CN114047276B - Chromatograph control method and device - Google Patents
Chromatograph control method and device Download PDFInfo
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- CN114047276B CN114047276B CN202210046344.0A CN202210046344A CN114047276B CN 114047276 B CN114047276 B CN 114047276B CN 202210046344 A CN202210046344 A CN 202210046344A CN 114047276 B CN114047276 B CN 114047276B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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Abstract
The invention provides a chromatograph control method and a chromatograph control device, which are applied to a carrier gas system of a chromatograph. On one hand, the process of chromatographic analysis is divided into stages, and different types of carrier gases are used in different stages, so that helium is not used in the whole analysis process, and is only used in the specific stage of sample analysis, so that the use amount of helium in the process of chromatographic analysis is reduced, and the analysis result is not influenced. On the other hand, in the process of using helium, the usage amount of the carrier gas in different subdivision stages is controlled, so that the analysis quality and efficiency are ensured, the usage amount of the helium is further reduced, and the analysis cost of the chromatograph is greatly reduced.
Description
Technical Field
The invention relates to the technical field of chromatograph control, in particular to a chromatograph control method and device.
Background
The gas chromatograph is a separation and analysis tool for multi-component mixture, and its principle mainly utilizes the difference of boiling point, polarity and adsorption property of material to implement separation of mixture, including sample-feeding system, detection system, recording and data processing system, temperature control system and carrier gas system, etc. Generally, the carrier gas used to carry the sample for separation, which is the mobile phase of the gas chromatograph, should be an inert gas, and commonly used carrier gases are nitrogen, hydrogen, helium, and argon. Helium is often the carrier gas of choice due to sensitivity, efficiency, chemical inertness, safety or other considerations, but the relatively high price of helium adds significantly to the cost of the assay. Therefore, it is an urgent problem to provide a method for effectively reducing the consumption of carrier gas while ensuring the quality and efficiency of analysis.
Disclosure of Invention
In order to improve the above problems, the present invention provides a chromatograph control method and apparatus.
In a first aspect of the embodiments of the present invention, there is provided a chromatograph control method applied to a carrier gas system of a chromatograph, where the carrier gas system includes a first gas source containing helium gas and a second gas source containing other types of carrier gases, the method including:
detecting the state of the chromatograph, and judging the working stage of the chromatograph;
and performing supply control of the carrier gas according to the judgment result, wherein:
if the device is in the early preparation stage, supplying carrier gas to the chromatograph through a second gas source;
if the sample injection preparation stage is in, supplying carrier gas to the chromatograph through a first gas source, wherein the flow rate of the supplied carrier gas is less than the column flow rate of the chromatograph;
if the detection and analysis stage is in, carrier gas is supplied to the chromatograph through a first gas source, and meanwhile, a split flow or a purge flow is supplied to the chromatograph through a second gas source, wherein the carrier gas flow supplied to the chromatograph through the first gas source is larger than the split flow or the purge flow;
if the detection is completed, the carrier gas is supplied to the chromatograph through the second gas source.
Optionally, the detecting the state of the chromatograph and determining the working stage of the chromatograph may be performed in the following specific manner:
detect chromatographic column temperature, pressure before the post, judge the working phase that the chromatograph is located through parameter value and curve, wherein:
when the detected chromatographic column temperature is lower than the target temperature of the chromatograph, judging that the chromatographic column is in the early preparation stage;
when the detected temperature of the chromatographic column reaches the target temperature, the continuous stabilization time reaches a set first time threshold value, and when the detected pressure in front of the chromatographic column reaches the set target pressure and the continuous stabilization time reaches the set first time threshold value, the chromatographic column is judged to be in the sample preparation stage;
when the sample injection preparation stage is started, the sample injection system of the chromatograph is detected to start sample injection and a set second time threshold value is passed, and the detection and analysis stage is judged to be in;
and when detecting that the temperature of the chromatographic column is reduced and is less than the target temperature of the chromatograph and a third time threshold set by the duration, judging that the chromatographic column is in the detection completion stage.
Optionally, the method further comprises:
recording the actual gas consumption and the gas consumption curve of a first gas source in the whole analysis control process;
comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis, and comparing the gas consumption with the estimated ideal gas consumption; and adjusting the judgment mode of the working stage of the chromatograph according to the comparison result.
Optionally, the determining manner for adjusting the working stage of the chromatograph is specifically:
and respectively increasing or decreasing the sizes of the first time threshold, the second time threshold and the third time threshold according to a preset time interval, and gradually adjusting the setting values of the first time threshold, the second time threshold and the third time threshold under the condition of not influencing the chromatogram effect, so that the gas consumption gradually approaches to the estimated ideal gas consumption.
Optionally, the method further comprises:
recording the actual gas consumption and the gas consumption curve of a first gas source in the whole analysis control process;
comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis, and comparing the gas consumption with the estimated ideal gas consumption;
and adjusting at least one of the carrier gas flow of the sample preparation stage and the carrier gas flow of the detection and analysis stage according to the comparison result.
In a second aspect of the embodiments of the present invention, there is provided a chromatograph control apparatus for a carrier gas system of a chromatograph, the carrier gas system including a first gas source containing helium gas and a second gas source containing other types of carrier gases, the apparatus including:
the working stage judging unit is used for detecting the state of the chromatograph and judging the working stage of the chromatograph;
and a carrier gas control unit for controlling supply of the carrier gas according to the judgment result, wherein:
if the device is in the early preparation stage, supplying carrier gas to the chromatograph through a second gas source;
if the sample injection preparation stage is in, supplying carrier gas to the chromatograph through a first gas source, wherein the flow rate of the supplied carrier gas is less than the column flow rate of the chromatograph;
if the detection and analysis stage is in, carrier gas is supplied to the chromatograph through a first gas source, and meanwhile, a split flow or a purge flow is supplied to the chromatograph through a second gas source, wherein the carrier gas flow supplied to the chromatograph through the first gas source is larger than the split flow or the purge flow;
if the detection is completed, the carrier gas is supplied to the chromatograph through the second gas source.
Optionally, the carrier gas control unit is specifically configured to:
detect chromatographic column temperature, pressure before the post, judge the working phase that the chromatograph is located through parameter value and curve, wherein:
when the detected chromatographic column temperature is lower than the target temperature of the chromatograph, judging that the chromatographic column is in the early preparation stage;
when the detected temperature of the chromatographic column reaches the target temperature, the continuous stabilization time reaches a set first time threshold value, and when the detected pressure in front of the chromatographic column reaches the set target pressure and the continuous stabilization time reaches the set first time threshold value, the chromatographic column is judged to be in the sample preparation stage;
when the sample injection preparation stage is started, the sample injection system of the chromatograph is detected to start sample injection and a set second time threshold value is passed, and the detection and analysis stage is judged to be in;
and when detecting that the temperature of the chromatographic column is reduced and is less than the target temperature of the chromatograph and a third time threshold set by the duration, judging that the chromatographic column is in the detection completion stage.
Optionally, the apparatus further comprises:
the consumption recording unit is used for recording the actual gas consumption and the gas consumption curve of the first gas source in the whole analysis control process;
the first feedback unit is used for comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis and comparing the gas consumption with the estimated ideal gas consumption; and adjusting the judgment mode of the working stage of the chromatograph according to the comparison result.
Optionally, the first feedback unit adjusts a determination mode of a working stage of the chromatograph according to the comparison result, and the specific mode is as follows:
and respectively increasing or decreasing the sizes of the first time threshold, the second time threshold and the third time threshold according to a preset time interval, and gradually adjusting the setting values of the first time threshold, the second time threshold and the third time threshold under the condition of not influencing the chromatogram effect, so that the gas consumption gradually approaches to the estimated ideal gas consumption.
Optionally, the apparatus further comprises:
the consumption recording unit is used for recording the actual gas consumption and the gas consumption curve of the first gas source in the whole analysis control process;
the second feedback unit is used for comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis and comparing the gas consumption with the estimated ideal gas consumption; and adjusting at least one of the carrier gas flow of the sample preparation stage and the carrier gas flow of the detection and analysis stage according to the comparison result.
In summary, the present invention provides a method and an apparatus for controlling a chromatograph, which, on one hand, by dividing the process of the chromatographic analysis into stages and using different types of carrier gases at different stages, helium is not used in the whole analysis process, and helium is only used at the stage of performing specific sample analysis, so that the usage amount of helium in the process of the chromatographic analysis is reduced, and the analysis result is not affected. On the other hand, in the process of using helium, the usage amount of the carrier gas in different subdivision stages is controlled, so that the analysis quality and efficiency are ensured, the usage amount of the helium is further reduced, and the analysis cost of the chromatograph is greatly reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic view of an application scenario of a chromatograph control method according to an embodiment of the present invention;
fig. 2 is a flowchart of a method of controlling a chromatograph according to an embodiment of the present invention;
fig. 3 is a flowchart of a method of controlling a chromatograph according to another embodiment of the present invention;
fig. 4 is a functional block diagram of a control device for a chromatography apparatus according to an embodiment of the present invention.
Fig. 5 is a functional block diagram of a control device for a chromatography apparatus according to another embodiment of the present invention.
Icon:
a carrier gas system 100; a separation system 200; the detection and recording system 300; a temperature control system 400; a sample introduction system 500; a working phase determination unit 110; a carrier gas control unit 120; a consumption recording unit 130; a first feedback unit 140; a second feedback unit 150.
Detailed Description
The gas chromatograph is a separation and analysis tool for multi-component mixture, and its principle mainly utilizes the difference of boiling point, polarity and adsorption property of material to implement separation of mixture, including sample-feeding system, detection system, recording and data processing system, temperature control system and carrier gas system, etc. Generally, the carrier gas used to carry the sample for separation, which is the mobile phase of the gas chromatograph, should be an inert gas, and commonly used carrier gases are nitrogen, hydrogen, helium, and argon. Helium is often the carrier gas of choice due to sensitivity, efficiency, chemical inertness, safety or other considerations, but the relatively high price of helium adds significantly to the cost of the assay. Therefore, it is an urgent problem to provide a method for effectively reducing the consumption of carrier gas while ensuring the quality and efficiency of analysis.
In view of this, the present inventors have devised a chromatograph control method and apparatus, which, on one hand, do not use helium in the whole analysis process by dividing the chromatographic analysis process into stages and using different types of carrier gases in different stages, but only use helium in the specific sample analysis stage, so that the amount of helium used in the chromatographic analysis process is reduced and the analysis result is not affected. On the other hand, in the process of using helium, the usage amount of the carrier gas in different subdivision stages is controlled, so that the analysis quality and efficiency are ensured, the usage amount of the helium is further reduced, and the analysis cost of the chromatograph is greatly reduced.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "top", "bottom", "inside", "outside", and the like refer to orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships conventionally used to place products of the present invention, and are used for convenience in describing the present invention and simplifying the description, but do not refer to or imply that the devices or elements referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Examples
Referring to fig. 1, an application scenario of a chromatograph control method according to the present embodiment is schematically illustrated.
As shown in fig. 1, the chromatograph includes a carrier gas system 100, a separation system 200, a detection and recording system 300, a temperature control system 400, and a sample injection system 500, and the chromatograph control method and apparatus provided by the present invention are applied to the carrier gas system 100, wherein the carrier gas system includes a first gas source containing helium gas and a second gas source containing other types of carrier gases.
The first gas source and the second gas source can be different gas cylinders or different parts of the same gas cylinder, and the gas cylinder is divided into the first gas source and the second gas source through a spacing structure.
On the basis, as shown in fig. 2, the chromatograph control method provided by the present invention includes:
step S101, detecting the state of the chromatograph and judging the working stage of the chromatograph.
And judging whether helium is supplied as carrier gas or not by detecting the working stage of the chromatograph. In the whole analysis process, the influence of the carrier gas on the column effect is mainly reflected in the sample analysis stage, so that the key of judging whether the sample analysis stage is entered or not by detecting the state of the chromatograph is whether helium is supplied or not. Meanwhile, the time that different types of carrier gases enter from carrier gas inlets and fully cover the inside of the equipment is considered, so that the influence of other types of carrier gases on helium is avoided, and a certain time needs to be reserved before and after a sample analysis stage, so that the whole analysis process is divided into a plurality of different working stages and used as a judgment standard for inputting carrier gas types.
In step S102, the supply of carrier gas is controlled based on the determination result.
If the preliminary preparation stage is in the preliminary preparation stage, step S103 is executed, and carrier gas is supplied to the chromatograph through the second gas source;
if the sample is in the sample preparation stage, executing step S104, and supplying carrier gas to the chromatograph through the first gas source, wherein the flow rate of the supplied carrier gas is smaller than the column flow rate of the chromatograph;
if the detection and analysis stage is in progress, step S105 is performed to supply the carrier gas to the chromatograph through the first gas source, and simultaneously supply the split flow or the purge flow to the chromatograph through the second gas source. Wherein the flow rate of the carrier gas supplied to the chromatograph by the first gas source is greater than the split flow rate or the purge flow rate;
if the detection is completed, step S106 is executed to supply the carrier gas to the chromatograph through the second gas source.
For the reasons mentioned above, it is necessary to reserve a certain time before and after the sample analysis phase. Immediately after the start-up of the apparatus, the internal temperature of the apparatus gradually rises toward the target temperature under the control of the temperature control system 400, and at this time, the apparatus is still in the preparation stage, and there is a long time until the sample analysis is started. During this stage, additional carrier gas from the second gas source may be used. With the gradual rise of the temperature inside the device, the internal gas pressure gradually stabilizes and the device is ready to start the analysis. A short period of time before the sample analysis stage requires an early switch from other types of gas to helium.
After helium replaces other gases to be used as carrier gas, a sample to be analyzed enters through the sample injection system 500, and then enters into the chromatographic column through the carrier gas, and in this stage, in order to further reduce the consumption of the carrier gas on the basis of achieving the effect, the flow rate of the carrier gas of the helium can be controlled to be smaller than the column flow rate of the chromatographic column. After the sample to be analyzed enters the chromatographic column under the drive of the carrier gas, the sample analysis stage begins. At this point, to further reduce the use of chromatograph helium, the split flow or purge flow supply is provided by a second gas source containing another type of gas. Meanwhile, in order to prevent other types of gases from entering the chromatographic column, the carrier gas flow of helium needs to be increased to be larger than the shunt flow or the purge flow at this stage, so that the analysis effect of the chromatograph is ensured, and the use of helium is reduced as much as possible.
When different components of the sample to be analyzed flow out of the chromatographic column in a certain sequence, the detection and recording system 300 completes the detection and the generation of the chromatogram, the sample analysis stage is finished, helium is not needed to be used as a carrier gas in the following process, and at the moment, the supply of the carrier gas can be switched from the first gas source to the second gas source again. Therefore, in the analysis process of this time, the usage amount of the helium gas is not increased, and the process is repeated until the next analysis process is started.
In summary, in the chromatograph control method provided in this embodiment, on one hand, the process of the chromatographic analysis is divided into stages, and different types of carrier gases are used in different stages, so that helium is not used in the whole analysis process, and helium is only used in a specific stage of the sample analysis, so that the usage amount of helium in the process of the chromatographic analysis is reduced, and the analysis result is not affected. On the other hand, in the process of using helium, the usage amount of the carrier gas in different subdivision stages is controlled, so that the analysis quality and efficiency are ensured, the usage amount of the helium is further reduced, and the analysis cost of the chromatograph is greatly reduced.
As shown in fig. 3, a chromatograph control method according to another embodiment of the present invention is applied to a carrier gas system 100 of a chromatograph, and includes:
step S201, detecting the temperature and the pressure of the chromatographic column, and judging the working stage of the chromatographic instrument through the parameter value and the curve.
Whether the temperature of the chromatographic column reaches the target temperature, whether the pressure in front of the chromatographic column reaches the working standard requirement and whether the temperature and the pressure are stable are key indexes for judging whether the chromatograph finishes preparation. And effective judgment can be carried out by acquiring parameter values and curves of the two. Meanwhile, with the change of the temperature of the chromatographic column and the pressure before the chromatographic column, other working stages of the chromatograph can be correspondingly judged.
As a preferred implementation of the embodiments of the invention:
when the detected chromatographic column temperature is lower than the target temperature of the chromatograph, judging that the chromatographic column is in the early preparation stage; when the detected temperature of the chromatographic column reaches the target temperature, the continuous stabilization time reaches a set first time threshold value, and when the detected pressure in front of the chromatographic column reaches the set target pressure and the continuous stabilization time reaches the set first time threshold value, the chromatographic column is judged to be in the sample preparation stage; when the sample injection preparation stage is started, the sample injection system 500 of the chromatograph is detected to start sample injection and a set second time threshold value is passed, and the detection and analysis stage is judged to be in; and when detecting that the temperature of the chromatographic column is reduced and is less than the target temperature of the chromatograph and a third time threshold set by the duration, judging that the chromatographic column is in the detection completion stage.
The first time threshold is mainly used for distinguishing an early preparation stage and a sample preparation stage, the gas used as the carrier gas in the two stages comes from different gas sources, generally, the longer the first time threshold is set, the more stable and accurate the analysis result is, but the longer the analysis flow at each time is, and the earlier the sample preparation stage is entered, the more the usage amount of helium as the carrier gas is increased. The second time threshold is set by mainly controlling the flow rate of the carrier gas when helium is used as the carrier gas, and the set value of the second time threshold is related to the time of the carrier gas carrying the sample to be analyzed to enter the chromatographic column, so that enough time is provided for ensuring that the sample to be analyzed carried by the carrier gas enters the chromatographic column, and the time is reduced as much as possible. The third time threshold is set to be mainly used for judging whether the process of analyzing the area sample is finished or not, if so, the carrier gas is switched from the helium gas to other types of gases, so that the analysis result is not influenced, and the use of the helium gas is reduced. Through the three numerical values reasonably set, the helium usage amount of the equipment can be reduced to an ideal state, and meanwhile, the analysis quality and the efficiency of the equipment are not influenced.
In step S202, the supply of the carrier gas is controlled based on the determination result.
The specific control method has already been described in detail in the previous embodiment, and is not described herein again.
And step S203, recording the actual gas consumption and the gas consumption curve of the first gas source in the whole analysis control process.
After one-time chromatographic analysis is completed, the usage amount of helium in the whole analysis control process and a gas consumption curve corresponding to the usage amount of helium in each working stage are recorded, so that the space for optimizing and adjusting at which stage can be clearly known.
And step S204, comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis, and comparing the gas consumption with the estimated ideal gas consumption.
The gas consumption is compared with the estimated ideal gas consumption according to a time axis, so that the helium gas consumption in which working stage is more can be known. Comparing the gas consumption curve with the chromatogram generated by analysis according to a time axis, on one hand, adjusting various parameters such as dead zone size, peak time and the like according to an analysis result fed back by the chromatogram, and on the other hand, judging whether the adjustment of the previous parameter and the analysis quality are influenced, such as whether the front cannot be generated, the tail cannot be generated, whether the base line is shifted or not and the like.
When the helium gas consumption needs to be reduced by adjusting the judgment mode of the working stage, step S205 is executed to adjust the judgment mode of the working stage of the chromatograph according to the comparison result.
As a preferred implementation of the embodiment of the present invention, the specific way of performing the adjustment is: and respectively increasing or decreasing the sizes of the first time threshold, the second time threshold and the third time threshold according to a preset time interval, and gradually adjusting the setting values of the first time threshold, the second time threshold and the third time threshold under the condition of not influencing the chromatogram effect, so that the gas consumption gradually approaches to the estimated ideal gas consumption.
According to the comparison result, if it is found that the parameters can be adjusted, the first time threshold, the second time threshold and the third time threshold can be adjusted respectively or simultaneously. The specific way of adjustment may be to increase or decrease each time according to a preset time interval. After one adjustment, the equipment adopts the adjusted parameters in the next operation, and then judges whether the previous adjustment is effective according to the operation result. If the chromatogram effect is found to be influenced in the next comparison, the adjustment mode is changed again after rolling back from the value before the last adjustment. After the operation is repeated for a certain number of times, the three values can be set to the optimal values.
When it is necessary to reduce the consumption of helium by adjusting the supply flow rate of helium, step S206 is performed to adjust at least one of the carrier gas flow rate in the sample preparation stage and the carrier gas flow rate in the detection and analysis stage according to the comparison result.
When adjusting the carrier gas flow rate in the sample preparation stage, two factors need to be considered, on one hand, it is to be ensured that the carrier gas carries the sample to be analyzed into the chromatographic column within a certain time to avoid influencing the analysis effect, and on the other hand, if the carrier gas carries the sample to be analyzed into the chromatographic column for a longer time, the usage amount of helium as the carrier gas will also increase, so that an optimal value needs to be determined from two variables of the carrier gas flow rate and the usage time, which needs to be adjusted repeatedly for many times and then determined according to the comparison result.
When adjusting the carrier gas flow rate in the detection and analysis stage, two factors need to be considered, on one hand, to ensure sufficient carrier gas flow rate, prevent the shunt flow rate or purge flow rate from entering the chromatographic column, and avoid affecting the analysis effect, and on the other hand, to reduce the usage amount of helium of the carrier gas as much as possible, so that an optimal value also needs to be determined, which also needs to be adjusted repeatedly for many times and then determined according to the comparison result.
The specific adjustment manner for each time may be adjusted according to a preset flow interval, and each time the flow interval is increased or decreased. Or an adaptive feedback model associated with several parameters is established, and the optimal value matched with the corresponding use environment is obtained through dynamic solution of the model.
And helium consumption of the equipment in the sample preparation stage and the detection and analysis stage is reduced to a minimum value by respectively adjusting the carrier gas flow in the sample preparation stage and the carrier gas flow in the detection and analysis stage to optimal values.
As a preferred implementation manner of the embodiment of the present invention, step S205 and step S206 may be executed simultaneously, or one of them may be selected and executed according to the situation.
In summary, in the chromatograph control method provided in this embodiment, on one hand, the process of the chromatographic analysis is divided into stages, and different types of carrier gases are used in different stages, so that helium is not used in the whole analysis process, and helium is only used in a specific stage of the sample analysis, so that the usage amount of helium in the process of the chromatographic analysis is reduced, and the analysis result is not affected. On the other hand, in the process of using helium, the usage amount of the carrier gas in different subdivision stages is controlled, so that the analysis quality and efficiency are ensured, the usage amount of the helium is further reduced, and the analysis cost of the chromatograph is greatly reduced.
As shown in fig. 4, the present invention provides a control device for a chromatograph, which is applied to a carrier gas system 100 of the chromatograph, wherein the carrier gas system 100 comprises a first gas source containing helium and a second gas source containing other types of carrier gases, and the device comprises:
a working stage determining unit 110, configured to detect a state of the chromatograph and determine a working stage of the chromatograph;
and a carrier gas control unit 120 for controlling supply of the carrier gas according to the determination result, wherein:
if the device is in the early preparation stage, supplying carrier gas to the chromatograph through a second gas source;
if the sample injection preparation stage is in, supplying carrier gas to the chromatograph through a first gas source, wherein the flow rate of the supplied carrier gas is less than the column flow rate of the chromatograph;
if the detection and analysis stage is in, carrier gas is supplied to the chromatograph through a first gas source, and meanwhile, a split flow or a purge flow is supplied to the chromatograph through a second gas source, wherein the carrier gas flow supplied to the chromatograph through the first gas source is larger than the split flow or the purge flow;
if the detection is completed, the carrier gas is supplied to the chromatograph through the second gas source.
As shown in fig. 5, as an example preferred embodiment of the chromatograph control apparatus according to the present invention:
the carrier gas control unit 120 is specifically configured to:
detect chromatographic column temperature, pressure before the post, judge the working phase that the chromatograph is located through parameter value and curve, wherein:
when the detected chromatographic column temperature is lower than the target temperature of the chromatograph, judging that the chromatographic column is in the early preparation stage;
when the detected temperature of the chromatographic column reaches the target temperature, the continuous stabilization time reaches a set first time threshold value, and when the detected pressure in front of the chromatographic column reaches the set target pressure and the continuous stabilization time reaches the set first time threshold value, the chromatographic column is judged to be in the sample preparation stage;
when the sample injection preparation stage is started, the sample injection system 500 of the chromatograph is detected to start sample injection and a set second time threshold value is passed, and the detection and analysis stage is judged to be in;
and when detecting that the temperature of the chromatographic column is reduced and is less than the target temperature of the chromatograph and a third time threshold set by the duration, judging that the chromatographic column is in the detection completion stage.
Optionally, the apparatus further comprises:
the consumption recording unit 130 is used for recording the actual gas consumption and the gas consumption curve of the first gas source in the whole analysis control process;
the first feedback unit 140 is configured to compare the recorded gas consumption curve with the chromatogram generated by the analysis according to a time axis, and compare the gas consumption with the estimated ideal gas consumption; and adjusting the judgment mode of the working stage of the chromatograph according to the comparison result.
Optionally, the first feedback unit 140 adjusts a determination manner of the working stage of the chromatograph according to the comparison result, and the specific manner is as follows:
and respectively increasing or decreasing the sizes of the first time threshold, the second time threshold and the third time threshold according to a preset time interval, and gradually adjusting the setting values of the first time threshold, the second time threshold and the third time threshold under the condition of not influencing the chromatogram effect, so that the gas consumption gradually approaches to the estimated ideal gas consumption.
Optionally, the apparatus further comprises:
the consumption recording unit 130 is used for recording the actual gas consumption and the gas consumption curve of the first gas source in the whole analysis control process;
the second feedback unit 150 is configured to compare the recorded gas consumption curve with the chromatogram generated by the analysis according to a time axis, and compare the gas consumption with the estimated ideal gas consumption; and adjusting at least one of the carrier gas flow of the sample preparation stage and the carrier gas flow of the detection and analysis stage according to the comparison result.
The chromatograph control device provided in the embodiment of the present invention is used to implement the chromatograph control method, and therefore, the specific implementation is the same as the method described above, and is not described herein again.
In summary, the present invention provides a method and an apparatus for controlling a chromatograph, which, on one hand, by dividing the process of the chromatographic analysis into stages and using different types of carrier gases at different stages, helium is not used in the whole analysis process, and helium is only used at the stage of performing specific sample analysis, so that the usage amount of helium in the process of the chromatographic analysis is reduced, and the analysis result is not affected. On the other hand, in the process of using helium, the usage amount of the carrier gas in different subdivision stages is controlled, so that the analysis quality and efficiency are ensured, the usage amount of the helium is further reduced, and the analysis cost of the chromatograph is greatly reduced.
In the embodiments disclosed in the present application, it should be understood that the disclosed apparatus and method may be implemented in other ways. The apparatus embodiments described above are merely illustrative, and for example, the flowchart and block diagrams in the figures illustrate the architecture, functionality, and operation of possible implementations of apparatus, methods and computer program products according to various embodiments of the present application. In this regard, each block in the flowchart or block diagrams may represent a module, segment, or portion of code, which comprises one or more executable instructions for implementing the specified logical function(s). It should also be noted that, in some alternative implementations, the functions noted in the block may occur out of the order noted in the figures. For example, two blocks shown in succession may, in fact, be executed substantially concurrently, or the blocks may sometimes be executed in the reverse order, depending upon the functionality involved. It will also be noted that each block of the block diagrams and/or flowchart illustration, and combinations of blocks in the block diagrams and/or flowchart illustration, can be implemented by special purpose hardware-based systems which perform the specified functions or acts, or combinations of special purpose hardware and computer instructions.
In addition, functional modules in the embodiments of the present application may be integrated together to form an independent part, or each module may exist separately, or two or more modules may be integrated to form an independent part.
The functions, if implemented in the form of software functional modules and sold or used as a stand-alone product, may be stored in a computer readable storage medium. Based on such understanding, the technical solution of the present application or portions thereof that substantially contribute to the prior art may be embodied in the form of a software product stored in a storage medium and including instructions for causing a computer device (which may be a personal computer, a server, or a network device) to execute all or part of the steps of the method according to the embodiments of the present application. And the aforementioned storage medium includes: a U-disk, a removable hard disk, a Read-Only Memory (ROM), a Random Access Memory (RAM), a magnetic disk or an optical disk, and other various media capable of storing program codes.
Claims (6)
1. A chromatograph control method applied to a carrier gas system of a chromatograph, wherein the carrier gas system comprises a first gas source filled with helium and a second gas source filled with other types of carrier gases, and the method comprises the following steps:
detecting the state of the chromatograph, and judging the working stage of the chromatograph;
and performing supply control of the carrier gas according to the judgment result, wherein:
if the device is in the early preparation stage, supplying carrier gas to the chromatograph through a second gas source;
if the sample injection preparation stage is in, supplying carrier gas to the chromatograph through a first gas source, wherein the flow rate of the supplied carrier gas is less than the column flow rate of the chromatograph;
if the detection and analysis stage is in, carrier gas is supplied to the chromatograph through a first gas source, and meanwhile, a split flow or a purge flow is supplied to the chromatograph through a second gas source, wherein the carrier gas flow supplied to the chromatograph through the first gas source is larger than the split flow or the purge flow;
if the detection is finished, supplying carrier gas to the chromatograph through a second gas source;
the method further comprises the following steps:
recording the actual gas consumption and the gas consumption curve of a first gas source in the whole analysis control process;
comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis, and comparing the gas consumption with the estimated ideal gas consumption;
according to the comparison result, at least one of the carrier gas flow of the sample preparation stage and the carrier gas flow of the detection and analysis stage is adjusted;
and adjusting the judgment mode of the working stage of the chromatograph according to the comparison result.
2. The method of controlling a chromatograph according to claim 1, wherein the detecting the state of the chromatograph and determining the operating stage of the chromatograph are performed by:
detect chromatographic column temperature, pressure before the post, judge the working phase that the chromatograph is located through parameter value and curve, wherein:
when the detected chromatographic column temperature is lower than the target temperature of the chromatograph, judging that the chromatographic column is in the early preparation stage;
when the detected temperature of the chromatographic column reaches the target temperature, the continuous stabilization time reaches a set first time threshold value, and when the detected pressure in front of the chromatographic column reaches the set target pressure and the continuous stabilization time reaches the set first time threshold value, the chromatographic column is judged to be in the sample preparation stage;
when the sample injection preparation stage is started, the sample injection system of the chromatograph is detected to start sample injection and a set second time threshold value is passed, and the detection and analysis stage is judged to be in;
and when detecting that the temperature of the chromatographic column is reduced and is less than the target temperature of the chromatograph and a third time threshold set by the duration, judging that the chromatographic column is in the detection completion stage.
3. The method of controlling a chromatograph according to claim 2, wherein the manner of determining the adjustment of the operating stage of the chromatograph is specifically:
and respectively increasing or decreasing the sizes of the first time threshold, the second time threshold and the third time threshold according to a preset time interval, and gradually adjusting the setting values of the first time threshold, the second time threshold and the third time threshold under the condition of not influencing the chromatogram effect, so that the gas consumption gradually approaches to the estimated ideal gas consumption.
4. A chromatograph control apparatus for use in a carrier gas system of a chromatograph, the carrier gas system including a first gas source containing helium and a second gas source containing another type of carrier gas, the apparatus comprising:
the working stage judging unit is used for detecting the state of the chromatograph and judging the working stage of the chromatograph;
and a carrier gas control unit for controlling supply of the carrier gas according to the judgment result, wherein:
if the device is in the early preparation stage, supplying carrier gas to the chromatograph through a second gas source;
if the sample injection preparation stage is in, supplying carrier gas to the chromatograph through a first gas source, wherein the flow rate of the supplied carrier gas is less than the column flow rate of the chromatograph;
if the detection and analysis stage is in, carrier gas is supplied to the chromatograph through a first gas source, and meanwhile, a split flow or a purge flow is supplied to the chromatograph through a second gas source, wherein the carrier gas flow supplied to the chromatograph through the first gas source is larger than the split flow or the purge flow;
if the detection is finished, supplying carrier gas to the chromatograph through a second gas source;
the device further comprises:
the consumption recording unit is used for recording the actual gas consumption and the gas consumption curve of the first gas source in the whole analysis control process;
the first feedback unit is used for comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis and comparing the gas consumption with the estimated ideal gas consumption; adjusting the judging mode of the working stage of the chromatograph according to the comparison result;
the second feedback unit is used for comparing the recorded gas consumption curve with the chromatogram generated by analysis according to a time axis and comparing the gas consumption with the estimated ideal gas consumption; and adjusting at least one of the carrier gas flow of the sample preparation stage and the carrier gas flow of the detection and analysis stage according to the comparison result.
5. The control device of a chromatography apparatus according to claim 4, wherein the working phase determining unit is specifically configured to:
detect chromatographic column temperature, pressure before the post, judge the working phase that the chromatograph is located through parameter value and curve, wherein:
when the detected chromatographic column temperature is lower than the target temperature of the chromatograph, judging that the chromatographic column is in the early preparation stage;
when the detected temperature of the chromatographic column reaches the target temperature, the continuous stabilization time reaches a set first time threshold value, and when the detected pressure in front of the chromatographic column reaches the set target pressure and the continuous stabilization time reaches the set first time threshold value, the chromatographic column is judged to be in the sample preparation stage;
when the sample injection preparation stage is started, the sample injection system of the chromatograph is detected to start sample injection and a set second time threshold value is passed, and the detection and analysis stage is judged to be in;
and when detecting that the temperature of the chromatographic column is reduced and is less than the target temperature of the chromatograph and a third time threshold set by the duration, judging that the chromatographic column is in the detection completion stage.
6. The control device of the chromatographic instrument according to claim 5, wherein the first feedback unit adjusts the determination mode of the operating stage of the chromatograph according to the comparison result, specifically:
and respectively increasing or decreasing the sizes of the first time threshold, the second time threshold and the third time threshold according to a preset time interval, and gradually adjusting the setting values of the first time threshold, the second time threshold and the third time threshold under the condition of not influencing the chromatogram effect, so that the gas consumption gradually approaches to the estimated ideal gas consumption.
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Denomination of invention: Chromatograph control method and device Effective date of registration: 20220818 Granted publication date: 20220415 Pledgee: Xiamen International Bank Co.,Ltd. Beijing Branch Pledgor: China spectrum Tech (Beijing) Technology Co.,Ltd. Registration number: Y2022990000537 |