CN-121978198-A - Method, apparatus and storage medium for quadrupole power calibration

CN121978198ACN 121978198 ACN121978198 ACN 121978198ACN-121978198-A

Abstract

The invention discloses a method, a device and a storage medium for calibrating a quadrupole rod power supply, wherein the method comprises the steps of obtaining an initial correction coefficient of the quadrupole rod power supply, and establishing an initial voltage correction equation based on a quadrupole rod ion motion equation; setting a characteristic mass number, a target resolution and a pre-scanning range, collecting spectrogram data in the pre-scanning range according to an initial voltage correction equation, presetting a mass number deviation initial value, dynamically adjusting the mass number deviation according to a comparison result of the resolution in the spectrogram data and the target resolution, positioning a preliminary spectral peak corresponding to the characteristic mass number, carrying out iterative adjustment on the resolution error and the peak error, optimizing a correction coefficient and the initial correction coefficient until the error between the peak center and the characteristic mass number is smaller than a preset threshold value, determining a final correction coefficient, and calibrating the spectral peak of the whole mass axis based on the final correction coefficient to finish the quadrupole power supply calibration. The invention can realize rapid and accurate initial parameter calibration of the quadrupole rod power supply under the condition of no manual intervention.

Inventors

LI MAN
WANG LEI
LI KAI
YANG XIANGQIAN

Assignees

钢研纳克检测技术股份有限公司

Dates

Publication Date: 20260505
Application Date: 20260130

Claims (10)

1. A method for quadrupole power calibration comprising the steps of: S1, calculating an initial correction coefficient of a quadrupole rod power supply based on an ion motion equation of a quadrupole rod, and establishing an initial voltage correction equation, wherein the initial correction coefficient comprises a radio frequency voltage initial correction coefficient and a direct current voltage initial correction coefficient; S2, in a quadrupole mass spectrometer, setting a characteristic mass number m 0 and a target resolution R, setting a pre-scanning range of each mass number, setting scanning voltage according to the initial voltage correction equation, and acquiring mass spectrum data to acquire spectrogram data in the pre-scanning range; S3, presetting a quality number deviation initial value, and dynamically adjusting the quality number deviation according to a comparison result of the resolution in spectrogram data and the target resolution until a spectrum peak with the resolution of R appears in a pre-scanning range of each quality number, wherein the spectrum peak is a preliminary spectrum peak corresponding to the characteristic quality number; S4, adjusting the resolution error and the peak error based on the center mass number of the spectrum peak obtained in the step S3 to obtain a correction coefficient of the characteristic mass number m 0 , and updating an initial correction coefficient; S5, repeating the steps S3-S4 until the error between the peak center and the characteristic quality number m 0 is smaller than a preset threshold value and the resolution is R, and determining a final correction coefficient; and S6, calibrating the spectrum peak of the whole mass axis based on the final correction coefficient, and completing the quadrupole rod power supply calibration.
2. The method for calibrating a quadrupole rod power according to claim 1, wherein in S1, the initial correction factor K RF0 for the radio frequency voltage and the initial correction factor K DC0 for the direct current voltage are calculated by a marry equation, and the calculation is based on the structural size and the working frequency of the quadrupole rod; The initial voltage correction equation is expressed as: U RF =K RF0 (K RF *m+Δm RF ); U DC =K DC0 (K DC *m+Δm DC ); Wherein, U RF is a radio frequency voltage, U DC is a direct current voltage, m is a mass number, K RF is a mass number coefficient corresponding to the radio frequency voltage, K DC is a mass number coefficient corresponding to the direct current voltage, Δm RF is a mass number deviation corresponding to the radio frequency voltage, and Δm DC is a mass number deviation corresponding to the direct current voltage.
3. The method for calibrating a quadrupole power source according to claim 1, wherein in S2, the characteristic mass number m 0 is a mass number corresponding to an element having a signal intensity greater than 2Mcps in a non-solution state in the quadrupole mass spectrometer and in a normal operation state of the instrument, the upper and lower limits of the target resolution R are expressed as R min 、R max , the pre-scan range is set to m 0 -5~m 0 +5, and the mass range difference m range =5.
4. The method for quadrupole power calibration according to claim 1, wherein in S3, a preset mass deviation initial value Δm DC0 =0, data are collected, and whether a spectral peak appears in a pre-scan range is observed; the adjustment rule of the mass number deviation is that the mass number deviation is increased when the detected resolution is larger than the target resolution R, and the mass number deviation is reduced when the detected resolution is smaller than the target resolution R until a spectrum peak with the resolution of R appears in the pre-scanning range of each target mass number, the peak center is m 01 , and the spectrum peak is a preliminary spectrum peak corresponding to the characteristic mass number m 0 .
5. The method for quadrupole power calibration according to claim 2, wherein the specific algorithm for resolution error adjustment in S4 is: If no spectrum peak is detected, adjusting the mass number deviation delta m' DC =Δm DC -5 corresponding to the direct-current voltage, and repeatedly collecting spectrum data until an effective spectrum peak is generated; If the detected resolution is smaller than the lower limit R min of the target resolution, adjusting the mass number deviation delta m' DC =Δm DC corresponding to the direct current voltage (target resolution-actual resolution) by a coefficient k 1 ; If the detected resolution is greater than the upper limit R max of the target resolution, adjusting the mass number deviation delta m' DC =Δm DC + (actual resolution-target resolution) corresponding to the direct current voltage by a coefficient k 2 ; Where the coefficients k 1 and k 2 are predefined adjustment gains.
6. The method for quadrupole power calibration according to claim 5, wherein the specific algorithm for peak error adjustment in S4 is: Calculating a new slope correction coefficient: K' RF =m 01 *(K RF *m 0 +Δm RF )/(m 0 *m 0 ); K' DC =m 01 *(K DC *m 0 +Δm DC )/(m 0 *m 0 ); And updates Δm RF =0;Δm DC =0; Updating initial correction coefficients: K' RF0 =K' RF *K RF0 ; K' DC0 =K' DC *K DC0 ; Wherein m 01 is the peak center of the spectrum peak positioned in step S3, K ' RF is the mass number coefficient corresponding to the updated radio frequency voltage, K' DC is the mass number coefficient corresponding to the updated direct current voltage, K ' RF0 is the updated radio frequency voltage initial correction coefficient, and K' DC0 is the updated direct current voltage initial correction coefficient.
7. The method for quadrupole power calibration of claim 6, wherein in S5, the error preset threshold for peak center and characteristic mass number m 0 is 0.1, and when |m 01 -m 0 | <0.1, stopping iterative adjustment, wherein m 01 is the peak center of the current spectral peak; Determining a final correction coefficient specifically includes: Obtaining a final correction coefficient of the characteristic quality number: K'' RF =(K RF *m 0 +Δm RF )/m 0 ; K'' DC =(K DC *m 0 +Δm DC )/m 0 ; obtaining a final correction coefficient of the quadrupole rod power supply: K'' RF0 =K'' RF *K RF0 ; K'' DC0 =K'' DC *K DC0 ; Wherein, K ' RF is the quality coefficient corresponding to the final RF voltage, K' DC is the quality coefficient corresponding to the final DC voltage, K ' RF0 is the final RF voltage initial correction coefficient, and K' DC0 is the final DC voltage initial correction coefficient.
8. The method for calibrating a quadrupole power source according to claim 1, wherein in S6, based on the final correction coefficient of the characteristic mass number, substituting an initial voltage correction equation, scanning a mass spectrum mass axis, finding a spectrum peak of the whole mass axis, obtaining a spectrum peak of low, medium and high mass numbers satisfying a target resolution and peak error, and realizing a spectrum peak positioning and calibration of the whole mass axis.
9. An apparatus for quadrupole power calibration, for use in performing the method for quadrupole power calibration of any one of claims 1-8, comprising: The system comprises an initial correction coefficient acquisition module, a power supply module and a power supply module, wherein the initial correction coefficient acquisition module is used for calculating an initial correction coefficient of a quadrupole rod power supply based on an ion motion equation of the quadrupole rod and establishing an initial voltage correction equation, and the initial correction coefficient comprises a radio frequency voltage initial correction coefficient and a direct current voltage initial correction coefficient; The spectrogram data acquisition module is used for setting a characteristic mass number m 0 and a target resolution R in the quadrupole mass spectrometer, setting a pre-scanning range of each mass number, setting scanning voltage according to the initial voltage correction equation, and acquiring mass spectrum data in the pre-scanning range; the spectral peak preliminary positioning module is used for presetting a quality number deviation initial value, dynamically adjusting the quality number deviation according to a comparison result of the resolution in the spectrogram data and the target resolution until a spectral peak with the resolution of R appears in a pre-scanning range of each quality number, wherein the spectral peak is a preliminary spectral peak corresponding to the characteristic quality number; The coefficient calculation and updating module is used for adjusting the resolution error and the peak error based on the center mass number of the spectrum peak to obtain a correction coefficient of the characteristic mass number m 0 and updating the initial correction coefficient, and carrying out iterative updating until the error between the peak center and the characteristic mass number m 0 is smaller than a preset threshold value and the resolution is R, so as to determine a final correction coefficient; and the full-mass axis calibration module is used for calibrating the spectrum peak of the whole mass axis based on the final correction coefficient to finish the quadrupole rod power supply calibration.
10. A non-transitory computer readable storage medium having stored thereon a computer program, which when executed by a processor implements the method for quadrupole power calibration according to any one of claims 1 to 8.

Description

Method, apparatus and storage medium for quadrupole power calibration Technical Field The invention relates to the technical field of quadrupole mass spectrometers, in particular to a method, a device and a storage medium for quadrupole power calibration. Background Quadrupole mass spectrometers are one of the most widely used mass analysis instruments at present, and are widely applied to the fields of chemistry, life sciences, material sciences and the like. However, quadrupole power sources are susceptible to environmental temperature, humidity, and mechanical dimensions, resulting in voltage drift. Such drift can cause significant differences between theoretical and actual voltages, making it difficult to accurately acquire mass spectrum signals of the target element. Therefore, before the mass axis calibration is performed, the voltage of the quadrupole power supply must be calibrated to obtain a mass spectrum at the target resolution, thereby performing the mass axis calibration. In the prior art, a 'translational' adjustment method based on experience or trial and error is mostly adopted for the calibration of the quadrupole rod power supply. The operator usually needs to manually and repeatedly adjust the voltage parameters, scan the mass axis for a plurality of times, observe the change of the spectrum peak position, and gradually approach the target mass number. This method is cumbersome, inefficient, highly dependent on the experience of the operator, and difficult to achieve accurate, repeatable automated calibration. The whole calibration process is long in time consumption, and when high resolution is pursued, small voltage deviation can lead to failure in spectral peak positioning or unqualified resolution, so that the method becomes a key bottleneck for restricting the improvement of analysis precision and automation level of the quadrupole mass spectrometer. Therefore, there is a great need in the art for a quadrupole power source tuning and calibration scheme that can be quickly, accurately and automatically implemented to address many of the pain points of the prior art. Disclosure of Invention The invention aims to provide a method, a device and a storage medium for quadrupole rod power supply calibration, which can realize rapid and accurate quadrupole rod power supply initial parameter calibration without manual intervention and lay a solid foundation for efficient and automatic correction of the whole subsequent mass axis. In order to achieve the above object, the present invention provides the following solutions: a method for quadrupole power calibration comprising the steps of: S1, calculating an initial correction coefficient of a quadrupole rod power supply based on an ion motion equation of a quadrupole rod, and establishing an initial voltage correction equation, wherein the initial correction coefficient comprises a radio frequency voltage initial correction coefficient and a direct current voltage initial correction coefficient; S2, in a quadrupole mass spectrometer, setting a characteristic mass number m 0 and a target resolution R, setting a pre-scanning range of each mass number, setting scanning voltage according to the initial voltage correction equation, and acquiring mass spectrum data to acquire spectrogram data in the pre-scanning range; S3, presetting a quality number deviation initial value, and dynamically adjusting the quality number deviation according to a comparison result of the resolution in spectrogram data and the target resolution until a spectrum peak with the resolution of R appears in a pre-scanning range of each quality number, wherein the spectrum peak is a preliminary spectrum peak corresponding to the characteristic quality number; S4, adjusting the resolution error and the peak error based on the center mass number of the spectrum peak obtained in the step S3 to obtain a correction coefficient of the characteristic mass number m 0, and updating an initial correction coefficient; S5, repeating the steps S3-S4 until the error between the peak center and the characteristic quality number m 0 is smaller than a preset threshold value and the resolution is R, and determining a final correction coefficient; and S6, calibrating the spectrum peak of the whole mass axis based on the final correction coefficient, and completing the quadrupole rod power supply calibration. Further, in the step S1, the radio frequency voltage initial correction coefficient K RF0 and the direct current voltage initial correction coefficient K DC0 are obtained by calculation according to a marry equation, and the calculation basis is the structural size and the working frequency of the quadrupole rod; The initial voltage correction equation is expressed as: URF=KRF0(KRF*m+ΔmRF); UDC=KDC0(KDC*m+ΔmDC); Wherein, U RF is a radio frequency voltage, U DC is a direct current voltage, m is a mass number, K RF is a mass number coefficient corresponding to the radio frequency voltage, K D