases the calibration cycle according to the first preset increment (for example, if the usage intensity of a liquid chromatograph is less than the second preset threshold, its calibration cycle is extended).
[0059] In some other embodiments, before performing step S204, the following step is included: Determine whether N is greater than or equal to a preset quantity threshold (e.g., M / 3, where M is the total number of all chromatographs in the same area). If so, divide the N chromatographs into a group and adopt a dispersed autonomous calibration mode; at the same time, divide the remaining chromatographs into another group and match different calibration modes based on the usage intensity within the group; if N is less than the preset quantity threshold, a regional centralized calibration mode can be adopted.
[0060] As mentioned earlier, since this involves the remaining portion of the liquid chromatographs (i.e., MN), the difference between the usage intensity of each liquid chromatograph within this group and the average usage intensity of this area is less than or equal to a preset difference threshold, meaning they are all close to the average. Therefore, If the minimum usage intensity in the group is greater than or equal to the first preset threshold (i.e., all are at high usage intensity), the calibration cycle of the chromatograph corresponding to the maximum usage intensity in the group is shortened according to the first preset reduction, and the calibration cycle is used as the calibration cycle of all chromatographs in the group (i.e., step S203a is executed, except that the calibration cycle of the maximum usage intensity in the group is used as the benchmark). If the highest usage intensity in the group is less than the second preset threshold (i.e., all are at low usage intensity), the calibration cycle of the chromatograph with the middle usage intensity in the group (i.e., the chromatograph in the middle position when sorted by usage intensity from largest to smallest or from smallest to largest) is shortened according to the first preset reduction, and the calibration cycle is used as the calibration cycle of all chromatographs in the group; (i.e., step S203b is executed, except that only the calibration cycle of the middle usage intensity in the group is used as the benchmark). If the usage intensity of some chromatographs in the group is less than the first preset threshold, and the usage intensity of another part is greater than or equal to the first preset threshold (i.e., some are at high usage intensity, and some are at normal usage intensity and / or low usage intensity), or if the usage intensity of some chromatographs in the group is greater than or equal to the second preset threshold (i.e., some are at low usage intensity, and another part are at high usage intensity and / or normal usage intensity), then step S203c is executed, that is, the calibration cycle of the chromatograph whose usage intensity in the group is closest to the average usage intensity of the group (if multiple exist, one can be selected) is shortened according to the first preset reduction, and the calibration cycle is used as the calibration cycle of all chromatographs in the group.
[0061] In some embodiments, spatial adjacency mainly refers to the fact that each chromatograph is located in the same or adjacent physical space unit, so that daily inspection and maintenance personnel can access all chromatographs from the first chromatograph in a short time (e.g., within 15 minutes).
[0062] In some embodiments, the distribution of usage intensity can characterize whether the workload of multiple liquid chromatographs in the same area is similar. The distribution of usage intensity can be determined by the difference between the usage intensity of each liquid chromatograph and the mean (if the difference between the usage intensity of each liquid chromatograph and the mean is small, it indicates that the usage intensity of each chromatograph is close and near the mean; if the difference between the usage intensity of multiple liquid chromatographs and the mean is large, it indicates that the usage intensity of each chromatograph is not close and deviates significantly from the mean).
[0063] In some embodiments, if the usage intensity of each instrument within a region is very similar (the difference between the usage intensity of each liquid chromatograph and the mean is less than or equal to a preset difference threshold), and the usage intensity is high (e.g., the minimum usage intensity is greater than or equal to a first preset intensity threshold), a uniform, smaller calibration period can be generated based on the highest usage intensity. This batch calibration mechanism allows all chromatographs within the group to be calibrated using a uniform calibration period, thereby reducing operational complexity.
[0064] In other words, when the usage intensity of instruments within the same area is very similar and high, a regional centralized calibration mode is suitable. Compared to setting individual calibration cycles for each chromatograph, this significantly reduces the complexity of centralized management. Furthermore, the instruments with the highest usage intensity typically have the highest risk of drift within the same area. Therefore, using the highest intensity as a baseline ensures that the instruments with the highest risk are calibrated in time before their performance may drift significantly, thus establishing a unified calibration baseline for the entire area. For other instruments within the same area whose usage intensity is not the highest, since the usage intensity of instruments within the same area is similar and high, the additional losses or costs incurred by early calibration (such as the need to light the deuterium lamp and run it for a period of time after each calibration) are acceptable. In other words, the focus shifts from simply pursuing high precision for individual instruments to pursuing overall system efficiency without significantly reducing the precision of individual instruments—that is, while ensuring the basic precision of each instrument.
[0065] In addition, for cases where the usage intensity is uniformly distributed and the usage intensity is generally low, adjusting the calibration cycle of all chromatographs in the group based on the calibration cycle corresponding to the chromatograph with moderate usage intensity can also achieve a good balance between calibration accuracy and calibration cost.
[0066] Alternatively, for cases where the usage intensity is evenly distributed but varies, the calibration cycle of all chromatographs in the group can be adjusted based on the calibration cycle corresponding to the chromatograph with the average usage intensity. This can also achieve a good balance between calibration accuracy and calibration cost.
[0067] In other embodiments, if the usage intensity of multiple liquid chromatographs in the same area varies greatly (e.g., the difference between the usage intensity of at least N liquid chromatographs and the mean is greater than a preset difference threshold), and the usage intensity of each of them is relatively high (e.g., the minimum usage intensity in the same area is greater than or equal to a first preset intensity threshold), then the calibration cycle can be adjusted based on the actual usage intensity of each device.
[0068] In other words, for multiple devices with significantly different and high usage intensities, the present invention preferably adjusts the calibration cycle based on the usage intensity of each device, thereby ensuring the actual compatibility of the calibration cycle with the chromatograph equipment and improving the reliability of the chromatograph detection and analysis data.
[0069] In other embodiments, the single-machine periodic calibration in Embodiment 1 is typically suitable for scenarios with a small number of chromatographs; while the partitioned calibration mechanism in this embodiment is suitable for scenarios with a large number of chromatographs that require centralized management. Of course, the two mechanisms can coexist. In this case, partitioned periodic calibration is preferred. If the two mechanisms conflict, the shortest calibration cycle is used as the calibration cycle for the corresponding chromatograph.
[0070] Furthermore, in some other embodiments, before shortening the calibration cycle of the chromatograph corresponding to the maximum usage intensity according to the first preset reduction in step S203a, and using the calibration cycle as the calibration cycle of all chromatographs in the same area, the method further includes the step of: adjusting the calibration cycle based on the personalized cycle offset coefficient of each chromatograph, and using the adjusted calibration cycle as the latest calibration cycle of the corresponding chromatograph; specifically including the following steps: Based on historical data of each liquid chromatograph in the current region, calculate its personalized periodic offset coefficient; including: performing linear fitting based on the wavelength deviation value (preferably, the absolute value) of each chromatograph within the historical calibration period (preferably within the most recent K calibration periods) to obtain the slope characterizing the wavelength drift rate, and using the reciprocal of the slope as the personalized periodic offset coefficient of the corresponding chromatograph. The calibration period obtained after adjusting the liquid chromatograph with the highest usage intensity in the current region is used as the regional reference period; The final calibration cycle for each liquid chromatograph in the current region is equal to the regional baseline cycle multiplied by the personalized cycle offset coefficient.
[0071] In some embodiments, the personalized cycle offset coefficient is negatively correlated with the total operating time of the corresponding device since it has been put into use (device working time); and / or, the personalized cycle offset coefficient is negatively correlated with the cumulative lighting time of its key optical components (such as deuterium lamps) (working time of specific components in the device).
[0072] For example: Personalized cycle offset coefficient = base coefficient * exp(-cumulative running time / life constant).
[0073] The base coefficient can be a preset value that is dynamically set based on historical data (such as failure frequency). For example, the higher the failure frequency, the smaller the corresponding base coefficient.
[0074] The cumulative runtime refers to the total runtime, that is, the operating time when the device is powered on. The cumulative runtime is the sum of the overall operating time of the device, while the cumulative lighting time refers to the working period of a specific component (such as the light source) in the device.
[0075] The lifespan constant is a device attribute that characterizes the expected lifespan of a critical component (light source). A smaller value indicates that the component ages faster. For example, the lifespan constant can be a manufacturer-recommended value.
[0076] The slope of the wavelength drift rate can be calculated as follows: record the first and second wavelength values before and after each correction, and obtain multiple wavelength deviation values by subtracting multiple first wavelength values and multiple second wavelength values; obtain multiple time differences corresponding to multiple first wavelength values and multiple second wavelength values (i.e., the difference between the correction period before correction and the correction period after correction, for example, the correction period before correction is T, and the correction period after correction is T+n, where n is the time difference); the slope of the wavelength drift rate can be obtained by linearly fitting multiple ratios of multiple wavelength deviation values and multiple time differences.
[0077] For example, the method of linear fitting of multiple ratios can be obtained from existing technologies, such as least squares linear fitting, and the present invention does not limit this.
[0078] The personalized period offset coefficient is negatively correlated with the slope. That is, the greater the wavelength drift rate (i.e., the slope), the smaller the personalized period offset coefficient, and the shorter the final calibration cycle of the liquid chromatograph.
[0079] It should be understood that a higher wavelength drift rate of a liquid chromatograph within a historical calibration period indicates a greater degree of wear and tear or aging of the equipment (this application does not consider equipment failure), resulting in poorer stability. Even if not under the most intensive use, the risk of exceeding the allowable error range within a short period is higher. Therefore, it is necessary to further shorten the calibration period based on the regional baseline period. This allows for assessment of the equipment's condition based on its historical performance and advance planning, while also improving adaptability to individual equipment under centralized calibration mode.
[0080] In other words, the faster the wavelength drift rate of a chromatograph, the shorter its calibration cycle is relative to the regional reference cycle. Through this synergistic mechanism of regional centralized calibration and individual device fine-tuning, both management complexity and individual accuracy can be balanced, improving the adaptability and reliability of the calibration cycle.
[0081] For example, the value range of the personalized cycle offset coefficient is constrained within the preset range [0.5, 1.5] to ensure that the calibration cycle of each device in the region maintains individual adaptability, and does not deviate too much from the regional reference cycle, thus making it impossible to carry out centralized regional management.
[0082] Generally speaking, the more intensive the use of a chromatograph, the faster the hardware wears out or ages, and the greater the risk of wavelength drift. By using the calibration cycle obtained after adjusting the liquid chromatograph with the highest usage intensity in the current area as the regional benchmark cycle, the calibration cycle of all equipment in the area can be shortened more conservatively. This ensures that all equipment can be calibrated in a timely manner or in advance, avoiding the problem of untimely calibration due to excessively long calibration cycles.
[0083] Alternatively, while shorter calibration cycles may result in other instruments being prematurely or slightly overcalibrated with less intensive use, the resulting costs (e.g., premature calibration for wavelengths within an acceptable drift range) are acceptable because the usage intensity of each liquid chromatograph in the regional centralized calibration mode is relatively similar, and the personalized cycle offset coefficient can adaptively correct for the regional reference cycle.
[0084] It should be understood that this invention is particularly applicable to scenarios requiring centralized management of a large number of liquid chromatographs (such as a single testing center). Specifically, this invention determines whether a centralized calibration mode or a decentralized autonomous calibration mode is applicable to a given area by using the distribution of intensity, thereby applying the same or different calibration cycles to multiple liquid chromatographs within the same area. This achieves a better balance between the efficiency of unified management and the accuracy of individual differences.
[0085] Furthermore, under the regional centralized calibration mode, the regional reference cycle (i.e., the uniformly applicable calibration cycle) is also finely adjusted by a personalized cycle offset coefficient to make the calibration cycle more suitable for the individual conditions of the liquid chromatograph, thereby further improving the efficiency of wavelength calibration.
[0086] Furthermore, in some other embodiments, the correction method includes, in addition to the steps of each embodiment, the following step: For each chromatograph, if the user manually triggers or receives a wavelength calibration task from the remote end within a calibration cycle, the wavelength calibration task is executed and the calibration is recorded as a non-periodic calibration task. Obtain the time interval between the non-periodic correction task and the previous periodic correction task; Calculate the ratio R of the time interval to the current correction period. If R < the first proportional threshold (e.g., 15%), the correction period is shortened according to the second preset reduction. If R ≥ the second proportional threshold (e.g., 90%), extend the correction period according to the second preset increment. If the first proportional threshold ≤ R < the second proportional threshold, keep the current correction period unchanged; The adjusted period is used as the new correction period, and the start time of the next correction period is the time of this non-periodic correction task.
[0087] In some embodiments, users can perform non-periodic calibration of the instrument wavelength based on the actual operating conditions of the chromatograph (such as sudden drift causing data anomalies) to cope with unplanned emergencies.
[0088] In some embodiments, non-periodic calibration tasks can be manually triggered by the user. For example, during routine work, an operator may discover inaccurate wavelengths (such as abnormal peak elution or poor repeatability of standards) and manually initiate calibration directly on the instrument control panel. Alternatively, non-periodic calibration tasks can be calibration commands issued remotely to a designated chromatograph by an administrator or engineer at a remote monitoring center via an Internet of Things (IoT) system.
[0089] In some embodiments, if the time interval between the non-periodic calibration task and the previous periodic calibration task is close, that is, the ratio of the time interval to the current calibration cycle is small (e.g., R < first proportional threshold), it means that manual calibration is required again right after the periodic calibration is performed. This may indicate that the actual working state of the chromatograph has deviated from expectations, or that the wavelength stability of the chromatograph may have decreased. In this case, a second preset reduction can be adopted to shorten the calibration cycle.
[0090] In some embodiments, if the time interval between the non-periodic correction task and the previous periodic correction task is relatively long, i.e., the ratio of the time interval to the current correction period is large (e.g., R ≥ the second proportional threshold), it indicates that the non-periodic correction task is initiated near the end of the current correction period. This may indicate that the current correction period setting is relatively conservative, or that the non-periodic correction task is for preventative maintenance. In this case, the correction period can be appropriately extended by adopting the second preset increment.
[0091] In some embodiments, if the time interval between the non-periodic calibration task and the previous periodic calibration task is always equal, such as the first proportional threshold ≤ R < the second proportional threshold, it may indicate that the chromatograph is in normal condition and the current calibration cycle can be maintained to avoid over-adjusting the calibration cycle.
[0092] In other embodiments, the above adjustment process is not triggered simply by detecting a non-periodic correction task. Instead, the execution frequency of the non-periodic correction task is determined based on the time interval between the most recent (e.g., 3) non-periodic correction tasks. That is, the time interval between two adjacent non-periodic correction tasks is determined to be getting smaller. If so, the above subsequent adjustment process is triggered based on the time interval between the current non-periodic correction task and the previous periodic correction task.
[0093] It should be understood that this invention proposes a periodic dynamic adjustment mechanism that can adjust the calibration cycle by utilizing feedback from non-periodic calibration tasks. This mechanism can monitor abnormal fluctuations in chromatograph wavelengths earlier and adaptively adjust the wavelength calibration cycle. Furthermore, using non-periodic calibration tasks as a reference characterization of the chromatograph's operating status can further improve the timeliness and effectiveness of chromatograph wavelength calibration.
[0094] In some embodiments, a primary correction peak (e.g., the characteristic spectral line of a deuterium lamp at 486.0 nm or 656.1 nm, or the absorption peak of a standard material such as holmium glass at a specific position) is used to calculate and correct wavelength deviations. However, the correction system itself may contain errors (such as nonlinear errors), and successful correction at only one wavelength point does not guarantee accuracy across the entire wavelength range.
[0095] To verify the correction effect, other characteristic peaks (or verification peaks) can be used. These peaks are known, stable absorption peaks with wavelengths different from the main correction peak.
[0096] In some embodiments, the correction process further includes a step of verifying the correction result, specifically including: Scan other characteristic peaks to verify whether the accuracy of the corrected wavelength meets the requirements; If the conditions are met, the corrected wavelength will be used as the working wavelength for the next detection cycle. If the conditions are not met, an anomaly will be reported via the Internet of Things.
[0097] In some embodiments, other characteristic peaks used to verify the correction results must meet the following conditions: (1) Clear and stable: The characteristic peak should come from internationally recognized standard materials (such as holmium glass filters, certain rare earth element solutions), and its peak wavelength is known and highly stable.
[0098] (2) Appropriate spacing from the main correction peak: The wavelength of the verification peak should be sufficiently far from the main correction peak used to calculate the deviation (e.g., the main correction is at 241 nm, and the verification peak can be selected at 360 nm or 536 nm) to verify the effectiveness of the correction curve throughout the working band, rather than single-point accuracy.
[0099] (3) Sharp peak shape: The ideal verification peak should have steep rising and falling edges, which makes it easy for the algorithm to accurately identify the peak position.
[0100] (4) High signal-to-noise ratio: The signal strength of the peak should be high enough to ensure measurement accuracy.
[0101] In some embodiments, after calibration, the absolute error between the measured actual wavelength value of the verification peak and the standard wavelength value is less than or equal to a preset threshold. For example, according to pharmacopoeia or industry standards (such as USP), this threshold is typically set to ±1 nm. That is, if the difference between the measured value and the standard value is within ±1 nm, the calibration is considered successful and the wavelength accuracy meets the requirements.
[0102] The standard wavelength value can be obtained from certificates or authoritative databases of internationally recognized standard materials (such as holmium glass filters or solutions of certain rare earth elements). For example, a certain standard material has a very stable and sharp characteristic absorption peak in the ultraviolet region, and its standard wavelength value is identified as 486.02 nm. This value can be used to determine whether the instrument's wavelength is accurate.
[0103] The main calibration peak is an absorption peak obtained from the spectrum of a standard substance when the instrument actually measures it. Ideally, the position of this peak (i.e., the actual measured wavelength) should coincide with the standard wavelength. The core of calibration is to calculate the deviation between this actually measured main calibration peak and the known standard wavelength.
[0104] In some embodiments, the chromatograph can calculate the wavelength deviation by measuring the actual position of the main calibration peak and comparing it with the standard wavelength value, thereby driving a mechanical structure (such as a grating) to compensate and correct for the deviation.
[0105] In some embodiments, if the error exceeds the aforementioned threshold (e.g., >±1nm), it is considered unacceptable. In this case, the anomaly can be reported via the Internet of Things, indicating that maintenance personnel may need to intervene to check for deeper issues such as the exhaustion of the light source lifespan, optical system contamination, or mechanical failure.
[0106] In some embodiments, the wavelength calibration process may fail due to various reasons (such as contamination or failure of standard materials, transient noise interference of photoelectric sensors, slight jamming of monochromator mechanical positioning, etc.). In this case, the wavelength accuracy can be verified by scanning the characteristic peaks.
[0107] For example, if the corrected wavelength meets the requirements, it may indicate that the correction period is reasonable, and the corrected wavelength can continue to be used; however, if the corrected wavelength does not meet the requirements, it may indicate that the wavelength correction task cannot be completed automatically through the preset correction period. In this case, the abnormality can be reported through the Internet of Things to prompt manual intervention and avoid untimely correction.
[0108] In some embodiments, wavelength correction includes the steps of: The monochromator is driven to scan within a preset wavelength range of the characteristic absorption peaks of the standard substance; During the scanning process, light intensity signals are collected to obtain the spectral curve of the preset wavelength region; Obtain the actual wavelength corresponding to the peak value of the absorption peak in the spectral curve; The actual wavelength corresponding to the peak value of the absorption peak is compared with the standard wavelength corresponding to the standard peak value of the standard substance to obtain the wavelength deviation value, and the offset correction is performed based on the deviation value.
[0109] In some embodiments, the present invention can verify wavelength accuracy by scanning characteristic absorption peaks, locating the peak wavelength of the actual absorption peak, comparing it with a standard value and calculating the deviation, and finally correcting and compensating the deviation value. This is prior art and will not be described in detail here.
[0110] In some embodiments, the grating or prism in the monochromator (the core spectrometer) can be precisely rotated to vary the wavelength of the light transmitted through the monochromator within a small range (e.g., 480-492 nm) near the known characteristic peak of the standard material (e.g., the 486.0 nm peak of holmium glass), thereby converting the broadband light source (deuterium lamp / tungsten lamp) into monochromatic light with precisely controllable wavelength, establishing a benchmark for measurement.
[0111] In some embodiments, at each wavelength step point, the photoelectric sensor measures the light intensity transmitted through a standard material. Through analog-to-digital conversion, a series of wavelength-intensity data points are plotted into a transmittance spectrum curve (represented as an absorption valley for the absorbing material).
[0112] In some embodiments, mathematical analysis (such as differentiation or curve fitting) can be performed on the obtained spectral curve to obtain the wavelength value corresponding to the lowest point of the absorption valley (or the point where the derivative crosses zero).
[0113] In some embodiments, the wavelength deviation Δλ is obtained by subtracting the actual wavelength value from the absolute standard value (e.g., 486.0 nm) specified on the standard material certificate. Subsequently, a compensation value can be generated based on Δλ and written into the monochromator's control system (e.g., to update the wavelength-grating position lookup table).
[0114] For example, offset correction based on the deviation value may include the following steps: when the user sets that a target wavelength (e.g., 254 nm) needs to be detected, the controller can issue a command to the monochromator drive system to actually move to a mechanical position corresponding to the target wavelength - wavelength deviation Δλ. This compensates for the error value by aligning the instrument with the offset position, so that the wavelength actually projected is exactly the target wavelength value.
[0115] In some embodiments, the steps further include: Receive remote tasks sent by the host computer and add the remote tasks to the task queue; Determine whether the priority of the remote task is higher than the priority of the currently executing task; If the value is high, interrupt the currently executing task to execute the remote task; The task queue includes data acquisition tasks, data reporting tasks, parameter configuration tasks, and periodic detection tasks, with priority decreasing in descending order. The parameter configuration task includes the remote task; the periodic detection task includes the wavelength correction task. For example, periodic correction is performed according to the aforementioned correction period.
[0116] In some embodiments, the priority of the task queue can also be sorted by the user according to their actual needs.
[0117] Among them, the data acquisition task has the highest priority, which can ensure that the detector signal is continuously and completely acquired, thereby avoiding problems such as chromatographic peak distortion and data point loss caused by signal interruption.
[0118] For example, when the computer system is performing wavelength calibration (a periodic detection task), if a sample arrives at the detector and a signal needs to be acquired, the calibration or reporting will be interrupted to prioritize the integrity of the sample data.
[0119] Among them, the parameter configuration task has a higher priority than the periodic detection task, which can improve the flexibility of emergency intervention and troubleshooting, as well as the timeliness and controllability of operation and maintenance.
[0120] Among them, the data acquisition task refers to the real-time acquisition and processing of raw sample signals from the detector, which is the highest priority core task to ensure the integrity of chromatographic analysis data.
[0121] Among them, the data reporting task refers to packaging the instrument status, alarm information and processed results data and sending them to the host computer or cloud, which is a key communication task for realizing remote monitoring.
[0122] Among them, parameter configuration tasks refer to tasks that modify or query instrument operating parameters (such as wavelength and flow rate) or system configuration in response to instructions issued locally or remotely.
[0123] Periodic testing tasks refer to tasks that are automatically and periodically performed in the background to verify and maintain the performance of the instrument itself, such as wavelength correction and baseline calibration.
[0124] Example 3: In some embodiments, the present invention also provides a control circuit for an ultraviolet-visible detector in a liquid chromatograph, comprising: a photoelectric sensor, a first amplifier, an ADC (analog to digital converter, which is usually an electronic component that converts analog signals into digital signals), three monochromator drive circuits, and a controller; The output of the photoelectric sensor is connected to the controller via a first amplifier and an ADC. The input terminals of the three monochromator drive circuits are all connected to the controller; The controller is configured to generate a PWM signal to drive the monochromator through three monochromator drive circuits, and to periodically perform wavelength correction according to a preset correction period; and to obtain the usage intensity in the most recent correction period; the usage intensity = K1 * normalized usage count + K2 * normalized total running time; and to determine whether the usage intensity in the most recent correction period is greater than or equal to a second preset threshold and less than a first preset threshold; if the usage intensity is greater than or equal to the first preset threshold, the correction period is shortened by a first preset reduction, and periodic wavelength correction is performed according to the adjusted correction period; if the usage intensity is less than the second preset threshold, the correction period is extended by a first preset increment, and periodic wavelength correction is performed according to the adjusted correction period; the second preset threshold is less than the first preset threshold; if the usage intensity is greater than or equal to the second preset threshold and less than the first preset threshold, the current correction period is maintained.
[0125] In other embodiments, it further includes an Ethernet communication module electrically connected to the controller. The controller is also configured to perform periodic corrections based on control commands received from the host computer via the Ethernet communication module. The control command is issued by the host computer (IoT) when it starts the regional centralized calibration mode or the decentralized autonomous calibration mode after acquiring the usage intensity of each liquid chromatograph in each region during the most recent calibration cycle and identifying the distribution of the usage intensity of all liquid chromatographs in each region. If the distribution meets a first preset condition, a regional centralized correction mode is adopted. The first preset condition is that the difference between the usage intensity and the mean of each liquid chromatograph in the current region is less than or equal to a preset difference threshold. The regional centralized correction mode includes: if the minimum usage intensity is greater than or equal to the first preset threshold, shortening the correction cycle of the chromatograph corresponding to the maximum usage intensity by a first preset reduction, and using the correction cycle as the correction cycle of all chromatographs in the current region; if the maximum usage intensity is less than a second preset threshold, extending the correction cycle of the chromatograph corresponding to the middle usage intensity by a first preset increment, and using the correction cycle as the correction cycle of all chromatographs in the same region. If the distribution meets the second preset condition, and N is greater than or equal to a preset quantity threshold, then a dispersed autonomous correction mode is adopted for the N liquid chromatographs; the second preset condition is: the difference between the usage intensity and the mean of at least N liquid chromatographs in the current area is greater than a preset difference threshold; the dispersed autonomous correction mode includes: each liquid chromatograph in the current area shortens the correction cycle according to a first preset reduction in its usage intensity, or increases the correction cycle according to a first preset increment.
[0126] In some embodiments, it further includes: a temperature sensor, a second amplifier, a leakage detection module, a third amplifier, a monochromator position detection module, and a deuterium lamp driving circuit, a tungsten lamp driving circuit, and an RS-485 communication interface electrically connected to the controller; The output of the temperature sensor is connected to the controller via a second amplifier; The output of the leakage detection module is connected to the controller via a third amplifier; The monochromator position detection module is electrically connected to the controller.
[0127] In some embodiments, the system further includes: a power management module electrically connected to the controller; the power management module includes: two sets of isolated DC / DC modules that supply power to the analog circuit and the microcontroller circuit respectively; and a set of non-isolated DC / DC circuits that supply power to the external I / O interface circuit.
[0128] In some embodiments, the two isolated DC / DC modules are essentially two independent, electrically isolated DC power supply outputs to achieve a degree of noise isolation. Digital circuits in the instrument (such as microcontrollers) generate significant high-frequency switching noise, while analog circuits (such as preamplifiers and ADC references) are extremely sensitive to noise. Using two independent DC power supplies ensures the signal-to-noise ratio and accuracy of the measurement signal.
[0129] Please see Figure 2 In some embodiments, the present invention also proposes a centralized monitoring system for a liquid chromatograph, comprising: Multiple liquid chromatographs, each including the control circuit described in any embodiment of the present invention; the liquid chromatographs are configured to periodically perform wavelength calibration at a preset calibration cycle; and the calibration cycle is dynamically adjusted according to the usage intensity within the most recent calibration cycle; the usage intensity = K1 * standardized number of uses + K2 * standardized total running time; The host computer is configured to acquire the usage intensity of each liquid chromatograph in each region during the most recent calibration period via the Internet of Things; and identify the distribution of usage intensity of all liquid chromatographs in each region; if the distribution meets a first preset condition, a regional centralized calibration mode is adopted; the first preset condition is: the difference between the usage intensity of each liquid chromatograph in the current region and the mean is less than or equal to a preset difference threshold; the regional centralized calibration mode includes: if the minimum usage intensity is greater than or equal to the first preset threshold, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period as the calibration period of all chromatographs in the current region; ... of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period of the chromatograph corresponding to the maximum usage intensity according to If the usage intensity is less than the second preset threshold, the calibration cycle of the corresponding chromatograph with the middle usage intensity is extended by the first preset increment, and the calibration cycle is used as the calibration cycle of all chromatographs in the same area; if the distribution meets the second preset condition, and N is greater than or equal to the preset quantity threshold, then a dispersed autonomous calibration mode is adopted for the N liquid chromatographs; the second preset condition is: the difference between the usage intensity and the mean of at least N liquid chromatographs in the current area is greater than the preset difference threshold; the dispersed autonomous calibration mode includes: each liquid chromatograph in the current area shortens the calibration cycle by reducing its usage intensity by the first preset amount, or increases the calibration cycle by the first preset increment.
[0130] It should be understood that the centralized monitoring system for liquid chromatographs can be used to perform the steps described in any embodiment of the present invention.
[0131] Please see Figure 4This invention proposes a control circuit for an ultraviolet-visible light detector. The control circuit uses a microcontroller as its core, combining a silicon photodiode, a pre-amplifier logarithmic transimpedance amplifier, and a high-precision analog-to-digital converter to measure spectral signals. The timer module built into the main control chip outputs a PWM (Pulse Width Modulation) signal, which, through a motor driver chip, controls the monochromator. An I2C interface controls a 16-bit DAC chip to achieve analog signal output. The main control chip has a built-in Ethernet MAC layer module, which, combined with an external physical layer chip, enables Ethernet communication. For instruments with lower precision requirements, temperature measurement and leakage detection signals are amplified and conditioned by an operational amplifier before being acquired by the ADC module built into the main control chip. The control circuit is powered by a 24V DC power supply.
[0132] The power management module includes two isolated DC / DC modules to power the analog circuits and the microcontroller circuits respectively, and also includes a non-isolated DC / DC circuit to power the external I / O interface circuits.
[0133] Among them, the microcontroller is the core of the entire control system, and the STM32F207 series microcontroller is preferred as the main control chip.
[0134] In some embodiments, the ultraviolet-visible light signal is acquired using a silicon photodiode sensor, amplified by a pre-logarithmic transimpedance amplifier, converted into a digital signal by a high-precision analog-to-digital converter, and then interacts with the main control chip via an SPI interface (Serial Peripheral Interface).
[0135] The monochromator contains three stepper motors (24V-1.5A, 24V-0.2A, 6V-0.8A), controlled by PWM signals generated by the main control chip's timer module. These control signals are magnetically isolated and then connected to a dedicated stepper motor driver chip to drive the monochromator. The monochromator's position signal is acquired by an internal photoelectric switch, magnetically isolated, and then connected to the main control chip's GPIO interface (General Purpose Input / Output) for detection.
[0136] The deuterium lamp is driven by a dedicated power supply (i.e., the light source control circuit), and the control signals and status signals are connected to the GPIO interface of the main control chip after magnetic isolation; the tungsten lamp is driven by the DC / DC power module of the main control board, and the power switch signal is controlled by the GPIO interface of the main control chip after magnetic isolation.
[0137] The communication interface (such as the RS-485 interface) preferably uses the MAX485 chip, and the Ethernet interface preferably uses the DP83848 chip. These are connected to the USART (Universal Synchronous / Asynchronous Receiver / Transmitter) and MII (Media Independent Interface) of the main control chip, respectively, to realize the communication connection with the computer.
[0138] The voltage signal output uses a 16-bit DAC chip, which is connected to the main control chip via an I2C interface. The external trigger interface is magnetically isolated and then connected to the GPIO interrupt interface of the main control chip to achieve synchronous trigger acquisition.
[0139] The instrument temperature detection preferably uses a PT100 sensor, and the leakage detection uses two thermistors to form a detection bridge. The signals are conditioned by operational amplifiers and then connected to the main control chip, which is then used for signal acquisition by the built-in ADC module of the main control chip.
[0140] Through the aforementioned control circuit, the detector (i.e., the chromatograph) converts the physical or chemical properties of the sample into easily measurable electrical signals, which are then input into the data processing system to obtain the chromatograms of the sample components. The ultraviolet-visible (UV-Vis) detector is the most widely used detector in HPLC (High Performance Liquid Chromatography), and can be used for the qualitative and quantitative detection of most common organic substances with UV absorption and some inorganic substances. Furthermore, it is not very sensitive to changes in ambient temperature, mobile phase composition, and flow rate fluctuations, and can be used for both isocratic and gradient elution.
[0141] The ultraviolet-visible detector is equipped with two light sources, a deuterium lamp and a tungsten lamp, and can be set in a wavelength range of 190nm–900nm. The optimized optical system gives the instrument a high signal-to-noise ratio, a wide linear range, and higher wavelength accuracy and repeatability.
[0142] It should be noted that, in this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Unless otherwise specified, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes that element.
[0143] Through the above description of the embodiments, those skilled in the art can clearly understand that the methods of the above embodiments can be implemented by means of software plus necessary general-purpose hardware platforms. Of course, they can also be implemented by hardware, but in many cases the former is a better implementation method. Based on this understanding, the technical solution of the present invention, or the part that contributes to the prior art, can be embodied in the form of a software product. This computer software product is stored in a storage medium (such as ROM / RAM, magnetic disk, optical disk) and includes several instructions to cause a computer terminal (which may be a mobile phone, computer, server, or network device, etc.) to execute the methods described in the various embodiments of the present invention.
[0144] The embodiments of the present invention have been described above with reference to the accompanying drawings. However, the present invention is not limited to the specific embodiments described above. The specific embodiments described above are merely illustrative and not restrictive. Those skilled in the art can make many other forms under the guidance of the present invention without departing from the spirit and scope of the claims. All of these forms are within the protection scope of the present invention.
[0145] In some embodiments, this application also provides a schematic block diagram of the structure of a computer device, please see... Figure 5 Computer programs can be used in situations such as Figure 5 It runs on the computer device shown. Figure 5 As shown, the computer device includes a processor, memory, and a network interface connected via a system bus. The memory may include non-volatile storage media and internal memory. The non-volatile storage media may store an operating system and computer programs. The computer programs include program instructions that, when executed, cause the processor to perform arbitrary methods. The processor provides computational and control capabilities to support the operation of the entire computer device. The internal memory provides an environment for the execution of the computer programs in the non-volatile storage media; when executed by the processor, these programs cause the processor to perform arbitrary methods. The network interface is used for network communication, such as sending assigned tasks. Those skilled in the art will understand that... Figure 5The structures shown are merely block diagrams of a portion of the structure related to the present application and do not constitute a limitation on the computer device to which the present application is applied. Specific computer devices may include more or fewer components than shown in the figures, or combine certain components, or have different component arrangements. It should be understood that the processor may be a Central Processing Unit (CPU), but it can also be other general-purpose processors, digital signal processors (DSPs), application-specific integrated circuits (ASICs), field-programmable gate arrays (FPGAs), or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components, etc. The general-purpose processor may be a microprocessor or any conventional processor.
Claims
1. A wavelength calibration method for a liquid chromatograph, characterized in that, Including the following steps: S101, performs wavelength correction periodically according to a preset correction cycle; S102, Obtain the usage intensity of the liquid chromatograph during the most recent calibration period; the usage intensity = K1 * standardized number of uses + K2 * standardized total running time; S103, determine whether the usage intensity within the most recent correction period is greater than or equal to a second preset threshold and less than a first preset threshold; The second preset threshold is less than the first preset threshold; S104, if the intensity of use is greater than or equal to the first preset threshold, shorten the correction period according to the first preset reduction, and perform periodic wavelength correction according to the adjusted correction period; S105, if the intensity of use is less than the second preset threshold, extend the correction period by the first preset increment, and perform periodic wavelength correction according to the adjusted correction period; S106, if the intensity of use is greater than or equal to the second preset threshold and less than the first preset threshold, maintain the current correction cycle.
2. The wavelength calibration method for a liquid chromatograph according to claim 1, characterized in that, The method further includes the step of dividing a plurality of spatially adjacent liquid chromatographs into a region: S201, The host computer obtains the usage intensity of each liquid chromatograph in each region during the most recent calibration period via the Internet of Things; S202, the host computer determines whether the difference between the usage intensity and the mean of each liquid chromatograph in each region is less than or equal to a preset difference threshold. If the host computer determines that the difference between the usage intensity and the mean of each liquid chromatograph in any region is less than or equal to a preset difference threshold, a regional centralized correction mode is adopted. The regional centralized correction mode is as follows: if the minimum usage intensity is greater than or equal to a first preset intensity threshold, the correction cycle of the chromatograph corresponding to the maximum usage intensity is shortened by a first preset reduction, and the correction cycle is used as the correction cycle of all chromatographs in any region; if the maximum usage intensity is less than a second preset threshold, the correction cycle of the chromatograph corresponding to the middle usage intensity is extended by a first preset increment, and the correction cycle is used as the correction cycle of all chromatographs in the same region. If the host computer determines that the difference between the usage intensity and the mean of at least N liquid chromatographs in any region is greater than the preset difference threshold, and N is greater than or equal to the preset quantity threshold, then a dispersed autonomous correction mode is adopted for the N liquid chromatographs. The decentralized autonomous calibration mode includes: each liquid chromatograph in any region shortens the calibration cycle by reducing its usage intensity according to a first preset reduction, or extends the calibration cycle by increasing its usage intensity according to a first preset increment.
3. The wavelength calibration method for a liquid chromatograph according to claim 2, characterized in that, The specific steps of employing the aforementioned regional centralized correction mode are as follows: Based on the historical data of each liquid chromatograph in any region, calculate its personalized periodic offset coefficient; specifically, it includes: performing linear fitting based on the wavelength deviation value of each chromatograph in the historical calibration period to obtain the slope characterizing the wavelength drift rate, and using the reciprocal of the slope as the personalized periodic offset coefficient. The calibration period obtained after adjusting the liquid chromatograph with the highest usage intensity in any of the regions is taken as the regional reference period; The final calibration cycle for each of the remaining liquid chromatographs in any given region is equal to the regional baseline cycle multiplied by the personalized cycle offset coefficient.
4. The wavelength calibration method for a liquid chromatograph according to claim 3, characterized in that, The process also includes the following steps: if, within one of the calibration cycles, the user manually triggers or receives a wavelength calibration task from a remote terminal, the user executes the wavelength calibration task and records this calibration as a non-periodic calibration task. Obtain the time interval between the non-periodic correction task and the previous periodic correction task; Calculate the ratio R of the time interval to the current correction period. If R < the first proportional threshold, the correction period is shortened according to the second preset reduction. If R ≥ the second proportional threshold, the correction period is extended according to the second preset increment. If the first proportional threshold ≤ R < the second proportional threshold, keep the current correction period unchanged; The adjusted period will be used as the new correction period, and the end time of this non-periodic correction task will be used as the start time of the next correction period.
5. The wavelength calibration method for a liquid chromatograph according to claim 1, characterized in that, It also includes the following steps: Receive remote tasks sent by the host computer and add the remote tasks to the task queue; Determine whether the priority of the remote task is higher than the priority of the currently executing task; If the value is high, interrupt the currently executing task to execute the remote task; The task queue includes data acquisition tasks, data reporting tasks, parameter configuration tasks, and periodic detection tasks, with priority decreasing in descending order. The parameter configuration task includes the remote task; the periodic detection task includes the wavelength correction task.
6. A control circuit for a UV-Vis detector in a liquid chromatograph, characterized in that, include: Photoelectric sensor, first amplifier, ADC, three monochromator drive circuits and controller; The output of the photoelectric sensor is connected to the controller via a first amplifier and an ADC. The input terminals of the three monochromator drive circuits are all connected to the controller; The controller is configured to generate PWM signals to drive the monochromator through three monochromator drive circuits, and to perform wavelength correction periodically according to a preset correction period. And obtain the usage intensity within the most recent calibration period; the usage intensity = K1 * standardized usage count + K2 * standardized total running time; And determine whether the usage intensity within the most recent correction period is greater than or equal to a second preset threshold and less than a first preset threshold; If the usage intensity is greater than or equal to a first preset threshold, the correction period is shortened by a first preset reduction, and periodic wavelength correction is performed according to the adjusted correction period; if the usage intensity is less than a second preset threshold, the correction period is extended by a first preset increment, and periodic wavelength correction is performed according to the adjusted correction period; the second preset threshold is less than the first preset threshold. If the intensity of use is greater than or equal to the second preset threshold and less than the first preset threshold, the current correction cycle is maintained.
7. The control circuit for the ultraviolet-visible detector in a liquid chromatograph according to claim 6, characterized in that, Also includes: The Ethernet communication module is electrically connected to the controller. The controller is also configured to perform periodic calibration based on control commands issued by the host computer according to the Ethernet communication module; the control commands are issued by the host computer when it starts the regional centralized calibration mode or the decentralized autonomous calibration mode after obtaining the usage intensity of each liquid chromatograph in each region in the most recent calibration period through the Internet of Things and identifying the distribution of the usage intensity of all liquid chromatographs in each region. If the distribution meets a first preset condition, a regional centralized correction mode is adopted. The first preset condition is that the difference between the usage intensity and the mean of each liquid chromatograph in the current region is less than or equal to a preset difference threshold. The regional centralized correction mode includes: if the minimum usage intensity is greater than or equal to the first preset threshold, shortening the correction cycle of the chromatograph corresponding to the maximum usage intensity by a first preset reduction, and using the correction cycle as the correction cycle of all chromatographs in the current region; if the maximum usage intensity is less than a second preset threshold, extending the correction cycle of the chromatograph corresponding to the middle usage intensity by a first preset increment, and using the correction cycle as the correction cycle of all chromatographs in the same region. If the distribution meets the second preset condition, and N is greater than or equal to a preset quantity threshold, then a dispersed autonomous correction mode is adopted for the N liquid chromatographs; the second preset condition is: the difference between the usage intensity and the mean of at least N liquid chromatographs in the current area is greater than a preset difference threshold; the dispersed autonomous correction mode includes: each liquid chromatograph in the current area shortens the correction cycle according to a first preset reduction in its usage intensity, or increases the correction cycle according to a first preset increment.
8. The control circuit for the ultraviolet-visible detector in a liquid chromatograph according to claim 7, characterized in that, Also includes: Temperature sensor, second amplifier, leakage detection module, third amplifier, monochromator position detection module, and deuterium lamp drive circuit, tungsten lamp drive circuit, and RS-485 communication interface electrically connected to the controller; The output of the temperature sensor is connected to the controller via a second amplifier; The output of the leakage detection module is connected to the controller via a third amplifier; The monochromator position detection module is electrically connected to the controller.
9. The control circuit for the ultraviolet-visible detector in a liquid chromatograph according to claim 8, characterized in that, Also includes: The power management module is electrically connected to the controller; The power management module includes: two sets of isolated DC / DC modules that provide power to the analog circuit and the microcontroller circuit, respectively; And a set of non-isolated DC / DC circuits to power the external I / O interface circuits.
10. A centralized monitoring system for a liquid chromatograph, characterized in that, include: Multiple liquid chromatographs, wherein the liquid chromatographs include the control circuitry described in any one of claims 6-9; The liquid chromatograph is configured to periodically perform wavelength calibration at a preset calibration cycle. The calibration period is dynamically adjusted based on the usage intensity within the most recent calibration period; the usage intensity = K1 * standardized usage count + K2 * standardized total running time. The host computer is configured to acquire the usage intensity of each liquid chromatograph in each region during the most recent calibration period via the Internet of Things; and identify the distribution of usage intensity of all liquid chromatographs in each region; if the distribution meets a first preset condition, a regional centralized calibration mode is adopted; the first preset condition is: the difference between the usage intensity of each liquid chromatograph in the current region and the mean is less than or equal to a preset difference threshold; the regional centralized calibration mode includes: if the minimum usage intensity is greater than or equal to the first preset threshold, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period as the calibration period of all chromatographs in the current region; ... of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, shortening the calibration period of the chromatograph corresponding to the maximum usage intensity according to a first preset reduction, and using the calibration period of the chromatograph corresponding to the maximum usage intensity according to If the usage intensity is less than the second preset threshold, the calibration cycle of the corresponding chromatograph with the middle usage intensity is extended by the first preset increment, and the calibration cycle is used as the calibration cycle of all chromatographs in the same area; if the distribution meets the second preset condition, and N is greater than or equal to the preset quantity threshold, then a dispersed autonomous calibration mode is adopted for the N liquid chromatographs; the second preset condition is: the difference between the usage intensity and the mean of at least N liquid chromatographs in the current area is greater than the preset difference threshold; the dispersed autonomous calibration mode includes: each liquid chromatograph in the current area shortens the calibration cycle by reducing its usage intensity by the first preset amount, or increases the calibration cycle by the first preset increment.
Citation Information
Patent Citations
Liquid chromatograph and method for correcting detector output value fluctuation of liquid chromatograph
CN107490632A