CN-121994958-A - Wavelength correction method, control circuit and monitoring system of liquid chromatograph

CN121994958ACN 121994958 ACN121994958 ACN 121994958ACN-121994958-A

Abstract

The invention relates to the technical field of liquid chromatograph, in particular to a wavelength correction method, a control circuit and a monitoring system of a liquid chromatograph. The wavelength correction method comprises the steps of periodically carrying out wavelength correction according to a preset correction period, obtaining the use intensity of the liquid chromatograph in the latest correction period, carrying out normalized use frequency +K2 of the use intensity=K1, carrying out normalized operation total duration, judging whether the use intensity in the latest correction period is larger than or equal to a first preset threshold value, shortening the correction period according to a first preset decrement if the use intensity is larger than or equal to the first preset threshold value, prolonging the correction period according to a first preset increment if the use intensity is smaller than a second preset threshold value, and carrying out periodical wavelength correction according to the adjusted correction period. The method can greatly improve the timeliness and the high efficiency of the wavelength correction of the chromatograph, and further is beneficial to improving the accuracy of detection and analysis data of the chromatograph.

Inventors

ZHOU LI
HUANG YINGZHANG
LIAO DAWEI

Assignees

重庆质谱科技有限公司

Dates

Publication Date: 20260508
Application Date: 20260206

Claims (10)

1. A method for wavelength correction of a liquid chromatograph, comprising the steps of: S101, periodically performing wavelength correction according to a preset correction period; S102, acquiring the use intensity of the liquid chromatograph in the latest correction period, wherein the use intensity=K1 is normalized and the use times+K2 is normalized; s103, judging whether the use intensity in the latest correction period is larger than or equal to a second preset threshold value and smaller than a first preset threshold value, wherein the second preset threshold value is smaller than the first preset threshold value; s104, if the use intensity is greater than or equal to the first preset threshold value, shortening the correction period according to a first preset decrement, and performing periodic wavelength correction according to the adjusted correction period; s105, if the use intensity is smaller than a second preset threshold value, prolonging the correction period according to a first preset increment, and performing periodic wavelength correction according to the adjusted correction period; and S106, if the use intensity is larger than or equal to the second preset threshold value and smaller than the first preset threshold value, maintaining the current correction period.
2. A method of wavelength correction for a liquid chromatograph according to claim 1, characterized in that a plurality of said liquid chromatographs spatially adjacent are divided into one area, and correspondingly, the method further comprises the steps of: S201, the upper computer obtains the use intensity of each liquid chromatograph in each region in the latest correction period through the Internet of things; s202, the upper computer judges whether the difference between the using intensity and the average value of each liquid chromatograph in each area is smaller than or equal to a preset difference threshold; If the difference between the using intensity and the average value of each liquid chromatograph in any area is smaller than or equal to a preset difference threshold value, adopting an area centralized correction mode, wherein the area centralized correction mode is to shorten the correction period of the chromatograph corresponding to the using intensity with the smallest using intensity according to a first preset decrement if the using intensity with the smallest using intensity is larger than or equal to a first preset intensity threshold value, and take the correction period as the correction period of all the chromatographs in any area; And if the upper computer judges that the difference between the using intensities and the average value of at least N liquid chromatographs in any area is larger than the preset difference threshold and N is larger than or equal to the preset quantity threshold, adopting a dispersion autonomous correction mode for the N liquid chromatographs, wherein the dispersion autonomous correction mode comprises that each liquid chromatograph in any area shortens the correction period according to a first preset decrement by using the using intensity of each liquid chromatograph or prolongs the correction period according to a first preset increment.
3. The method for correcting the wavelength of a liquid chromatograph according to claim 2, wherein the step of adopting the area concentration correction mode specifically comprises the steps of: Calculating a personalized period offset coefficient based on historical data of each liquid chromatograph in any region, wherein the method specifically comprises the steps of performing linear fitting based on wavelength offset values of each chromatograph in a historical correction period to obtain a slope representing a wavelength drift rate, and taking the reciprocal of the slope as the personalized period offset coefficient; The correction period obtained after the liquid chromatograph with the maximum use intensity in any region is adjusted is used as a region reference period; the final correction period of each of the remaining liquid chromatographs in any one region=the region reference period×the personalized period offset coefficient.
4. The method for calibrating a wavelength of a liquid chromatograph according to claim 3, further comprising the steps of, if a user manually triggers or receives a wavelength calibration task issued by a remote terminal in one of said calibration periods, executing said wavelength calibration task and recording the current calibration as an aperiodic calibration task; acquiring the time interval between the non-periodic correction task and the previous periodic correction task; Calculating the ratio R of said time interval to the current correction period, If R is smaller than the first proportional threshold, shortening the correction period according to the second preset decrement; if R is more than or equal to a second proportion threshold value, the correction period is prolonged according to a second preset increment; if the first proportion threshold value is less than or equal to R < the second proportion threshold value, keeping the current correction period unchanged; And taking the adjusted period as a new correction period, and taking the ending time of the non-periodic correction task as the starting time of the next correction period.
5. The method for wavelength correction of a liquid chromatograph according to claim 1, further comprising the steps of: Receiving a remote task issued by an upper computer, and adding the remote task into a task queue; Judging whether the priority of the remote task is higher than the priority of the currently executed task; if so, interrupting the current executing task to execute the remote task; The task queue comprises a data acquisition task, a data reporting task, a parameter configuration task and a periodic detection task, wherein the priorities of the data acquisition task, the data reporting task, the parameter configuration task and the periodic detection task are sequentially decreased; The parameter configuration task comprises the remote task, and the periodic detection task comprises the wavelength correction task.
6. A control circuit of an ultraviolet-visible light detector in a liquid chromatograph is characterized by comprising a photoelectric sensor, a first amplifier, an ADC, three monochromator driving circuits and a controller; The output end of the photoelectric sensor is connected with the controller through a first amplifier and an ADC, The input ends of the three monochromator driving circuits are connected with the controller; The controller is configured to generate a PWM signal to drive a monochromator to operate through three monochromator driving circuits, and periodically perform wavelength correction according to a preset correction period, and acquire a use intensity in a latest correction period, wherein the use intensity=K1 is normalized for a total operation time period normalized for a number of times +K2, and judges whether the use intensity in the latest correction period is greater than or equal to a second preset threshold value and smaller than a first preset threshold value, shortens the correction period according to a first preset decrement if the use intensity is greater than or equal to the first preset threshold value, and performs periodic wavelength correction according to the adjusted correction period, extends the correction period according to a first preset increment if the use intensity is smaller than a second preset threshold value, and performs periodic wavelength correction according to the adjusted correction period, and is smaller than the first preset threshold value if the use intensity is greater than or equal to the second preset threshold value and smaller than the first preset threshold value, and maintains the current correction period.
7. The control circuit for an ultraviolet visible light detector in a liquid chromatograph of claim 6, further comprising an Ethernet communication module electrically connected to the controller, The controller is further configured to perform periodic correction according to a control instruction issued by the Ethernet communication module, wherein the control instruction is issued by the upper computer in a region centralized correction mode or a distributed independent correction mode after the upper computer obtains the use intensity of each liquid chromatograph in each region in the latest correction period through the Internet of things and recognizes the distribution condition of the use intensity of all the liquid chromatographs in each region; The area centralized correction mode comprises the steps of shortening the correction period of the chromatograph corresponding to the maximum use intensity according to a first preset decrement and taking the correction period as the correction period of all chromatographs in the same area if the minimum use intensity is larger than or equal to a first preset threshold value, and prolonging the correction period of the chromatograph corresponding to the center of the use intensity according to a first preset increment if the maximum use intensity is smaller than a second preset threshold value; And if the distribution condition accords with a second preset condition and N is greater than or equal to a preset quantity threshold, adopting a scattered autonomous correction mode for the N liquid chromatographs, wherein the second preset condition is that the difference between the using intensity and the average value of at least N liquid chromatographs in the current area is greater than a preset difference threshold, and the scattered autonomous correction mode comprises that each liquid chromatograph in the current area shortens the correction period according to the first preset decrement by using the using intensity of each liquid chromatograph or increases the correction period according to the first preset increment.
8. The control circuit for an ultraviolet visible light detector in a liquid chromatograph of claim 7, further comprising a temperature sensor, a second amplifier, a liquid leakage detection module, a third amplifier, a monochromator position detection module, and a deuterium lamp driving circuit, a tungsten lamp driving circuit, an RS-485 communication interface electrically connected to the controller; the output end of the temperature sensor is connected with the controller through a second amplifier; The output end of the liquid leakage detection module is connected with the controller through a third amplifier; The monochromator position detection module is electrically connected with the controller.
9. The control circuit for an ultraviolet visible light detector in a liquid chromatograph of claim 8, further comprising a power management module electrically coupled to the controller, the power management module comprising two sets of isolated DC/DC modules that power the analog circuitry and the microcontroller circuitry, respectively, and a set of non-isolated DC/DC circuits that power the external I/O interface circuitry.
10. A centralized monitoring system for a liquid chromatograph, comprising: A plurality of liquid chromatographs comprising the control circuit of any one of claims 6-9, the liquid chromatographs configured to periodically perform wavelength correction for a preset correction period, and dynamically adjust the correction period according to a usage intensity in a latest correction period, the usage intensity=k1+k2 being a normalized total length of operation; The upper computer is configured to acquire the use intensity of each liquid chromatograph in each area in the latest correction period through the Internet of things, identify the distribution condition of the use intensity of all the liquid chromatographs in each area, and adopt an area centralized correction mode if the distribution condition meets a first preset condition, wherein the first preset condition is that the difference between the use intensity of each liquid chromatograph in the current area and the mean value is smaller than or equal to a preset difference threshold value, the area centralized correction mode comprises that the correction period of each liquid chromatograph corresponding to the maximum use intensity in the current area is shortened according to a first preset decrement if the minimum use intensity is larger than or equal to the first preset threshold value, the correction period of each liquid chromatograph in the current area is taken as the correction period of all the chromatographs in the current area, and the correction period of each liquid chromatograph corresponding to the maximum use intensity in the current area is lengthened according to a first preset increment if the distribution condition meets a second preset condition, the dispersion number of each liquid chromatograph in the current area is increased according to the first preset increment, and the difference between the N is equal to the first preset threshold value, and the correction period of each liquid chromatograph in the current area is increased according to the first preset increment.

Description

Wavelength correction method, control circuit and monitoring system of liquid chromatograph Technical Field The invention relates to the technical field of liquid chromatograph, in particular to a wavelength correction method, a control circuit and a monitoring system of a liquid chromatograph. Background The current maintenance field of the wavelength accuracy of the liquid chromatograph is highly dependent on manual experience judgment, and a user or a maintainer needs to judge whether the wavelength is deviated through experience or not and manually trigger a correction flow or contact special person to process after a problem is found. On the one hand, the traditional method has strong dependence on professional experience of personnel, and on the other hand, the fine early offset is difficult to find in time, and often needs to be developed into obvious deviation and can be found when the reliability of data is affected, so that a certain hysteresis exists from the occurrence of the offset to the detection of the offset. In this regard, some methods for correcting the detector output value of the liquid chromatograph have been attempted in the prior art. For example, patent publication No. CN107490632a proposes a liquid chromatograph and a detector output value fluctuation correction method for the liquid chromatograph. The selection of the correction wavelength is based on the experience of the user, and when the excessive correction processing is performed, information of the trace component detected as a peak on the chromatogram, particularly a minute peak, is lost, and a correct analysis result cannot be obtained. The minimum peak value is determined based on the analysis result, a correction wavelength at which the S/N ratio of the minimum peak value is the maximum is determined, and the correction of the minimum peak value is performed using the determined correction wavelength. A plurality of detector output value correction methods are registered in the arithmetic device unit, and the correction is performed by selecting the correction method from the plurality of registered correction methods according to an initially set correction method or purpose. But this solution focuses on processing the output data after the sample analysis is completed. Therefore, there is a need for a more efficient method of wavelength calibration for liquid chromatographs. Disclosure of Invention The invention aims to provide a wavelength correction method, a control circuit and a monitoring system of a liquid chromatograph, which partially solve or alleviate the defects in the prior art and can improve the efficiency of wavelength correction of liquid chromatograph equipment. In order to solve the technical problems, the invention adopts the following technical scheme: In a first aspect of the present invention, there is provided a wavelength correction method for a liquid chromatograph, comprising the steps of: S101, periodically performing wavelength correction according to a preset correction period; S102, acquiring the use intensity of the liquid chromatograph in the latest correction period, wherein the use intensity=K1 is normalized and the use times+K2 is normalized; s103, judging whether the use intensity in the latest correction period is larger than or equal to a second preset threshold value and smaller than a first preset threshold value, wherein the second preset threshold value is smaller than the first preset threshold value; s104, if the use intensity is greater than or equal to the first preset threshold value, shortening the correction period according to a first preset decrement, and performing periodic wavelength correction according to the adjusted correction period; s105, if the use intensity is smaller than a second preset threshold value, prolonging the correction period according to a first preset increment, and performing periodic wavelength correction according to the adjusted correction period; and S106, if the use intensity is larger than or equal to the second preset threshold value and smaller than the first preset threshold value, maintaining the current correction period. In some embodiments, the method further comprises the step of dividing the plurality of spatially adjacent liquid chromatographs into one region, and correspondingly: S201, the upper computer obtains the use intensity of each liquid chromatograph in each region in the latest correction period through the Internet of things; s202, the upper computer judges whether the difference between the using intensity and the average value of each liquid chromatograph in each area is smaller than or equal to a preset difference threshold; If the difference between the using intensity and the average value of each liquid chromatograph in any area is smaller than or equal to a preset difference threshold value, adopting an area centralized correction mode, wherein the area centralized correction mode is to shorten the correction