A chromatograph gas inlet control method, system, terminal and storage medium
By analyzing the chromatograph detector signal and the component-specific standard database, and optimizing the carrier gas flow rate using the extended van Dimmel equation, the problem of poor separation effect when the carrier gas leaks in the gas chromatograph was solved, and good component separation effect was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-19
- Publication Date
- 2026-04-10
AI Technical Summary
When the carrier gas leaks, the electronic gas path control of the existing gas chromatograph cannot detect it, resulting in poor separation performance, prolonged retention time, and increased peak width.
By acquiring the detector signal and component-specific standard database of the chromatograph, the separated components and parameter deviation rates are analyzed. The theoretical plate height and carrier gas flow rate are calculated using the extended van der Munte equation, and the electronic gas path control is adjusted to optimize the carrier gas flow rate.
It effectively reduces the abnormal impact of carrier gas flow rate on component separation, provides good separation effect, and ensures that the retention time and half-peak width of components are within the allowable range.
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Figure CN121186277B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of chromatographs, and in particular to a chromatograph inlet control method, system, terminal and storage medium. Background Technology
[0002] A chromatograph is a precision analytical instrument used to separate, identify and analyze the components in a mixture. Based on the physicochemical principle of chromatography, it is widely used in fields such as chemistry, biology, medicine, environment, food, and materials science.
[0003] In related technologies, the carrier gas control of gas chromatographs generally adopts electronic gas path control (EPC), which includes pressure / flow sensors, electronic proportional valves, and control software. The pressure / flow sensors monitor gas pressure and flow in real time, while the control software compares the detected gas pressure and flow with the set gas parameters, thereby controlling the electronic proportional valve to automatically adjust the opening and precisely control the gas flow.
[0004] Regarding the aforementioned technologies, EPC controls the physical parameters at a certain point in the gas path. When an anomaly occurs downstream of the sensor, such as a leak, EPC cannot detect it. In this case, the EPC's detection result is still that the flow rate / pressure is stable, but the actual amount of carrier gas entering the chromatographic column is reduced, resulting in a longer retention time and a wider peak width in the chromatograph, leading to poor separation performance of the chromatograph. There is still room for improvement. Summary of the Invention
[0005] To provide good separation results, this application provides a chromatograph inlet control method, system, terminal, and storage medium.
[0006] In a first aspect, this application provides a chromatograph inlet control method, which adopts the following technical solution:
[0007] A method for controlling the inlet gas of a chromatograph, comprising:
[0008] Acquire detector signals and component-specific standard databases for chromatographs;
[0009] Analyze detector signals and component-specific standard databases to determine the separated components and their corresponding parameter deviation rates;
[0010] Determine whether the parameter deviation rate meets the requirements of the component-specific standard database;
[0011] If the condition is met, the detector signal of the chromatograph will continue to be acquired for cyclical analysis and judgment.
[0012] If not, obtain the real-time carrier gas flow rate and real-time carrier gas purity;
[0013] The real-time carrier gas flow rate and real-time carrier gas purity are analyzed and calculated based on the pre-set extended van der Munte equation to determine the theoretical plate height of the separated components.
[0014] The theoretical tray height, real-time carrier gas flow rate, and parameter deviation rate were analyzed to determine the final adjustment flow rate.
[0015] The carrier gas flow rate is adjusted based on the final adjusted flow control electronic gas circuit control.
[0016] Optionally, the step of analyzing detector signals and a component-specific standard database to determine the separated components and their corresponding parameter deviation rates includes:
[0017] The detector signal is truncated according to the preset sliding window width to generate a window analysis signal;
[0018] The window analysis signal is analyzed to determine the peak time, peak signal, and half-peak time;
[0019] Obtain the injection time;
[0020] Analyze the peak time and injection time to determine the real-time retention time;
[0021] Analyze the half-peak time and peak time to determine the real-time half-peak width;
[0022] The real-time retention time, real-time half-peak width, and component-specific standard database were analyzed to determine the separated components and the corresponding parameter deviation rates.
[0023] Optionally, the steps of analyzing the windowed signal to determine the peak-to-peak time, peak-to-peak signal, and half-peak time include:
[0024] Differentiate the windowed signal to determine its first and second derivatives;
[0025] When the first derivative and the second derivative of the signal meet the requirements of the preset peak start condition, determine whether the first derivative and the second derivative of the signal meet the requirements of the preset peak apex condition.
[0026] If it does not meet the requirements, the detector signal will continue to be truncated according to the sliding window width to generate a window analysis signal;
[0027] If the conditions are met, the real-time recording time and the real-time recording signal are obtained, and the real-time recording time is defined as the peak time and the real-time recording signal is defined as the peak signal.
[0028] The real-time recorded signal and the window analysis signal are analyzed to determine the half-peak time.
[0029] Optionally, the steps of analyzing the real-time recorded signal and the windowed analysis signal to determine the half-peak time include:
[0030] Analyze the real-time recorded signals to determine the half-peak signal;
[0031] Determine whether the window analysis signal meets the requirements of a half-peak signal;
[0032] If it does not meet the requirements, the detector signal will continue to be truncated according to the sliding window width to generate a window analysis signal;
[0033] If the conditions are met, the matching window time is obtained and defined as the half-peak time.
[0034] Optionally, the steps to analyze the theoretical plate height, real-time carrier gas flow rate, and parameter deviation rate to determine the final adjusted flow rate include:
[0035] The partial derivative of the real-time carrier gas flow rate is calculated based on the theoretical tray height, and the partial derivative is set to 0 to generate the real-time optimal flow rate.
[0036] The real-time optimal flow rate, parameter deviation rate, and real-time carrier gas flow rate are analyzed to determine the final adjusted flow rate.
[0037] Optionally, the steps of analyzing the real-time optimal flow rate, parameter deviation rate, and real-time carrier gas flow rate to determine the final adjusted flow rate include:
[0038] The parameter deviation rate and the preset deviation correction coefficient are analyzed to determine the flow adjustment coefficient;
[0039] Analyze the flow adjustment coefficient and the real-time optimal flow to determine the actual optimal flow;
[0040] The actual optimal flow rate and real-time carrier gas flow rate are analyzed to determine the basic adjustment flow rate;
[0041] Analyze the baseline adjustment flow to determine the final adjustment flow.
[0042] Optionally, the steps of analyzing the baseline adjustment flow to determine the final adjustment flow include:
[0043] The separated components and component-specific standard databases were analyzed to determine the number of theoretical plates for each component and the total number of standard theoretical plates.
[0044] The component theoretical plate number and the total number of standard theoretical plates are analyzed to determine the component flow weights;
[0045] The component flow weights and baseline adjustment flow rates are analyzed to determine the final adjustment flow rate.
[0046] Secondly, this application provides a chromatograph inlet control system, which adopts the following technical solution:
[0047] A chromatograph inlet control system, comprising:
[0048] The acquisition module is used to acquire detector signals, component-specific standard databases, real-time carrier gas flow rate, and real-time carrier gas purity.
[0049] A memory for storing a program for a chromatograph inlet control method as described in any of the preceding claims;
[0050] The processor and the program in the memory can be loaded and executed by the processor to implement a chromatograph inlet control method as described in any of the above.
[0051] Thirdly, this application provides a smart terminal, which adopts the following technical solution:
[0052] A smart terminal includes a memory and a processor, wherein the memory stores a computer program that can be loaded by the processor and executed as described in any of the preceding claims for a chromatograph inlet control method.
[0053] Fourthly, this application provides a computer storage medium capable of storing corresponding programs, which is characterized by its ease of implementation and ability to provide good separation, and adopts the following technical solution:
[0054] A computer-readable storage medium storing a computer program that can be loaded by a processor and executed any of the above-described chromatograph inlet control methods.
[0055] In summary, this application includes at least one of the following beneficial technical effects:
[0056] 1. By analyzing the detector signal and the component-specific standard database, the separated components and their corresponding parameter deviation rates are obtained. When it is determined that the parameter deviation rate does not meet the requirements of the component-specific standard data, the theoretical plate height of the separated components is calculated based on the real-time carrier gas flow rate and real-time carrier gas purity according to the extended van Deumert equation. The final adjustment amount is obtained after analyzing the theoretical plate height, real-time carrier gas flow rate and parameter deviation rate. Thus, the abnormal parameters of component separation are fed back to the carrier gas flow rate adjustment, reducing the abnormal impact of carrier gas flow rate on component separation and providing good separation effect. Attached Figure Description
[0057] Figure 1 This is a flowchart of a chromatograph inlet control method according to an embodiment of this application.
[0058] Figure 2This is a flowchart of the steps in this application embodiment to analyze the detector signal and the component-specific standard database to determine the separated components and the corresponding parameter deviation rates.
[0059] Figure 3 This is a flowchart of the steps in this application embodiment to analyze the window analysis signal to determine the peak time, peak signal, and half-peak time.
[0060] Figure 4 This is a flowchart of the steps in this application embodiment to analyze the real-time recorded signal and the window analysis signal to determine the half-peak time.
[0061] Figure 5 This is a flowchart illustrating the steps in this application embodiment to analyze the theoretical plate height, real-time carrier gas flow rate, and parameter deviation rate to determine the final flow rate adjustment.
[0062] Figure 6 This is a flowchart illustrating the steps in this application embodiment to analyze the real-time optimal flow rate, parameter deviation rate, and real-time carrier gas flow rate to determine the final adjusted flow rate.
[0063] Figure 7 This is a flowchart illustrating the steps in this application embodiment to analyze the basic adjustment flow to determine the final adjustment flow. Detailed Implementation
[0064] To make the purpose, technical solution, and advantages of this application clearer, the following description is provided in conjunction with the appendix. Figures 1 to 7 The present application will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are for illustrative purposes only and are not intended to limit the scope of the application.
[0065] Reference Figure 1 This application discloses a method for controlling the gas inlet of a chromatograph, comprising the following steps:
[0066] Step S100: Obtain the detector signal and component-specific standard database of the chromatograph.
[0067] Among them, the detector signal refers to the real-time signal output by the chromatograph detector, that is, the voltage change curve over time. For example, in a flame ionization detector, when the sample components flow through the detector with the mobile phase, a voltage signal positively correlated with the component concentration is generated. The curve of the signal change over time is the chromatographic elution curve. Collecting the detector signal provides data support for subsequent analysis of whether the carrier gas affects the separation of components.
[0068] The component-specific standard database stores different components and their corresponding standard retention times, allowable deviation ranges for retention times, standard half-widths (HWHM), allowable deviation ranges for HWHM, standard theoretical plate numbers, and allowable deviation ranges for plate numbers. Operators select 3-5 typical analysis cycles to ensure instrument stability and record the following parameters for all target components in the sample: standard carrier gas conditions: purity, initial flow rate, column temperature; standard separation parameters for the components: standard retention time, standard peak width, standard theoretical plate number; carrier gas anomaly simulation data: by fine-tuning leakage, purity, and flow rate, the changes in standard retention time, standard peak width, and standard theoretical plate number for components under different anomalies are recorded for model fitting, thereby determining the allowable deviation ranges for retention time, HWHM, and plate number.
[0069] Step S101: Analyze the detector signal and component-specific standard database to determine the separated components and their corresponding parameter deviation rates.
[0070] Here, "separated component" refers to the specific component being separated, and "parameter deviation rate" refers to the retention time deviation rate and half-width at half-maximum deviation rate of the separated component. These are obtained by the processing terminal after analyzing the detector signal and the component-specific standard database. The specific method is described in [reference needed]. Figure 2 The steps.
[0071] Step S102: Determine whether the parameter deviation rate meets the requirements of the component-specific standard database.
[0072] The requirement for the component-specific standard database is that it does not exceed the allowable deviation range of retention time and the allowable deviation range of half-peak width for the corresponding components in the component-specific standard database.
[0073] By processing the terminal, it is determined whether the retention time deviation rate and half-peak width deviation rate corresponding to the parameter deviation rate do not exceed the allowable deviation range of retention time and half-peak width corresponding to the component in the component-specific standard database, thereby determining whether the current carrier gas state is normal and whether it affects the component separation.
[0074] Step S1021: If the condition is met, continue to acquire the detector signal of the chromatograph for cyclic analysis and judgment.
[0075] If the retention time deviation rate and half-peak width deviation rate corresponding to the parameter deviation rate determined by the processing terminal do not exceed the allowable deviation range of retention time and half-peak width corresponding to the component in the component-specific standard database, it indicates that the current carrier gas state is normal and has not affected the separation of the components. Therefore, the detector signal of the chromatograph continues to be collected to continuously monitor the separation of the components.
[0076] Step S1022: If not, obtain the real-time carrier gas flow rate and real-time carrier gas purity.
[0077] If the retention time deviation rate and half-peak width deviation rate corresponding to the parameter deviation rate determined by the processing terminal exceed the allowable deviation range of retention time and half-peak width for the corresponding components in the component-specific standard database, it indicates that the current carrier gas state is abnormal and affects the separation of components. Therefore, the real-time carrier gas flow rate and real-time carrier gas purity are detected to provide data support for subsequent adjustments to the carrier gas state.
[0078] Real-time carrier gas flow rate refers to the current carrier gas flow rate in the gas path, which is detected in real time by the flow sensor in the electronic gas path control. Real-time carrier gas purity refers to the purity of the carrier gas in the current gas path, which is detected by the satellite purity sensor in the gas path.
[0079] Step S103: Analyze and calculate the real-time carrier gas flow rate and real-time carrier gas purity according to the preset extended van der Munte equation to determine the theoretical plate height of the separated components.
[0080] The theoretical plate height refers to the theoretical plate height of the separated components at the current moment, reflecting column efficiency. The smaller the theoretical plate height, the higher the column efficiency. It is calculated by the processing terminal by substituting the real-time carrier gas flow rate and real-time carrier gas purity into the extended van der Mutt equation.
[0081] The extended van der Munte equation is an algorithm used to calculate the theoretical plate height of components. It involves calculating the first product of real-time carrier gas flow rate and real-time carrier gas purity at the processing terminal, then calculating the second product of real-time carrier gas flow rate and mass transfer resistance term, followed by calculating the quotient of the longitudinal diffusion term and the first product. Finally, the theoretical plate height is obtained by summing the eddy diffusion term, the second product, and the quotient. The determination methods for the eddy diffusion term, longitudinal diffusion term, and mass transfer resistance term are as follows: six flow rate gradients are set within the standard carrier gas flow rate range, and the retention time and half-peak width of the components are measured at each gradient. After calculating the theoretical plate height, the eddy diffusion term, longitudinal diffusion term, and mass transfer resistance term are obtained through nonlinear fitting.
[0082] Step S104: Analyze the theoretical plate height, real-time carrier gas flow rate, and parameter deviation rate to determine the final adjustment flow rate.
[0083] The final adjusted flow rate refers to the flow rate ultimately adjusted by the electronic gas circuit control, which is obtained by the processing terminal after analyzing the theoretical plate height, real-time carrier gas flow rate, and parameter deviation rate. The specific method is described in [reference needed]. Figure 5 These steps ensure proper separation of the components.
[0084] Step S105: Adjust the carrier gas flow rate according to the final adjusted flow control electronic gas circuit control.
[0085] In this process, after the processing terminal determines the final adjustment flow rate, the electronic gas path control adjusts the opening of the electronic proportional valve according to the final adjustment flow rate, thereby reducing the abnormal influence of the carrier gas flow rate on component separation, keeping the retention time and half-peak width of the separated components within the allowable range, and thus providing a good separation effect.
[0086] Reference Figure 2 The steps for analyzing detector signals and component-specific standard databases to determine separated components and corresponding parameter deviation rates include:
[0087] Step S200: The detector signal is truncated according to the preset sliding window width to generate a window analysis signal.
[0088] The sliding window width refers to the sampling time of the detector signal, which is determined according to the peak interval. When the peak interval is less than 10 seconds, the sliding window width is determined to be 3-5 seconds, and when the peak interval is greater than 10 seconds, the sliding window width is determined to be 6-10 seconds.
[0089] Window analysis signal refers to detector signal with a fixed time length. The processing terminal extracts the detector signal based on the time length corresponding to the width of the sliding window, and then processes the detector signal point by point in real time.
[0090] Step S201: Analyze the window analysis signal to determine the peak time, peak signal, and half-peak time.
[0091] Among them, peak-peak time refers to the time when the current outflow peak reaches its peak, peak-peak signal refers to the voltage when the current outflow peak reaches its peak, and half-peak time refers to the time at the half-peak height position. All three are obtained by the processing terminal after analyzing the window analysis signal. For specific methods, please refer to [link to relevant documentation]. Figure 3 The steps.
[0092] Step S202: Obtain the injection time.
[0093] The injection time refers to the moment when the sample is injected into the chromatographic system. It is the reference point for calculating the retention time and is usually 0 seconds.
[0094] Step S203: Analyze the peak time and injection time to determine the real-time retention time.
[0095] Among them, real-time retention time refers to the time from injection to peak in chromatographic analysis. It is a key basis for component identification because the retention time of different components under the same chromatographic conditions is basically fixed. It is obtained by calculating the difference between peak time and injection time by the processing terminal.
[0096] Step S204: Analyze the half-peak time and peak time to determine the real-time half-peak width.
[0097] Among them, the real-time half-peak width refers to the peak width at half the peak height, reflecting the sharpness of the peak. The deeper the peak, the higher the separation effect. The wider the peak, the more likely it is that the column is malfunctioning or the flow rate is abnormal. It is an auxiliary parameter for component quantification and is obtained by multiplying the difference between the half-peak time and the peak time by 2 after the processing terminal calculates it.
[0098] Step S205: Analyze the real-time retention time, real-time half-peak width, and component-specific standard database to determine the separated components and the corresponding parameter deviation rates.
[0099] In this step, the separation component and parameter deviation rate are consistent with those in step S101. The processing terminal searches for components with similar retention times in the component-specific standard database based on the real-time retention time, defines the component as the separation component, and then calls the standard retention time and standard half-peak width of the component to calculate the first difference between the real-time retention time and the standard retention time. The retention time deviation rate is obtained by calculating the quotient of the first difference and the standard retention time. The second difference between the real-time half-peak width and the standard half-peak width is calculated, and the half-peak width deviation rate is obtained by calculating the quotient of the second difference and the standard half-peak width. The parameter deviation rate is obtained by associating the retention time deviation rate and the half-peak width deviation rate.
[0100] Reference Figure 3 The steps for analyzing the windowed signal to determine the peak time, peak signal, and half-peak time include:
[0101] Step S300: Calculate the derivative of the window analysis signal to determine the first and second derivatives of the signal.
[0102] The first derivative of the signal refers to the first derivative of the signal analyzed by the window, which is the rate of change of the signal. When the first derivative of the signal is greater than 0, it is in the rising peak phase, at which point the components begin to flow out and the signal moves upward from the baseline. When the first derivative of the signal is 0, it is in the peak peak phase, the signal reaches its maximum value, and then begins to decline. When the first derivative of the signal is less than 0, it is in the falling peak phase, the component outflow decreases, and the signal moves downward.
[0103] The second derivative of a signal refers to the second derivative of the signal analyzed by a window, which is the rate of change of the rate of change. It reflects the concavity and convexity of the peak. When the second derivative of the signal is greater than 0, it is in the rising phase of the peak, the signal rises faster and faster, and the curve is convex upward. When the second derivative of the signal changes from positive to negative, it is at the peak, the turning point where the rising rate changes from positive to negative. When the second derivative of the signal is less than 0, it is in the falling phase of the peak, the signal falls faster and faster, and the curve is convex downward.
[0104] Step S301: When the first derivative and the second derivative of the signal meet the requirements of the preset peak start condition, determine whether the first derivative and the second derivative of the signal meet the requirements of the preset peak apex condition.
[0105] Among them, the peak start condition refers to the judgment condition when the signal deviates from the baseline and enters the rising phase at the beginning of the component outflow. That is, the first derivative of the signal is greater than 3 times the average baseline signal and the second derivative of the signal is greater than 0. The requirement of the peak start condition is that the peak start condition is met. The average baseline signal refers to the background signal of the detector when there is no component outflow, which is a smooth fluctuation curve. Its average signal is the average baseline signal.
[0106] The peak condition refers to the condition for determining when a signal reaches its maximum value and then begins to decline. Specifically, it requires that the first derivative of the signal is 0 and the second derivative of the signal is less than 0. The requirement of the peak condition is that the peak condition is met.
[0107] At the processing terminal, it is determined that the first and second derivatives of the signal meet the requirements of the peak start condition, that is, the first derivative of the signal is greater than 3 times the baseline average signal and the second derivative of the signal is greater than 0. At this time, the component has just started to flow out. Then, it is determined whether the first and second derivatives of the signal meet the requirements of the peak condition, that is, whether the first derivative of the signal is 0 and whether the second derivative of the signal is less than 0, so as to determine whether it is at the peak.
[0108] Step S3011: If it does not meet the requirements, continue to truncate the detector signal according to the sliding window width to generate a window analysis signal.
[0109] If the processing terminal determines that the first derivative of the signal is not 0 or the second derivative of the signal is not less than 0, it indicates that the outflow peak is not at the peak apex. Therefore, the detector signal is truncated according to the sliding window width to generate a new window analysis signal, thereby continuously analyzing whether the outflow peak is at the peak apex.
[0110] Step S3012: If the conditions are met, obtain the real-time recording time and the real-time recording signal, and define the real-time recording time as the peak time and the real-time recording signal as the peak signal.
[0111] If the processing terminal determines that the first derivative of the signal is 0 and the second derivative of the signal is less than 0, it indicates that the outflow peak is at the peak apex. Therefore, the real-time recording time and the real-time recording signal are recorded, and the real-time recording time is defined as the peak apex time and the real-time recording signal is defined as the peak apex signal.
[0112] Real-time recording time refers to the current time of the window analysis signal. The real-time recording signal refers to the signal value of the window analysis signal. The processing terminal finds the maximum signal value in the current window analysis signal, which is the real-time recording signal, and identifies the time corresponding to the real-time recording signal as the real-time recording time.
[0113] Step S302: Analyze the real-time recorded signal and the window analysis signal to determine the half-peak time.
[0114] The half-peak time in this step is the same as the half-peak time in step S201, and is obtained by the processing terminal after analyzing the real-time recorded signal and the window analysis signal. The specific method is described in [reference needed]. Figure 4 The steps.
[0115] Reference Figure 4 The steps for analyzing real-time recorded signals and windowed analysis signals to determine the half-peak time include:
[0116] Step S400: Analyze the real-time recorded signal to determine the half-peak signal.
[0117] Among them, the half-peak signal refers to the signal value when it is at half-peak, which is obtained by the processing terminal calculating half of the corresponding signal value of the real-time recorded signal.
[0118] Step S401: Determine whether the window analysis signal meets the requirements of a half-peak signal.
[0119] The requirement for a half-peak signal is that it is equal to half the peak signal. The processing terminal determines whether the signal value is equal to the half-peak signal by analyzing the signal value corresponding to the signal through the judgment window.
[0120] Step S4011: If it does not meet the requirements, continue to truncate the detector signal according to the sliding window width to generate a window analysis signal.
[0121] If the processing terminal determines that the signal value corresponding to the window analysis signal is not equal to the half-peak signal, it indicates that the half-peak has not yet been reached. Therefore, the detector signal is truncated according to the sliding window width to generate a new window analysis signal, thereby continuously monitoring the changes in the signal.
[0122] Step S4012: If the conditions are met, obtain the matching window time and define the matching window time as the half-peak time.
[0123] If the processing terminal determines that the signal value corresponding to the window analysis signal is equal to the half-peak signal, it indicates that the half-peak has been reached. Therefore, the conformance window time is detected, and the conformance window time is defined as the half-peak time.
[0124] The coincidence window time refers to the signal time after the peak point. The processing terminal defines the time in the signal that is equal to the half-peak signal as the coincidence window time.
[0125] Reference Figure 5 The steps to determine the final flow rate adjustment include analyzing the theoretical tray height, real-time carrier gas flow rate, and parameter deviation rate.
[0126] Step S500: Calculate the partial derivative of the real-time carrier gas flow rate with respect to the theoretical plate height, and set the partial derivative to 0 to generate the real-time optimal flow rate.
[0127] The real-time optimal flow rate refers to the optimal carrier gas flow rate of the component at the current carrier gas concentration, which can simultaneously satisfy the requirements of reasonable retention time and minimum peak broadening. The partial derivative of the real-time carrier gas flow rate is calculated from the theoretical plate height at the processing terminal and made to zero. After simplification, the simplified expression is the product of the mass transfer resistance term and the real-time carrier gas purity. The square root of the quotient of the longitudinal diffusion term and the product is then taken as the real-time optimal flow rate.
[0128] Step S501: Analyze the real-time optimal flow rate, parameter deviation rate, and real-time carrier gas flow rate to determine the final adjusted flow rate.
[0129] The final adjusted flow rate in this step is consistent with the final adjusted flow rate in step S104, and is obtained by the processing terminal after analyzing the real-time optimal flow rate, parameter deviation rate, and real-time carrier gas flow rate. The specific method is described in [reference needed]. Figure 6 The steps.
[0130] Reference Figure 6 The steps to determine the final flow rate adjustment include analyzing the real-time optimal flow rate, parameter deviation rate, and real-time carrier gas flow rate.
[0131] Step S600: Analyze the parameter deviation rate and the preset deviation correction coefficient to determine the flow adjustment coefficient.
[0132] The deviation correction coefficient is a coefficient that corrects the retention time deviation. It is obtained by fitting multiple sets of retention time-flow adjustment experiments and quantifying the inverse correlation strength between retention time deviation and flow adjustment. For example, a deviation correction coefficient of 0.8 means that if the retention time deviation rate is 1%, the flow needs to be adjusted in the opposite direction by 0.8%.
[0133] The flow adjustment coefficient is a coefficient that enables reverse correction of retention time deviation. It is obtained by multiplying the retention time deviation rate and the deviation correction coefficient in the parameter deviation rate calculated by the processing terminal, and then calculating the difference between 1 and the product.
[0134] Step S601: Analyze the flow adjustment coefficient and the real-time optimal flow to determine the actual optimal flow.
[0135] The actual optimal flow rate refers to the carrier gas flow rate adjusted based on the retention time deviation rate, which is obtained by multiplying the flow adjustment coefficient calculated by the processing terminal with the real-time optimal flow rate.
[0136] Step S602: Analyze the actual optimal flow rate and the real-time carrier gas flow rate to determine the basic adjustment flow rate.
[0137] Among them, the basic adjustment flow rate refers to the carrier gas adjustment flow rate of the component, which is obtained by the difference between the actual optimal flow rate and the real-time carrier gas flow rate calculated by the processing terminal.
[0138] Step S603: Analyze the basic adjustment flow to determine the final adjustment flow.
[0139] The final adjustment flow rate in this step is the same as the final adjustment flow rate in step S501, and is obtained by the processing terminal after analyzing the basic adjustment flow rates of all components. The specific method is described in [reference needed]. Figure 7 The steps.
[0140] Reference Figure 7 The steps for analyzing the baseline adjustment flow to determine the final adjustment flow include:
[0141] Step S700: Analyze the separated components and the component-specific standard database to determine the number of theoretical plates for each component and the total number of standard theoretical plates.
[0142] Among them, the theoretical plate number of a component refers to the standard theoretical plate number of the separated component, which is obtained by the processing terminal by looking up the corresponding standard theoretical plate number of the separated component in the component-specific standard database.
[0143] The total number of standard theoretical plates refers to the sum of the standard theoretical plate numbers for all separated components, which is obtained by summing the standard theoretical plate numbers for all separated components at the processing terminal.
[0144] Step S701: Analyze the number of theoretical plates for each component and the total number of standard theoretical plates to determine the component flow weights.
[0145] The component flow weight refers to the weight of the adjusted flow rate of the separated component in the total adjusted flow rate, which is obtained by calculating the quotient between the theoretical number of the component and the total number of standard theoretical plates at the processing terminal.
[0146] Step S702: Analyze the component flow weights and the basic adjustment flow to determine the final adjustment flow.
[0147] In this step, the final adjustment flow rate is the same as that in step S603, and is obtained by the processing terminal by weighting and summing the component flow rate weights and the basic adjustment flow rate.
[0148] Based on the same inventive concept, embodiments of this application provide a chromatograph inlet control system, including:
[0149] The acquisition module is used to acquire detector signals, component-specific standard database, real-time carrier gas flow rate, real-time carrier gas purity, injection time, real-time recording time, real-time recording signal, and coincidence window time.
[0150] A memory for storing a program for a chromatograph inlet control method;
[0151] The processor is capable of loading and executing programs in memory to implement a chromatograph inlet control method.
[0152] Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the above-described division of functional modules is used as an example. In practical applications, the above functions can be assigned to different functional modules as needed, that is, the internal structure of the device can be divided into different functional modules to complete all or part of the functions described above. The specific working process of the system, device, and unit described above can be referred to the corresponding process in the foregoing method embodiments, and will not be repeated here.
[0153] This application provides a computer-readable storage medium storing a computer program that can be loaded by a processor and executed as a chromatograph inlet control method.
[0154] Computer storage media include, for example, USB flash drives, portable hard drives, read-only memory (ROM), random access memory (RAM), magnetic disks, optical disks, and other media that can store program code.
[0155] Based on the same inventive concept, this application provides a smart terminal, including a memory and a processor, wherein the memory stores a computer program that can be loaded and executed by the processor to control the gas intake of a chromatograph.
[0156] Those skilled in the art will clearly understand that, for the sake of convenience and brevity, the above-described division of functional modules is used as an example. In practical applications, the above functions can be assigned to different functional modules as needed, that is, the internal structure of the device can be divided into different functional modules to complete all or part of the functions described above. The specific working process of the system, device, and unit described above can be referred to the corresponding process in the foregoing method embodiments, and will not be repeated here.
[0157] The above are all preferred embodiments of this application and are not intended to limit the scope of protection of this application. Any feature disclosed in this specification (including the abstract and drawings) may be replaced by other equivalent or similar features unless specifically stated otherwise. That is, unless specifically stated otherwise, each feature is only one example of a series of equivalent or similar features.
Claims
1. A method of gas inlet control for a chromatograph, characterized by, The method comprises the following steps: acquiring a detector signal of a chromatograph and a component-specific standard database; analyzing the detector signal and the component-specific standard database to determine a separation component and a corresponding parameter deviation rate; the parameter deviation rate refers to a retention time deviation rate and a half-peak width deviation rate of the separation component; judging whether the parameter deviation rate meets a requirement of the component-specific standard database; if yes, continuously acquiring the detector signal of the chromatograph for cyclic analysis and judgment; if no, acquiring a real-time carrier gas flow rate and a real-time carrier gas purity; analyzing and calculating the real-time carrier gas flow rate and the real-time carrier gas purity according to a preset extended van deemter equation to determine a theoretical plate height of the separation component; analyzing the theoretical plate height, the real-time carrier gas flow rate and the parameter deviation rate to determine a final adjustment flow rate; controlling an electronic gas circuit to control and adjust the carrier gas flow rate according to the final adjustment flow rate; the step of analyzing the theoretical plate height, the real-time carrier gas flow rate and the parameter deviation rate to determine the final adjustment flow rate comprises: calculating a partial derivative of the real-time carrier gas flow rate with respect to the theoretical plate height and setting the partial derivative to zero to generate a real-time optimal flow rate; analyzing the real-time optimal flow rate, the parameter deviation rate and the real-time carrier gas flow rate to determine the final adjustment flow rate; the step of analyzing the real-time optimal flow rate, the parameter deviation rate and the real-time carrier gas flow rate to determine the final adjustment flow rate comprises: analyzing the parameter deviation rate and a preset deviation correction coefficient to determine a flow rate adjustment coefficient; analyzing the flow rate adjustment coefficient and the real-time optimal flow rate to determine an actual optimal flow rate; analyzing the actual optimal flow rate and the real-time carrier gas flow rate to determine a basic adjustment flow rate; analyzing the basic adjustment flow rate to determine the final adjustment flow rate; the step of analyzing the basic adjustment flow rate to determine the final adjustment flow rate comprises: analyzing the separation component and the component-specific standard database to determine a component theoretical plate number and a standard theoretical plate total number; analyzing the component theoretical plate number and the standard theoretical plate total number to determine a component flow rate weight; analyzing the component flow rate weight and the basic adjustment flow rate to determine the final adjustment flow rate.
2. The method of claim 1, wherein, the step of analyzing the detector signal and the component-specific standard database to determine the separation component and the corresponding parameter deviation rate comprises: cutting the detector signal according to a preset sliding window width to generate a window analysis signal; analyzing the window analysis signal to determine a peak top point time, a peak top point signal and a half-peak time; acquiring an injection time; analyzing the peak top point time and the injection time to determine a real-time retention time; analyzing the half-peak time and the peak top point time to determine a real-time half-peak width; analyzing the real-time retention time, the real-time half-peak width and the component-specific standard database to determine the separation component and the corresponding parameter deviation rate.
3. A method of controlling gas admission to a chromatograph according to claim 2, wherein, the step of analyzing the window analysis signal to determine the peak top point time, the peak top point signal and the half-peak time comprises: deriving the window analysis signal to determine a signal first-order derivative and a signal second-order derivative; When the first derivative of the signal and the second derivative of the signal meet the preset peak starting point condition requirement, it is determined whether the first derivative of the signal and the second derivative of the signal meet the preset peak vertex condition requirement; If not, the detector signal is continuously intercepted according to the sliding window width to generate a window analysis signal; If yes, a real-time recording time and a real-time recording signal are obtained, and the real-time recording time is defined as a peak vertex time and the real-time recording signal is defined as a peak vertex signal; The real-time recording signal and the window analysis signal are analyzed to determine a half-peak time.
4. A method of controlling gas admission to a chromatograph according to claim 3, wherein, The step of analyzing the real-time recording signal and the window analysis signal to determine the half-peak time comprises: The real-time recording signal is analyzed to determine a half-peak signal; It is determined whether the window analysis signal meets the half-peak signal requirement; If not, the detector signal is continuously intercepted according to the sliding window width to generate a window analysis signal; If yes, a meeting window time is obtained, and the meeting window time is defined as the half-peak time.
5. A chromatograph gas inlet control system characterized by, It comprises: An acquisition module is configured to acquire a detector signal, a component-specific standard database, a real-time carrier gas flow rate, and a real-time carrier gas purity; A memory is configured to store a program of the gas inlet control method of the chromatograph according to any one of claims 1 to 4; A processor is configured to load and execute the program in the memory, and implement the gas inlet control method of the chromatograph according to any one of claims 1 to 4.
6. A smart terminal, characterized by It comprises a memory and a processor, and the memory stores a computer program capable of being loaded and executed by the processor to implement the gas inlet control method of the chromatograph according to any one of claims 1 to 4.
7. A computer readable storage medium characterized in that, It stores a computer program capable of being loaded and executed by the processor to implement the gas inlet control method of the chromatograph according to any one of claims 1 to 4.
Citation Information
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