A chromatograph sample injection method, system, intelligent terminal and storage medium

Abstract

The application relates to a chromatograph sampling method and system, an intelligent terminal and a storage medium, and relates to the technical field of chromatographs. The application comprises the following steps: acquiring a reference dead volume of a preset sampling needle and sampling sample parameters; determining a sample reference adhesion amount according to the sampling sample parameters and a preset sample adhesion relationship; analyzing the reference dead volume, the reference adhesion amount and the sampling sample parameters to determine an actual sampling sample amount; controlling the sampling needle to sample from a preset sample bottle according to the actual sampling sample amount, and controlling the sampling needle to flush the sample into a preset chromatographic column. The application has the effect of improving the accuracy of chromatograph sampling.

Description

Technical Field

[0001] This application relates to the technical field of chromatographs, and in particular to a chromatograph injection method, system, intelligent terminal and storage medium. Background Technology

[0002] A chromatograph is an instrument that uses chromatography to separate and analyze components in a complex mixture, allowing for qualitative or quantitative analysis.

[0003] In related technologies, when the liquid chromatograph uses a partial filling mode for sample injection, a flow needle design is usually adopted. The needle moves to the sample vial, and the metering pump controls the needle to draw a set volume of sample from the sample vial. Then the needle carries the sample to the injection port and inserts into the needle seat. At this time, the inner cavity of the needle is connected to the high-pressure flow path, and the high-pressure mobile phase flows directly through the inner cavity of the needle, flushing the sample into the chromatographic column.

[0004] Regarding the aforementioned technologies, the quantitative pump uses a set volume control needle to draw samples from the sample vial. However, due to the dead volume of the needle itself and the adhesion effect of the sample after contact with the flow path, the amount of sample entering the chromatographic column is less than the set volume, resulting in inaccurate injection into the chromatograph. There is still room for improvement. Summary of the Invention

[0005] To improve the accuracy of chromatograph injection, this application provides a chromatograph injection method, system, intelligent terminal, and storage medium.

[0006] Firstly, this application provides a chromatograph injection method, employing the following technical solution:

[0007] A chromatograph injection method, comprising:

[0008] Obtain the baseline dead volume of the preset sampling needle and the sampling sample parameters;

[0009] The baseline adhesion amount of the sample is determined based on the sample parameters and the preset sample adhesion relationship;

[0010] The baseline dead volume, baseline adhesion amount, and sample parameters were analyzed to determine the actual sample quantity.

[0011] The sampling needle is controlled to take samples from the preset sample vial according to the actual sample volume, and the sampling needle is controlled to flush the sample into the preset chromatographic column.

[0012] By adopting the above technical solution, the reference adhesion amount of the sample is determined based on the sample parameters and the sample adhesion relationship. After analyzing the reference dead volume, reference adhesion amount and sample parameters, the actual sample quantity is obtained. Then, the sampling needle is controlled to take the sample from the sample vial based on the actual sample quantity and flush the sample into the chromatographic column. This takes into account the influence of dead volume and adhesion effect on the sample quantity during the sampling process, thereby improving the accuracy of chromatograph injection.

[0013] Optionally, the steps of analyzing the baseline dead volume, baseline adhesion amount, and sample parameters to determine the actual sample quantity include:

[0014] Obtain real-time monitoring temperature and flow path usage count;

[0015] The actual dead volume is determined by analyzing the baseline dead volume, real-time temperature, and number of times the flow path is used.

[0016] Determine the sample viscosity and sample contact time based on the sample parameters.

[0017] The sample viscosity, reference adhesion amount, sample contact time, preset reference viscosity, and preset surface adsorption coefficient are analyzed to determine the actual adhesion amount.

[0018] The parameters of the sampled sample, the actual dead volume, and the actual amount of adhesion were analyzed to determine the actual amount of sampled sample.

[0019] By adopting the above technical solution, the reference dead volume, real-time detection temperature, and flow path usage frequency are analyzed to consider the influence of temperature on the dead volume and obtain the actual dead volume. Then, the sample viscosity, reference adhesion amount, sample contact time, reference viscosity, and surface adsorption coefficient are analyzed to consider the influence of viscosity and contact time on the adhesion amount and determine the actual adhesion amount. Finally, the sample parameters, actual dead volume, and actual adhesion amount are added together to obtain the actual sample quantity, thereby improving the accuracy of the actual sample quantity.

[0020] Optionally, the steps to determine the actual dead volume by analyzing the baseline dead volume, real-time monitored temperature, and flow path usage count include:

[0021] The real-time detected temperature and the preset reference temperature are analyzed to determine the temperature deviation;

[0022] The temperature deviation, reference dead volume, and preset temperature coefficient are analyzed to determine the temperature correction volume;

[0023] The number of times the flow path is used and the preset maximum number of times the flow path is used are analyzed to determine the aging degree of the flow path;

[0024] The baseline dead volume, flow path aging degree, and preset aging coefficient are analyzed to determine the aging correction volume;

[0025] The baseline dead volume, temperature-corrected volume, and aging-corrected volume were analyzed to determine the actual dead volume.

[0026] By adopting the above technical solution, the temperature deviation, reference dead volume and temperature coefficient are analyzed to consider the influence of temperature on volume and obtain the temperature-corrected volume. Then, the aging degree and aging coefficient of the flow path are analyzed to consider the influence of flow path aging on volume and obtain the aging-corrected volume. Finally, the sum of the reference dead volume, temperature-corrected volume and aging-corrected volume is calculated to obtain the actual dead volume, thereby improving the accuracy of the actual dead volume.

[0027] Optionally, the steps of analyzing the sample parameters, actual dead volume, and actual adhesion amount to determine the actual sample quantity include:

[0028] Determine the required sample quantity based on the sample parameters.

[0029] The required sample volume, actual dead volume, and actual adhesion amount were analyzed to determine the basic sample volume.

[0030] The required injection peak area is determined based on the relationship between the required sample volume and the preset sample peak area.

[0031] Obtain the peak area of ​​historical sample injections;

[0032] Analyze the historical injection peak area and the required injection peak area to determine the peak area difference;

[0033] The peak area difference and the preset volume peak area coefficient are analyzed to determine the error compensation amount;

[0034] The basic sample quantity and error compensation quantity are analyzed to determine the actual sample quantity.

[0035] By adopting the above technical solution, the peak area of ​​historical injection and the peak area of ​​required injection are analyzed to obtain the peak area difference. Then, the error compensation amount is calculated by using the peak area difference and the volume peak area coefficient. This takes into account the error amount in actual sampling, calculates the sum of the basic sampling sample amount and the error compensation amount to obtain the actual sampling sample amount, and thus improves the accuracy of the actual sampling sample amount.

[0036] Optionally, the steps for controlling the sampling needle to take samples from a preset sample vial based on the actual sample volume include:

[0037] The actual sample quantity and sample parameters were analyzed to determine the total real-time absorption.

[0038] The total real-time absorption volume and the actual sample volume were analyzed to determine the sample return volume;

[0039] Control the sampling needle to take samples from the sample vial at the total real-time aspiration volume and acquire the sampling completion trigger signal;

[0040] The sampling needle is controlled to retract the sample into the sample vial according to the sampling completion trigger signal to complete the sampling.

[0041] By adopting the above technical solution, the sampling needle is controlled to take samples from the sample bottle with a real-time total aspiration volume, and then the sampling needle is controlled to retract the sample into the sample bottle with a sample retraction volume to complete the sampling. This reduces the influence of gas on the sample volume during sampling and thus improves the accuracy of sampling.

[0042] Optionally, the steps of analyzing the actual sample volume and sample parameters to determine the real-time total absorption include:

[0043] Determine the sampling viscosity based on the sample parameters;

[0044] Analyze the sample viscosity to determine the viscosity correction term;

[0045] The actual sample volume, viscosity correction term, and preset basic safety margin coefficient are analyzed to determine the real-time total absorption volume.

[0046] By adopting the above technical solution, a viscosity correction term is obtained after analyzing the sample viscosity. The actual sample quantity is then corrected using the viscosity correction term and the basic safety margin coefficient to obtain the real-time total absorption quantity. This takes into account the influence of viscosity on the actual absorption quantity and the influence of the back-off quantity on the absorption quantity, thereby improving the accuracy of the real-time absorption quantity.

[0047] Optionally, the step of controlling the sampling needle to retract the sample into the sample vial by the sample retraction amount, based on the sampling completion trigger signal, includes:

[0048] The sampled viscosity and the preset reference viscosity are analyzed to determine the viscosity adjustment factor;

[0049] The viscosity adjustment coefficient and the preset reference viscosity rollback rate are analyzed to determine the actual rollback rate;

[0050] Based on the sampling completion trigger signal, the sampling needle is controlled to retract the sample into the sample vial at the actual retraction speed and sample retraction amount to complete the sampling.

[0051] By adopting the above technical solution, the viscosity adjustment coefficient is obtained after analyzing the sample viscosity and the reference viscosity. Then, the actual retraction speed is obtained by correcting the reference viscosity retraction speed with the viscosity adjustment coefficient. The sample is then retracted into the sample bottle at the actual retraction speed, minimizing the generation of air bubbles during the retraction process and thus improving the accuracy of retraction control.

[0052] Secondly, this application provides a chromatograph injection system, which adopts the following technical solution:

[0053] A chromatograph sample introduction system, comprising:

[0054] The acquisition module is used to acquire the baseline dead volume and sample parameters;

[0055] A memory for storing a program for a chromatograph injection method as described in any of the preceding claims;

[0056] The processor and the program in the memory can be loaded and executed by the processor to implement a chromatograph injection method as described in any of the above.

[0057] By adopting the above technical solution, the processor loads and executes a chromatograph injection method program stored in the memory, controls the acquisition module to acquire a series of data related to chromatograph injection, and determines the reference adhesion amount of the sample based on the sample parameters and the sample adhesion relationship. After analyzing the reference dead volume, reference adhesion amount and sample parameters, the actual sample volume is obtained. Then, based on the actual sample volume, the sampling needle is controlled to take the sample from the sample vial and flush the sample into the chromatographic column. This takes into account the influence of dead volume and adhesion effect on the sample volume during the sampling process, thereby improving the accuracy of chromatograph injection.

[0058] Thirdly, this application provides a smart terminal, which adopts the following technical solution:

[0059] 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, a chromatograph injection method.

[0060] By adopting the above technical solution, the processor loads and executes a computer program for a chromatograph injection method stored in the memory through the operation of the intelligent terminal. The sample reference adhesion amount is determined based on the sample parameters and the sample adhesion relationship. After analyzing the reference dead volume, reference adhesion amount and sample parameters, the actual sample amount is obtained. Then, the sampling needle is controlled to take the sample from the sample vial and flush the sample into the chromatographic column based on the actual sample amount. This takes into account the influence of dead volume and adhesion effect on the sample amount during the sampling process, thereby improving the accuracy of chromatograph injection.

[0061] Fourthly, this application provides a computer storage medium capable of storing corresponding programs, which facilitates improving the accuracy of chromatograph sample injection, and adopts the following technical solution:

[0062] A computer-readable storage medium storing a computer program that can be loaded by a processor and executed any of the above-described chromatograph injection methods.

[0063] By adopting the above technical solution, a computer program for a chromatograph injection method is stored in a computer-readable storage medium. The processor loads and executes the computer program in the storage medium, thereby determining the reference adhesion amount of the sample based on the sample parameters and the sample adhesion relationship. After analyzing the reference dead volume, reference adhesion amount, and sample parameters, the actual sample amount is obtained. Then, based on the actual sample amount, the sampling needle is controlled to take the sample from the sample vial and flush the sample into the chromatographic column. This takes into account the influence of dead volume and adhesion effect on the sample amount during the sampling process, thereby improving the accuracy of chromatograph injection.

[0064] In summary, this application includes at least one of the following beneficial technical effects:

[0065] 1. By determining the reference adhesion amount of the sample based on the sampling parameters and the sample adhesion relationship, the actual sample amount is obtained after analyzing the reference dead volume, reference adhesion amount and sampling parameters. Then, the sampling needle is controlled to take the sample from the sample vial and flush the sample into the chromatographic column based on the actual sample amount. This takes into account the influence of dead volume and adhesion effect on the sample amount during the sampling process, thereby improving the accuracy of chromatograph injection.

[0066] 2. By analyzing the baseline dead volume, real-time temperature, and number of times the flow path is used, the influence of temperature on the dead volume is considered to obtain the actual dead volume. Then, the sample viscosity, baseline adhesion amount, sample contact time, baseline viscosity, and surface adsorption coefficient are analyzed to consider the influence of viscosity and contact time on the adhesion amount, so as to determine the actual adhesion amount. Finally, the sample parameters, actual dead volume, and actual adhesion amount are added together to obtain the actual sample quantity, thereby improving the accuracy of the actual sample quantity.

[0067] 3. By controlling the sampling needle to take samples from the sample vial with a real-time total aspiration volume, and then controlling the sampling needle to retract the sample back into the sample vial with a sample retraction volume to complete the sampling, the influence of gas on the sample volume during sampling is reduced, thereby improving the accuracy of sampling. Attached Figure Description

[0068] Figure 1 This is a flowchart of a chromatograph injection method in an embodiment of this application.

[0069] Figure 2This is a flowchart illustrating the steps in this application embodiment to analyze the baseline dead volume, baseline adhesion amount, and sample parameters to determine the actual sample quantity.

[0070] Figure 3 This is a flowchart of the steps in this application embodiment to analyze the baseline dead volume, real-time detection temperature, and flow path usage frequency to determine the actual dead volume.

[0071] Figure 4 This is a flowchart illustrating the steps in this application embodiment to analyze the sample parameters, actual dead volume, and actual adhesion amount to determine the actual sample quantity.

[0072] Figure 5 This is a flowchart illustrating the steps of controlling the sampling needle to take samples from a preset sample bottle based on the actual sample volume in this embodiment of the application.

[0073] Figure 6 This is a flowchart illustrating the steps in this application embodiment to analyze the actual sample quantity and sample parameters to determine the real-time total absorption volume.

[0074] Figure 7 This is a flowchart illustrating the steps in this application where the sampling needle is controlled to retract the sample into the sample vial according to the sampling completion trigger signal to complete the sampling. Detailed Implementation

[0075] 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.

[0076] Reference Figure 1 This application discloses a chromatograph injection method, including the following steps:

[0077] Step S100: Obtain the baseline dead volume of the preset sampling needle and the sampling parameters.

[0078] The sampling needle refers to a device used to transfer a sample from a sample vial to a chromatographic column. In this embodiment, a flow needle is used.

[0079] The reference dead volume refers to the area in the sampling needle that results in the actual sample volume being less than the required sample volume. In partial fill mode, the sample only fills the set volume segment of the needle cavity, while the connecting segment between the needle tip and the needle seat (such as the gap between the needle shaft and the needle seat) is the dead volume. Water is used for detection. The injection volume is set, and the corresponding peak area of ​​the chromatograph is recorded. Then, it is gradually increased to another volume. When the peak area no longer increases significantly with the increase of volume, it indicates that the dead volume has been completely filled. The difference between the two volumes is the dead volume.

[0080] Sampling parameters refer to parameters such as sample type, viscosity, quantity, and time, which are determined by the operator based on the actual condition of the sample and actual needs, and then entered into the processing terminal.

[0081] Step S101: Determine the baseline adhesion amount of the sample based on the sample parameters and the preset sample adhesion relationship.

[0082] Among them, the sample adhesion relationship refers to the amount of adhesion of different types of samples in the flow path. The operator injects different samples into the flow path in a quantitative manner and then recovers them, thereby calculating the difference in sample amount before and after to obtain the amount of adhesion of the sample. The operator then forms a mapping table that maps the sample type to the amount of adhesion.

[0083] The baseline adhesion amount of a sample refers to the amount of adhesion of the sample in an ideal environment. It is obtained by the processing terminal by looking up the sample adhesion relationship in a mapping table based on the sample type corresponding to the sample parameters.

[0084] Step S102: Analyze the baseline dead volume, baseline adhesion amount, and sample parameters to determine the actual sample quantity.

[0085] The actual sample volume refers to the sample volume that ensures the amount of sample entering the chromatographic column meets the usage requirements. This volume is obtained by analyzing the reference dead volume, reference adhesion, and sample parameters at the processing terminal. Specific methods are detailed in [reference needed]. Figure 2 The steps.

[0086] Step S103: Control the sampling needle to take a sample from the preset sample vial according to the actual sample volume, and control the sampling needle to flush the sample into the preset chromatographic column.

[0087] After determining the actual sample volume, the processing terminal controls the sampling needle to extract samples from the sample vial based on the actual sample volume. The specific method is described in [reference needed]. Figure 5 The steps involve controlling the high-pressure mobile phase to flush the sample from the sampling needle into the chromatographic column, thereby completing the injection.

[0088] A sample vial is a container for holding samples. A chromatographic column is a tube containing a stationary phase, connected at both ends to a mobile phase delivery system.

[0089] Reference Figure 2 The steps for determining the actual sample quantity by analyzing the baseline dead volume, baseline adhesion amount, and sample parameters include:

[0090] Step S200: Obtain the real-time detection temperature and the number of times the flow path is used.

[0091] Among them, real-time temperature detection refers to the real-time temperature when the sampling needle takes a sample. It is detected by a temperature sensor and sent to the processing terminal to provide data support for subsequent analysis of the effect of temperature on volume.

[0092] The number of times the flow path is used refers to the number of times the sampling needle flow path is used. It is accumulated when the processing terminal controls the sampling needle to take samples, and is used to provide data support for subsequent analysis of the impact of flow path wear on volume.

[0093] Step S201: Analyze the baseline dead volume, real-time detection temperature, and number of times the flow path is used to determine the actual dead volume.

[0094] The actual dead volume refers to the dead volume of the sampling needle after being affected by external environmental factors and usage. It is obtained by the processing terminal through analysis of the baseline dead volume, real-time detection temperature, and the number of times the flow path has been used. For specific methods, please refer to [link / reference needed]. Figure 3 The steps.

[0095] Step S202: Determine the sample viscosity and sample contact time based on the sample parameters.

[0096] Sample viscosity refers to the real-time dynamic viscosity of the sample, reflecting its flowability. Higher viscosity indicates poorer flowability and a greater likelihood of residue buildup. A miniature vibrating viscosity sensor can be integrated near the sampling needle to detect viscosity in real time during sampling. Sample contact time refers to the time it takes for the sample to travel from the sampling needle to the chromatographic column, and is determined by the operator based on actual needs.

[0097] Step S203: Analyze the sample viscosity, reference adhesion amount, sample contact time, preset reference viscosity, and preset surface adsorption coefficient to determine the actual adhesion amount.

[0098] The reference viscosity refers to the viscosity of water, which is 1 centipoise. The surface adsorption coefficient is a parameter indicating the strength of the adsorption between the sample and the flow path material. The larger the surface adsorption coefficient, the faster the amount of adhesion increases per unit time. Operators can conduct experiments using the same sample and material to detect the amount of adhesion at different contact times, and then plot a curve with the amount of adhesion and time, and calculate the slope of the curve.

[0099] The actual adhesion amount refers to the amount of sample that adheres under the influence of the sampling needle. The viscosity influence value is obtained by taking the square root of the quotient of the sample viscosity and the reference viscosity from the processing terminal. Then, the adsorption influence value is obtained by multiplying the sample contact time and the surface adsorption coefficient by 1. Finally, the actual adhesion amount is obtained by multiplying the reference adhesion amount, the viscosity influence value, and the adsorption influence value.

[0100] Step S204: Analyze the sample parameters, actual dead volume, and actual adhesion amount to determine the actual sample quantity.

[0101] The actual sample quantity in this step is consistent with the actual sample quantity in step S102, and is obtained by the processing terminal after analyzing the sample parameters, actual dead volume, and actual adhesion amount. The specific method is described in [reference needed]. Figure 4 The steps.

[0102] Reference Figure 3 The steps to determine the actual dead volume by analyzing the baseline dead volume, real-time temperature, and number of times the flow path has been used include:

[0103] Step S300: Analyze the real-time detected temperature and the preset reference temperature to determine the temperature deviation.

[0104] The reference temperature refers to the standard temperature for calculating temperature deviation; in this embodiment, 25 degrees Celsius is used as an example.

[0105] Temperature deviation refers to the difference between the sampling temperature and the reference temperature. It is calculated by the processing terminal based on the difference between the real-time detection temperature and the reference temperature, providing data support for subsequent determination of the impact of temperature on dead volume.

[0106] Step S301: Analyze the temperature deviation, the reference dead volume, and the preset temperature coefficient to determine the temperature correction volume.

[0107] The temperature coefficient refers to the relative change rate of dead volume caused by a unit temperature change. It reflects the thermal expansion and contraction properties of the flow path material. It is obtained by the operator setting different temperatures in the temperature control chamber, measuring the dead volume at the corresponding temperature, and then calculating it through linear fitting.

[0108] Temperature-corrected volume refers to the effect of temperature on dead volume, which is obtained by multiplying the temperature deviation, the reference dead volume, and the temperature coefficient calculated by the processing terminal.

[0109] Step S302: Analyze the number of times the flow path is used and the preset maximum number of times the flow path is used to determine the aging degree of the flow path.

[0110] The maximum number of times a flow path can be used refers to the number of times the flow path can be used, which is determined by the operator according to the user manual.

[0111] Flow path aging degree refers to a quantitative indicator of the aging state of the flow path, which is obtained by calculating the quotient between the number of times the flow path is used and the maximum number of times the flow path is used by the processing terminal.

[0112] Step S303: Analyze the baseline dead volume, flow path aging degree, and preset aging coefficient to determine the aging correction volume.

[0113] The aging coefficient refers to the relative change rate of dead volume caused by unit aging degree, reflecting the degree of influence of flow path wear or deformation on dead volume. The operator measures the initial dead volume of the new system, simulates actual use, measures the dead volume periodically, defines the aging degree at this time, fits the relationship between dead volume and aging degree, and calculates the aging coefficient by least squares method.

[0114] The aging correction volume refers to the impact of flow path aging on the dead volume, which is obtained by multiplying the flow path aging degree, aging coefficient and reference dead volume at the processing terminal.

[0115] Step S304: Analyze the baseline dead volume, temperature-corrected volume, and aging-corrected volume to determine the actual dead volume.

[0116] The actual dead volume in this step is consistent with the actual dead volume in step S201, and is obtained by the processing terminal by calculating the sum of the reference dead volume, the temperature correction volume, and the aging correction volume.

[0117] Reference Figure 4 The steps for determining the actual sample quantity by analyzing the sample parameters, actual dead volume, and actual adhesion amount include:

[0118] Step S400: Determine the required sample quantity based on the sample parameters.

[0119] The required sample quantity refers to the amount of sample required to enter the chromatographic column, which is obtained by the processing terminal from the sample parameters.

[0120] Step S401: Analyze the required sample quantity, actual dead volume, and actual adhesion amount to determine the basic sample quantity.

[0121] The basic sampling quantity refers to the sampling quantity after correction for dead volume and adhesion amount, which is obtained by the processing terminal by calculating the required sample quantity, actual dead volume and actual adhesion amount.

[0122] Step S402: Determine the required injection peak area based on the required sample volume and the preset sample peak area relationship.

[0123] The peak area relationship refers to the ratio coefficient between different sample amounts and peak areas. In this embodiment, 0.005 is used as an example.

[0124] The peak area required for sample injection refers to the peak area corresponding to the required sample volume, which is obtained by the processing terminal calculating the quotient between the required sample volume and the sample peak area.

[0125] Step S403: Obtain the area of ​​historical injection peaks.

[0126] Among them, the historical injection peak area refers to the actual peak area at the time of the last injection, which is recorded by the processing terminal.

[0127] Step S404: Analyze the historical injection peak area and the required injection peak area to determine the peak area difference.

[0128] The peak area difference refers to the difference between the peak area during actual injection and simulated injection, which is obtained by the processing terminal calculating the difference between the historical injection peak area and the required injection peak area.

[0129] Step S405: Analyze the peak area difference and the preset volume peak area coefficient to determine the error compensation amount.

[0130] The volume peak area coefficient refers to the ratio of different sample volumes to peak areas; in this application, 0.005 is used as an example.

[0131] Error compensation refers to the error value between the actual injection and the simulated injection, which is obtained by multiplying the peak area difference and the volume peak area coefficient calculated by the processing terminal.

[0132] Step S406: Analyze the basic sample quantity and error compensation quantity to determine the actual sample quantity.

[0133] In this step, the actual sample quantity is consistent with the actual sample quantity in step S204. It is obtained by the processing terminal by calculating the sum of the basic sample quantity and the error compensation quantity, thereby closing the loop to correct unmodeled errors such as sensor measurement deviation and sample volatilization.

[0134] Reference Figure 5 The steps for controlling the sampling needle to take samples from the preset sample vial according to the actual sample volume include:

[0135] Step S500: Analyze the actual sample quantity and sample parameters to determine the real-time total absorption.

[0136] The real-time total sample volume refers to the total amount of sample drawn from the sample vial by the sampling needle. It is calculated by adding dead volume, adhesion, error, viscosity influence, and safety margin to the required volume. This is obtained by the processing terminal after analyzing the actual sample volume and sample viscosity parameters. For specific methods, please refer to [reference needed]. Figure 6 The steps.

[0137] Step S501: Analyze the real-time total absorption volume and the actual sample volume to determine the sample return volume.

[0138] Among them, the sample return amount refers to the amount of sample returned to the sample vial by the sampling needle. It is obtained by the processing terminal by calculating the difference between the real-time total aspirate amount and the actual sample aspirate amount, which provides data support for subsequent control of the sample return of the sampling needle.

[0139] Step S502: Control the sampling needle to take a sample from the sample vial at the real-time total aspiration volume, and obtain a sampling completion trigger signal.

[0140] After determining the total real-time aspiration volume, the processing terminal controls the sampling needle to take samples from the sample vial at the total real-time aspiration volume. After sampling is completed, a sampling completion trigger signal is output to provide data support for subsequent sample return.

[0141] The sampling completion trigger signal is the signal that the sampling needle has completed sampling from the sample vial. After the metering pump controls the sampling needle to complete sampling, the electrical signal indicating the sampling completion trigger signal is sent to the processing terminal.

[0142] Step S503: Based on the sampling completion trigger signal, control the sampling needle to retract the sample into the sample vial by the sample retraction amount to complete the sampling.

[0143] Upon receiving a sampling completion trigger signal, the processing terminal responds by controlling the sampling needle to retract the sample into the sample vial by the specified sample retraction amount. The specific method is described in [reference needed]. Figure 7 This process eliminates air bubbles and dead volume residues during sampling, thereby improving the quality of subsequent injections.

[0144] Reference Figure 6 The steps for determining the real-time total absorption volume by analyzing the actual sample quantity and sample parameters include:

[0145] Step S600: Determine the sampling viscosity based on the sample parameters.

[0146] Among them, the sampling viscosity refers to the viscosity of the sample, which is identified by the processing terminal from the sampling parameters.

[0147] Step S601: Analyze the sample viscosity to determine the viscosity correction term.

[0148] The viscosity correction term refers to the correction value of viscosity for the amount of sample taken. It is obtained by multiplying the natural logarithm of the sample viscosity calculated by the processing terminal by a conversion factor, and then adding 1. The higher the viscosity, the more air bubbles are introduced during the aspiration process, thus requiring a larger aspiration volume to ensure accurate sample injection. The conversion factor quantifies the degree of influence of sample viscosity on the additional aspiration volume, ensuring that air bubbles are avoided during the aspiration of high-viscosity samples, while also preventing excessive sample waste. In this embodiment, 0.05 is used as an example.

[0149] Step S602: Analyze the actual sample volume, viscosity correction term, and preset basic safety margin coefficient to determine the real-time total absorption volume.

[0150] The basic safety margin coefficient refers to the ratio of the backoff amount to the total amount. In this embodiment, 1.1 is used as an example.

[0151] The real-time total absorption in this step is consistent with the real-time total absorption in step S500, and is obtained by the processing terminal by calculating the product between the actual sample quantity, viscosity correction term and basic safety margin factor.

[0152] Reference Figure 7 The steps for completing the sampling process, based on the sampling completion trigger signal, include controlling the sampling needle to retract the sample into the sample vial by the sample retraction amount:

[0153] Step S700: Analyze the sampled viscosity and the preset reference viscosity to determine the viscosity adjustment factor.

[0154] The reference viscosity refers to the standard viscosity used to analyze the effect of the sample viscosity on the retraction speed, which is the viscosity of water.

[0155] The viscosity adjustment coefficient refers to the coefficient of influence of viscosity on the retraction speed. It is obtained by calculating the quotient between the reference viscosity and the sample viscosity at the processing terminal. It achieves an adaptive adjustment that the higher the viscosity, the slower the retraction speed, thereby reducing the turbulence generated by the liquid flow inertia of the sample, which causes some samples to adhere to the needle wall or needle tip gap.

[0156] Step S701: Analyze the viscosity adjustment coefficient and the preset reference viscosity rollback speed to determine the actual rollback speed.

[0157] The reference viscosity retreat rate refers to the retreat rate at the standard viscosity. In this embodiment, 5 microliters per second is used as an example.

[0158] The actual retraction speed refers to the speed at which the sample is retracted from the sampling needle into the sample vial. It is obtained by calculating the product between the viscosity adjustment coefficient and the reference viscosity retraction speed using the processing terminal.

[0159] Step S702: Based on the sampling completion trigger signal, control the sampling needle to retract the sample into the sample vial at the actual retraction speed and sample retraction amount to complete the sampling.

[0160] In this process, after the processing terminal receives the sampling completion trigger signal, it responds to the sampling completion trigger signal by controlling the sampling needle to retract the sample into the sample vial at the actual retraction speed. This ensures that the amount of sample entering the chromatographic column after removing the dead volume and adhering amount is the required amount, and also ensures that there are no air bubbles or dead volume residues in the sampling needle, thereby ensuring the quality of the injection.

[0161] Based on the same inventive concept, embodiments of this application provide a chromatograph sample injection system, including:

[0162] The acquisition module is used to acquire the baseline dead volume, real-time detection temperature of sample parameters, flow path usage count, and historical injection peak area;

[0163] A memory used to store the program for a chromatograph injection method;

[0164] The processor is a program in memory that can be loaded and executed by the processor to implement a chromatograph injection method.

[0165] 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.

[0166] This application provides a computer-readable storage medium storing a computer program that can be loaded by a processor and executed as a chromatograph injection method.

[0167] 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.

[0168] Based on the same inventive concept, embodiments of this application provide a smart terminal, including a memory and a processor, wherein the memory stores a computer program that can be loaded by the processor and executed as a chromatograph injection method.

[0169] 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.

[0170] 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 injecting a sample into a chromatograph, the method comprising: The method comprises the following steps: acquiring a preset reference dead volume and sampling sample parameters; determining a sample reference adhesion amount according to the sampling sample parameters and a preset sample adhesion relationship; analyzing the reference dead volume, the reference adhesion amount and the sampling sample parameters to determine an actual sampling sample amount; controlling the sampling needle to sample from a preset sample bottle according to the actual sampling sample amount, and controlling the sampling needle to flush the sample into a preset chromatographic column; the step of analyzing the reference dead volume, the reference adhesion amount and the sampling sample parameters to determine the actual sampling sample amount comprises: acquiring a real-time detection temperature and a flow path use frequency; analyzing the reference dead volume, the real-time detection temperature and the flow path use frequency to determine an actual dead volume; determining a sample viscosity and a sample contact time according to the sampling sample parameters; analyzing the sample viscosity, the reference adhesion amount, the sample contact time, a preset reference viscosity and a preset surface adsorption coefficient to determine an actual adhesion amount; analyzing the sampling sample parameters, the actual dead volume and the actual adhesion amount to determine the actual sampling sample amount; the step of controlling the sampling needle to sample from the preset sample bottle according to the actual sampling sample amount comprises: analyzing the actual sampling sample amount and the sampling sample parameters to determine a real-time total suction amount; analyzing the real-time total suction amount and the actual sampling sample amount to determine a sample back-off amount; controlling the sampling needle to sample from the sample bottle with the real-time total suction amount, and acquiring a sampling completion trigger signal; controlling the sampling needle to back off the sample into the sample bottle with the sample back-off amount to complete sampling according to the sampling completion trigger signal.

2. A method of injecting a sample into a chromatograph according to claim 1, wherein, the step of analyzing the reference dead volume, the real-time detection temperature and the flow path use frequency to determine the actual dead volume comprises: analyzing the real-time detection temperature and a preset reference temperature to determine a temperature deviation; analyzing the temperature deviation, the reference dead volume and a preset temperature coefficient to determine a temperature correction volume; analyzing the flow path use frequency and a preset maximum flow path use frequency to determine a flow path aging degree; analyzing the reference dead volume, the flow path aging degree and a preset aging coefficient to determine an aging correction volume; analyzing the reference dead volume, the temperature correction volume and the aging correction volume to determine the actual dead volume.

3. A method for injecting a sample into a chromatograph according to claim 1, wherein, the step of analyzing the sampling sample parameters, the actual dead volume and the actual adhesion amount to determine the actual sampling sample amount comprises: determining a required sample amount according to the sampling sample parameters; analyzing the required sample amount, the actual dead volume and the actual adhesion amount to determine a basic sampling sample amount; determining a required injection peak area according to the required sample amount and a preset sample peak area relationship; acquiring a historical injection peak area; analyzing the historical injection peak area and the required injection peak area to determine a peak area difference; analyzing the peak area difference and a preset volume peak area coefficient to determine an error compensation amount; analyzing the basic sampling sample amount and the error compensation amount to determine the actual sampling sample amount.

4. The method of claim 1 wherein, the step of analyzing the actual sampling sample amount and the sampling sample parameters to determine the real-time total suction amount comprises: determining a sampling viscosity according to the sampling sample parameters; analyzing the sampling viscosity to determine a viscosity correction term; The actual sampling sample amount, the viscosity correction term and the preset basic safety margin coefficient are analyzed to determine the real-time total suction amount.

5. A method of injecting a sample into a chromatograph according to claim 4, wherein, The step of controlling the sampling needle to back the sample into the sample bottle by the sample back-off amount to complete the sampling according to the sampling completion trigger signal includes: The sampling viscosity and the preset reference viscosity are analyzed to determine a viscosity adjustment coefficient; The viscosity adjustment coefficient and the preset reference viscosity back-off speed are analyzed to determine an actual back-off speed; The sample is back into the sample bottle by the actual back-off speed and the sample back-off amount to complete the sampling according to the sampling completion trigger signal.

6. A chromatograph sample introduction system characterized by, It comprises: An acquisition module is configured to acquire a reference dead volume and sampling sample parameters; A memory is configured to store a program of the chromatographic sample injection method according to any one of claims 1 to 5; A processor, the program in the memory can be loaded and executed by the processor, and the chromatographic sample injection method according to any one of claims 1 to 5 is implemented.

7. A smart terminal, characterized in that It comprises a memory and a processor, and the memory stores a computer program which can be loaded and executed by the processor to implement the chromatographic sample injection method according to any one of claims 1 to 5.

8. A computer-readable storage medium, characterized in that, It stores a computer program which can be loaded and executed by the processor to implement the chromatographic sample injection method according to any one of claims 1 to 5.

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