Setting method using response function for gas analysis device

Abstract

The invention relates to a setting method (100) for a gas analysis device (10), in which method at least a first response factor (28) for a first substance sample component (21) is determined by means of a calibration gas mixture (15). On this basis, a first response function (31) is determined. Furthermore, a device parameter data set (25) having at least one device parameter (26) is detected and linked to a first response function (31). On the basis of the first response function (31), a second response function (32) for the second substance sample component (22) is determined by means of the transformation function (30). The first response function and the second response function (31, 32) are defined as a measured operating parameter (45). The transformation function (30) can be set using the device parameter data set (25). The invention further relates to a correspondingly designed computer program product (65) and to an evaluation unit (60). The invention also relates to a gas analysis device (10) and a system (50) having such an evaluation unit (60), belonging to such a gas analysis device (10).

Description

Technical Field

[0001] This invention relates to a method for setting up a gas analysis apparatus and a computer program product designed thereto. Similarly, this invention relates to an evaluation unit implemented in accordance with such a method. Furthermore, this invention relates to a gas analysis apparatus equipped with such an evaluation unit, and also to a system for detecting the composition of a substance sample using a higher-level control unit, wherein the control unit is configured to at least partially execute the setup method upon which it is based. Background Technology

[0002] A method for calibrating gas chromatography is known from European Patent EP 3 276 342 B1, in which a calibration mixture containing components of known concentrations is used. A relative response factor, abbreviated RRF, is determined and compared with a universal relative response factor, abbreviated uRRF. Here, the universal relative response factor remains unchanged.

[0003] Patent application WO 2021 / 081553 A1 discloses a method for calibrating a gas sensor, in which environmental conditions within the range of the gas sensor are determined. Furthermore, an initial calibration factor is determined, which describes the sensitivity of the gas sensor to the electrolyte to be measured.

[0004] Gas analyzers are used in many applications in the chemical industry, raw material extraction, and research. To achieve high measurement accuracy, specifying a precise response factor is essential. There is also a need to accelerate and simplify the calibration of gas analyzers. Therefore, there is a demand for improved setup methods that address one of these considerations. Summary of the Invention

[0005] This objective is achieved by a setup method according to the invention, applicable to calibrating a gas analysis device, correcting its settings, and / or making it effective. The setup method is performed on a gas analysis device including a detector, implemented to provide a measurement signal, which is a scale for detecting a component of a substance sample. Here, the substance sample component is a substance sample provided as a calibration gas mixture or a running substance sample. The gas analysis device can be set via multiple device parameters and operated using the corresponding current settings. The measurement characteristics of the detector can be specified first through the device parameters. The setup method includes a first step in which the gas analysis device is provided and a first response factor for a first substance sample component is determined. For this purpose, a calibration gas mixture is used and provided to the gas analysis device. The first response factor can, for example, be a correlation between the area under the curve of the measurement signal at the detector and the concentration of the first substance sample component in a chromatogram. The curve of the measurement signal is generated in response to the detection of the first substance sample component. Furthermore, in the first step, a first response function is determined based on the first response factor. The first response factor represents a point on the graph of the first response function. For example, the first response function can be a straight line passing through the zero point of the coordinate system, which can already be fully described using the first response factor as a point on the straight line. Alternatively or supplementarily, the first step can also be performed multiple times. Here, different calibration gas mixtures with different concentrations of the first substance sample components are used, and the value for the first response factor is determined separately. These are combined in the first step to determine the first response function.

[0006] Furthermore, the setup method according to the invention includes a second step in which a device parameter dataset is detected. Therefore, the device parameter dataset includes multiple device parameters that specify the operation of the gas analysis device, particularly during the first step. Thus, the device parameter dataset includes at least one current device parameter. The device parameter dataset is linked to a first response function determined in the first step.

[0007] Similarly, the third step belongs to the required setup method, in which a second response function for the second substance sample component is determined. The second response function correspondingly and consistently defines the correlation of how the detector responds to the second substance sample component. The second response function is determined based on the first response function and the transformation function. The transformation function at least partially reflects the correlation between the first and second response functions. According to the invention, the transformation function can be set according to a device parameter dataset. The device function can, for example, be constructed as a polynomial having coefficients specified by the device parameters in the device parameter dataset.

[0008] Furthermore, the setup method according to the invention includes a fourth step, in which at least a second response function is specified as a measurement operating parameter for the gas analysis apparatus. Alternatively, both a first and a second response function can be specified as measurement operating parameters for the gas analysis apparatus in the fourth step. The measurement operating parameters define how to evaluate the detector's measurement signal, i.e., what concentration of the substance sample component in the supplied working substance sample corresponds to in which measurement signal.

[0009] The setup method according to the invention allows for the calibration of a gas analyzer based on a reduced balance between the calibration gas mixture and the detector's measurement signals. Therefore, the gas analyzer utilizes a simpler calibration gas mixture, which has a reduced number of substance sample components. Accordingly, a calibration gas mixture, which is particularly stable in its composition, can be used and thus can be stored for a longer period. Furthermore, additional calibration processes for other substance sample components are saved. Such calibration processes often require user intervention, which on the other hand leads to an increased probability of failure. The setup method according to the invention has a higher degree of automation and thus prevents operational errors particularly effectively. The setup of the gas analyzer is simplified, accelerated, and designed more reliably overall through the setup method according to the invention. Furthermore, the method according to the invention can be applied to any number of structurally identical gas analyzers. The setup process, particularly the device-specific matching for the calibration of the gas analyzer, is optional.

[0010] In one embodiment of the claimed setup method, the transformation function is constructed as a multidimensional transformation, the number of its dimensions corresponding to the number of device parameters in the device parameter dataset. Therefore, the device parameters can be specified independently of each other, and a precise transformation can be performed for each conceivable group of device parameters, thereby determining at least a second response function. Thus, the claimed setup method can be incorporated into any setup of a gas analysis apparatus. A decisive calibration setup of the gas analyzer via the corresponding device parameter dataset is optional. This also simplifies and accelerates the setup of the gas analysis apparatus. The transformation function can be parameterized, for example, by coefficients for polynomials and / or matrices. Furthermore, the transformation function comprises a multidimensional sequence, particularly the number of its dimensions corresponding to the number of device parameters in the device data parameter data record. The transformation function can be constructed as at least a two-dimensional function, preferably at least a three-dimensional function, and particularly preferably at least a four-dimensional function. The transformation function can be specified for device parameters that fail empirical testing on structurally identical gas analysis apparatuses. Alternatively or supplementarily, the transformation function can be specified through simulation of the gas analysis apparatus, for example by means of a digital twin or model. The required setup method is based on the understanding that there are tolerance-determined deviations between structurally identical gas analysis devices, namely, the transitivity of the corresponding transformation functions between different samples of the gas analysis device. Similarly, the required setup method is based on the understanding that the operating characteristics of the gas analysis device, especially its detector, can be simulated in a digital twin with such high realism that the results are applicable to setting up an actual gas analysis device.

[0011] Furthermore, in the required setup method, the second response function can be determined at least partially based on a general relative response function, particularly a second general relative response function, starting from the first response function. The second general relative response function represents the relationship between the first and second response functions in a reference state. Here, the second general relative response function can be constructed as a general relative response factor, for example, as described in detail in EP 3 276 342 A1. The disclosure of EP 3 276 342 A1 is incorporated herein by reference. Alternatively, the second general relative response function can also be constructed as a correspondingly consistent function, for example, when the first response function and / or the second response function are functions of quadratic or higher order. In the reference state, there exists a first reference response function for the first material sample component, which is associated with a second reference response function for the second material sample component via the first general relative response function. According to the transformation function, the first reference response function can be uniformly converted to the first response function depending on the current device parameter dataset. Similarly, reference response functions such as the second reference response function and the third reference response function can also be uniformly converted to their respective second response functions, third response functions, etc., depending on the current device parameter dataset. Therefore, the required setup method allows for the use of known universal relative response factors or functions, depending on the current set of device parameters. Consequently, the quality of the gas analysis setup is highly data-driven, less prone to failure, and less dependent on the experience of its users. It reduces the use of cost-intensive reference materials that can only be provided by limited sources, such as authorized testing institutions. Similarly, in contrast to existing solutions, it reduces the need for complex global logistics and trained personnel for the proper handling of reference materials.

[0012] In another embodiment of the claimed setup method, the calibration gas mixture used in the first step is implemented without a second substance sample component. Therefore, a second response function is determined for the second substance sample component without physically presenting it in the setup method. The second substance sample component can be a toxic, harmful to health, flammable, or explosive gas. Alternatively, the second substance sample component is a gas, the long-term stable maintenance of which in the calibration gas cylinder is costly. In particular, the second substance sample component can chemically react with the first substance sample component, thus spontaneously converting itself into another substance. Therefore, the claimed setup method allows specifying a response function as a measurement operating parameter for the substance sample component, which actually requires increased costs or care, without actually requiring such costly handling from the user. Therefore, the second substance sample component can be selected regardless of its hazard and / or compatibility with the first substance sample component. Overall, the claimed setup method is for setup related to calibration gas mixtures in gas analysis devices. Accordingly, the claimed setup method allows the use of calibration cylinders with non-hazardous and stable calibration gas mixtures without affecting the versatility of the gas analysis device's functionality. In particular, calibrated gas mixtures that are subject to seasonal conditions and have very low content due to their dew point or require expensive temperature control during transport are dispensable for the required setup method.

[0013] Furthermore, the first and / or second response functions can be constructed as linear functions, zero-point lines, quadratic functions, and / or cubic functions. Alternatively, the first and / or second response functions can also be functions, particularly polynomial functions, of the fourth or higher order. Alternatively or supplementarily, the first and / or second response functions can also be constructed as piecewise composite functions. Such response functions are described by different functions depending on their concentration, which are interconnected according to their accuracy range. The required setup method allows for the establishment of coupling or transformation functions between the response functions of the load. Further transformation calculations of polynomial functions at higher dimensions can be performed algebraically and can also be achieved with reduced computational power. Therefore, the required setup method can also be implemented on existing gas analysis devices using simple hardware, for example, within the scope of software upgrades.

[0014] Furthermore, in the third step of the required setup method, a third response function for the third substance sample component can also be determined, and specified as a measurement operating parameter in the fourth step. Here, the third response function can be determined by combining the first response function with a transformation function. In particular, a general relative response function can be used, which describes the relationship between the first and third response functions in the reference state. Therefore, the response function between the current state and the reference state specified by the device parameters can be transferred by means of the transformation function. Therefore, the required setup method can be easily transferred to multiple substance sample components. Here, the calibration gas mixture can be without the third substance component. After performing the required setup method, the concentration of the third substance sample component in the operating sample is also determined for the gas analysis device on which it is based. Thus, the functional range of the gas analysis device can also be extended to multiple different operating substance samples based on data. Therefore, the required setup method is scalable and allows for the full utilization of the technical potential of existing gas analysis devices in a simple manner.

[0015] Specifically, in the fourth step, the number of response functions specified as measurement operating parameters exceeds the number of components in the calibration gas mixture. Therefore, the calibration gas mixture can be a simple mixture of non-toxic, chemically stable, and non-volatile substances, exhibiting only reduced isolation tendency and / or a stable temperature characteristic curve. Accordingly, the calibration gas mixture used in the required setup method can be manufactured cost-effectively and simply. The required setup method is suitable for gas analyzers also configured for measurement operations with complex operating substance samples. In particular, the required setup method resolves the previous relationship that the more complex the setup of the gas analyzer, the more complex the operating substance sample to be measured. Since the required setup method is essentially data-driven, the handling of hazardous materials is reduced. In particular, the number of response functions specified in the fourth step of the required setup method can be at least ten, preferably at least 14, and particularly preferably at least 17. Therefore, the required setup method is suitable for replacing the calibration process, which utilizes multiple calibration gas mixtures in known solutions. Simultaneously, the possibility of malfunction is reduced when setting up the gas analyzer.

[0016] In another embodiment of the required setup method, the device parameters can include dosage specification, sample temperature, sample pressure, ambient pressure, detector voltage, dosage specification, gain factor, detector response function, physical properties of at least one sample component, chemical properties of at least one sample component, thermal conductivity of at least one sample component, its ionization cross section, and / or structural information related to the gas analyzer. Each of these device parameters affects the expected response function and the expected measurement signal, such as a chromatogram. In particular, the quantity of material to be determined can change due to variations in sample pressure and / or ambient pressure. Furthermore, the dosage specification determines the absolute quantity of the sample and sample components reaching the detector. Increasing the dosage can yield a so-called peak width in the chromatogram. For example, increasing the detector voltage can be used to improve sensitivity so that weak measurement signals can be determined as quantitatively as possible. Here, the signal response can change from linear to nonlinear characteristics with variations in gain factor and signal level. The device parameters can be set continuously or in stages. The device parameters can be used as input values ​​for the operation of a digital twin of the gas analyzer. The transformation function can be at least partially determined by simulation of the operating characteristics of the gas analyzer using a digital twin.

[0017] Furthermore, the required setup method can include a fifth step, in which a measurement operation is performed using a gas analyzer. The measurement operation is based on a response function, which is specified as measurement operating parameters in the fourth step. During the measurement operation, a sample of the substance is supplied to the gas analyzer, and the concentrations of the sample components contained therein are determined. In the fifth step, the measurement data are accordingly determined and stored, i.e., at least temporarily.

[0018] Furthermore, a sixth step, belonging to the implementation of the setup method, is included, in which the measurement data from the fifth step is used as input for a machine learning algorithm. The measurement data determined in the fifth step is fed to the machine learning algorithm, and it runs accordingly. The machine learning algorithm is designed to improve the transformation function, for example, by determining the coefficients for changes in a multidimensional sequence belonging to the transformation function. The machine learning algorithm can be constructed, for example, as artificial intelligence, particularly neural networks or generative artificial intelligence. The measurement data can, for example, form training data records, through which the machine learning algorithm is further trained. Furthermore, the machine learning algorithm is executed on a higher-level control unit, which is coupled to the gas analysis device via a communication data connection. In the sixth step, a modified transformation function is determined according to the machine learning algorithm. The modified transformation function can provide a basis for re-executing the required setup method. Re-executing is a confirmation and / or adjustment of the setup of the gas analysis device. Alternatively or supplementarily, the re-executing of the required setup method can also be implemented on other gas analysis devices. The modified transformation function can, for example, be transmitted to other gas analysis devices via the higher-level control unit. Here, the two gas analysis devices can be implemented with identical structures. Machine learning algorithms are particularly effective at automatically refining, or improving, parameter sets through machine learning. Therefore, the required setup method is suitable for evaluating measurement data from multiple gas analyzers and improving the underlying transformation function. Consequently, the measurement accuracy of multiple gas analyzers can be rapidly and automatically improved during ongoing measurement operations.

[0019] Furthermore, the required setup method can include a seventh step, in which a comparison value for at least one response factor for the second substance sample component is determined, and a comparison response function is determined based on the comparison value. This is substantially similar to the first step, where at least one corresponding factor for the second substance sample component is determined using a calibration sample containing a known concentration of the second substance sample component and stored at least temporarily as a comparison value. The comparison response function is then determined based on this comparison value or multiple comparison values. For example, when the response function for the second substance sample is a zero-point linearity, a single comparison value is sufficient to determine the comparison response function.

[0020] The required setup method also includes an eighth step, in which the deviation between the comparison response function and the second response function is determined. When both are linear at zero points, this deviation can, for example, be the difference between the increase factors of the second response function and the comparison response function. Similarly, the deviation can be the difference between the coefficients of any polynomial function, depending on the degree of the second and comparison response functions. When the amount of deviation exceeds a boundary value, the deviation continues to be compared with the boundary value and a warning is issued. The boundary value can be a set of boundary values ​​for the coefficients of the polynomial function, similar to the deviation. The seventh and eighth steps essentially serve as verification samples to confirm whether the response function specified in the fourth step is genuine and reliable. Therefore, the required setup method is suitable for self-monitoring. Alarms triggered when the amount exceeds the boundary value can be sent to the user and / or the data interface. In particular, the warning can be sent to the upper-level control unit via the data interface. The upper-level control unit can be configured to interrupt the operation of the gas analyzer and / or interfere with the connected equipment process in the presence of a warning. Therefore, the required setup method improves the achievable process safety of the equipment process in which the appropriately configured gas analyzer is connected. Similarly, bias identification can be used to identify unintentional user intervention in control and / or to identify tampering or tampering attempts on the gas analyzer. Therefore, the required setup method provides an enhanced level of security, both in a safety and assurance sense.

[0021] Furthermore, in the required setup method, at least one of steps three through eight is performed on a higher-level control unit connected to the gas analyzer via a communication data connection. The higher-level control unit can be a control computer, operator station, and / or computer cloud, on which the required setup method is at least partially executed. Computationally intensive steps, such as further training of machine learning algorithms and / or determination of modified transformation functions, can be designed on hardware platforms with appropriate power capabilities. The required setup method is functionally separable, thus also implementable on existing gas analyzers, providing only reduced computational power. The additional measurement accuracy and versatility achievable using the setup method can be implemented on multiple existing gas analyzers. This extends the technically reasonable lifespan of the gas analyzer and thus improves its durability. Similarly, the functional separability of the required setup method allows for the centralized control operation of multiple gas analyzers. Furthermore, the modified transformation function is thus adopted more quickly on each gas analyzer. For example, the durable operation of multiple gas analyzers can be simplified through centralized upgrades. Furthermore, it can expand the functional environment of the gas analysis device, for example, by coupling the gas analysis device with predicted emission monitoring.

[0022] Similarly, this objective is achieved by a computer program product according to the invention, which is implemented by receiving and processing measured values ​​of a response function. The computer program product is also implemented by determining the response function, for example, based on the received measured values. According to the invention, the computer program product is implemented by performing at least one of the above-described setup methods. Therefore, the features of the setup method are readily transferable to the requested computer program product. The computer program product can be implemented monolithically, i.e., for implementation on a single hardware platform. Alternatively, the computer program product can be implemented modularly, i.e., comprising multiple subroutines implemented on different hardware platforms and operating together via at least one communicative data connection. Furthermore, the computer program product can be partially or completely constructed as software. Similarly, the computer program product is implemented with at least partial fixed wiring, for example, constructed as an integrated circuit, chip, or FPGA (Field-Programmable Gate Array). Furthermore, the computer program product can be constructed as a combination of these. The computer program product can be a storage medium, such as a hard disk, solid-state drive, and / or optical storage medium, on which corresponding code is stored as programming language and / or machine-executable code.

[0023] Similarly, the purpose described at the beginning is achieved by an evaluation unit according to the invention. The evaluation unit is designed to determine the composition of a substance sample, particularly a calibration gas mixture and / or a running substance sample. Here, the substance sample is fed to a gas analysis apparatus. The determination of the composition of the substance sample is based on multiple response functions for the corresponding substance components present in the substance sample. The evaluation unit is also configured to specify the response functions, which are applied in the measurement operation. For this purpose, the evaluation unit is equipped with a computer program product. According to the invention, the computer program product is designed according to one of the embodiments described above. Therefore, the features of the computer program product and the subsequent setup method can be similarly transferred to the required evaluation unit. The evaluation unit is part of the gas analysis apparatus and is coupled at least to its detector via a communication data connection. In particular, the evaluation unit is configured to receive and evaluate the measurement signals of the detector.

[0024] Similarly, the above-mentioned objective is achieved by a gas analysis apparatus according to the invention. The gas analysis apparatus is designed to determine the composition of a substance sample, particularly a gas mixture used for calibration or operation, having multiple substance sample components. The gas analysis apparatus has at least one detector and an evaluation unit connected thereto. The at least one detector can be configured as a thermal conductivity detector, flame ionization detector, nitrogen-phosphorus detector, electron capture detector, measurement spectrum detector, photometer, and / or Raman photometer. The gas analysis apparatus can be operated with configurable parameters. According to the invention, the evaluation unit of the gas analysis apparatus is designed according to one of the above embodiments. The characteristics of the evaluation device, along with the associated computer program product and the thus implemented setup method, can be similarly transmitted to the gas analysis apparatus. The gas analysis apparatus can be configured, for example, as a gas chromatograph or a continuous gas analyzer, also known as a continuous gas analyzer or simply CGA.

[0025] Furthermore, the aforementioned objective is achieved by a system according to the invention for determining the composition of a substance sample, particularly a calibration gas mixture or a running substance sample, comprising multiple substance sample components. This system has a higher-level control unit connected to an evaluation unit via a communication data connection, which is also part of the system according to the invention. The higher-level control unit is arranged to determine at least one second response function based on a first response function. In this regard, the higher-level control unit in the system according to the invention is implemented by performing at least a third step in an execution setup method according to one of the above embodiments. Attached Figure Description

[0026] The present invention will now be described in detail with reference to the various embodiments shown in the accompanying drawings. As long as the drawings are considered complementary, the same reference numerals in different drawings have the same technical meaning. Furthermore, the various features of the embodiments shown in the drawings can also be combined with each other and with the features described above. These are shown here respectively: Figure 1 It is a schematic structure of a gas analysis device on which the required setup method is performed; Figure 2 This is a schematic diagram of a stage of the second embodiment of the required setup method; Figure 3 This is a schematic diagram of the third implementation of the required setup method. Detailed Implementation

[0027] Figure 1The claimed gas analysis apparatus 10 is schematically illustrated, on which a first embodiment of the claimed setup method 100 is performed. The gas analysis apparatus 10 is configured as a gas chromatograph 11 and includes a separation unit 12 capable of separating a delivered calibration gas mixture 15 or a delivered running substance sample 16 into its corresponding substance sample components 21, 22, 23 or calibration gas 18. Therefore, the separation unit includes at least one separation column. The gas analysis apparatus 10 is configured to determine, in a defined measurement operation, the composition 17 of the running substance sample 16, i.e., the concentrations of the first substance sample component, the second substance sample component, and the third substance sample component 21, 22, 23 contained therein. The gas analysis apparatus 10 also includes a detector 20 connected to the separation unit 12. The detector 20 is configured to transmit a measurement signal 29 representing the concentrations, i.e., a measure of the amount of substance, of the detected first substance sample component, second substance sample component, and third substance sample component 21, 22, 23. The measurement signal 29 can be processed by the evaluation unit 60, which is equipped with a subroutine 66 of a corresponding computer program product 65. The gas analysis device 10 can be set via multiple device parameters 26, which are combined to form a device parameter dataset 25. The device parameters 26 can be specified by the user and, in particular, can determine the operating behavior of the detector 20.

[0028] In the first step 110 of the setup method 100, a gas analysis device 10 is provided and a calibration gas mixture 15 is delivered. The calibration gas mixture 15 has a first substance sample component 21 of known concentration and also contains a calibration gas 18. The first substance sample component 21 is separated from the calibration gas 18 by a separation device 12 and reaches a detector 20, which sends a measurement signal 29 to an evaluation unit 60 based on the concentration of the first substance sample component in device parameters 26. At least one first response factor 28 for the first substance sample component 21 is determined based on the measurement signal. The response factor 28 gives a quantitative relationship between the concentration of the first substance sample component 21 in the calibration gas mixture 15 and the measurement signal 29 belonging to the detector 20. The first response factor 28 is a point on the graph of a first response function 31 for the first substance sample component 21. The first response function 31 forms a zero-point line and is therefore fully characterized by the first response factor 28 alone.

[0029] A second step 120 also belongs to the setup method 100, in which the first response function 31 is associated with the device parameter dataset 25. In this second step 120, the current device parameter dataset 25 is detected and stored at least temporarily. The association determines which device parameters 26 exist when the first and second steps 110 and 120 are executed. Based on this, the third step 130 of the required setup method 100 is executed.

[0030] In the third step 130, a second response function 32 for the second substance sample component 22 is determined, and the concentration of the second substance sample component in the running substance sample 16, which is not present in the calibration gas mixture 15, is determined. For this purpose, a reference response function 51 is detected in the third step 130; the reference response function can be stored, for example, in a computer program product 65. The reference response function 51 describes the response function for the first substance sample component 21 in the reference state. Furthermore, a second general relative response function 52 is determined. The second general relative response function 52 is characterized by a first relative function 35. The reference response function 51 and the second general relative response function 52 are two linear functions, specifically a zero-point line, such that the first relative function 35 is an angle difference or a difference in the slope of a straight line. When the second substance sample component arrives at the detector 20 and the reference state is present, the second general relative response function 52 represents the expected response characteristics, i.e., the reaction behavior, of the detector 20 to the second substance sample component 22.

[0031] Furthermore, in the third step 130, a transformation function 40 is applied. This transformation function essentially allows for the conversion from a reference state to the state of the gas analysis apparatus 10, specified by apparatus parameters 26 in the apparatus parameter dataset 25, and / or vice versa. The transformation function 40 allows for multidimensional transformations. Here, the number of dimensions 42 of the transformation parameter 40 corresponds to the number of apparatus parameters 26 in the apparatus parameter dataset 25. The multidimensionality of the transformation function 40 is demonstrated in… Figure 1 The transformation function 40 is represented by a hypercube notation. Furthermore, the transformation function 40 is defined, i.e., set, by the device parameter 26 in the device parameter dataset 25. The transformation function 40 includes a set of coefficients 44 stored in a corresponding multidimensional sequence. Accordingly, a second response function 32 for the second substance sample component 22 is determined based on the first response function 31 and the transformation function 40. Here, when the second substance sample component 22 arrives at the detector 20 in the state specified by the device parameter 26 in the current device parameter dataset 25, the second response function 32 corresponds to the concentration-related behavior, i.e., the reaction behavior, of the detector 20. Thus, the gas analysis device 10 can be calibrated with respect to the second substance sample component 22 without the presence of the second substance sample component 22 in the calibration mixture 15.

[0032] Furthermore, in the third step 130, a third response function 33 for the third substance sample component 23 is determined. This third response function is similar to the second response function 32, based on the reference response function 31 for the first substance sample component 21. A third general relative response function 53 is employed, which is defined by the second relative function 36. The third general relative response function 53 is a quadratic polynomial function, such that the second relative function 36 describes the difference in change relative to the reference response function 51. When the third substance sample component 23 arrives at the detector 20, the third general relative response function 53 describes the expected response characteristics of the detector 20 in the reference state. Similarly, a transformation function 40 is employed to describe the relationship between the reference state on which the third general relative response function 53 is based and the state specified by the device parameters 26 in the current device parameter dataset 25. When the third substance sample component 33 arrives at the detector 20, the third response function 33 determined in the third step 130 based on this describes the expected corresponding behavior of the detector 20 in the gas analysis device 10 due to the current state of the device parameter dataset 25. Accordingly, the gas analyzer 10 can be calibrated in terms of the third substance sample component 23 without having to include the third substance sample component in the calibration gas mixture 15.

[0033] Furthermore, the setup method 100 includes a fourth step 140, in which a first response function, a second response function, and third response functions 31, 32, and 33 are provided as measurement operation parameters 45 and specified to the evaluation unit 60. The measurement operation is set up by specifying the measurement operation parameters 45, in which a sample of the running substance 16 is delivered to the gas analysis device 10, and its composition 17 is determined by the gas analysis device 10. The determined composition 17 can be transmitted via the display unit 62 and / or the data interface 64.

[0034] The second and third steps 120 and 130 of setting method 100 are in Figure 1 In the illustrated embodiment, execution takes place on a higher-level control unit 70, which is connected to the evaluation unit 60 via a communication data connection 48. The higher-level control unit 70 is equipped with a subroutine 66 of a computer program product 65, and the subroutine 66 on the evaluation unit 60 is also part of this computer program product. The subroutine 66 works together via the communication data connection 48 and implements the setup method 100. The gas analysis device 10 and the higher-level control unit 70 constitute a system 50 for determining the composition 17 of the substance samples 15 and 16 delivered to the gas analysis device 10.

[0035] The second embodiment of the required setup method 100 is in Figure 2The diagram schematically illustrates one stage. In the first step 110 of the setup method 100, a gas analysis device 10 (not shown in detail) is provided and a first response factor 28 belonging to a first response function 31 is determined. The first response function 31 is constructed as a zero-point straight line, and therefore can be fully described by the first response factor 28 alone. The first response function 31 enables the gas analysis device 10 to be calibrated with respect to a first substance sample component 21. The first substance sample component 21 is contained in a calibration mixed gas 15 (not shown in detail). Furthermore, in the second step 120, a device parameter dataset 25 having multiple device parameters 26 is detected. The operation of the gas analysis device 10 can be set by the device parameters 26. The device parameters 26 in the device parameter dataset 25 describe which setup state the gas analysis device 10 is in during the setup method 100.

[0036] A reference response function 51 exists for the first substance sample component 21, which calibrates the gas analyzer 10 with respect to the first substance sample component 21 under reference conditions. A reference device parameter dataset 27 exists under the reference conditions, which is understood to represent an ideal state. This is in... Figure 2 The same values ​​are used for device parameter 26. The reference response function 51 is coupled with multiple general relative response functions 52, 53, 54 for the second, third, and fourth sample components 22, 23, 24, etc. For each of the general relative response functions 52, 53, 54, there are relative functions 35, 36, 37 defining the relationship with the reference response function 51. The second general relative response function 52 is a zero-point straight line, like the reference response function 51. The first relative function 35 defines the angular difference between the reference response function 51 and the second general relative response function 52, i.e., their graphs. This similarly applies to the relationship between the reference response function 51 and the third general relative response function 54. The third general relative response function 53 is constructed as a quadratic function, such that the second relative function 36 is a function that can change across the possible concentration spectrum. Accordingly, the second relative function 36 represents the computational correlation between the graphs of the third general relative response function 53 and the reference response function 51. The general relative response functions 52, 53, and 54 for the second, third, and fourth material sample components 32, 33, and 34 can exist as numerical tables.

[0037] The device parameter dataset 25 detected in step 120 is continued to be used to set the transformation function. For this, device parameter dataset 25, i.e., its device parameters 26, is used as input. The transformation function 40 transforms the general relative response functions 52, 53, 54 related to the reference state and the reference device parameter dataset 27 to the current state of the gas analysis device 10 defined by device parameter dataset 25. The transformation function 40 has a dimension 42 corresponding to the number of device parameters 26 in device parameter dataset 25. The multidimensionality of device parameter dataset 25 is... Figure 2 The transformation function 40 is represented by a hypercube notation. A coefficient set 44 belongs to the transformation function 40, which parameterizes the transformation function 40. A second response function 32 for the second substance sample component 22 is determined from the second general relative response function 52 by applying the transformation function 40. The second response function 32 is associated with the state of the gas analysis device 10 by applying the transformation function 40, the state of which is described by device parameters 26 in the device parameter dataset 25. Similarly, third and fourth response functions 33 and 34 are determined accordingly for the third and fourth substance sample components 23 and 24, respectively, based on the third and fourth general relative response functions 53, 54, etc. Here, the calibration gas mixture 15 (not shown in detail) does not contain the second, third, and fourth substance sample components 32, 33, 34. The number of response functions 32, 33, 34 determined in the third step 130 is higher than the number of substance sample components in the calibration gas mixture 15. Therefore, the second, third, and fourth sample components 22, 23, and 24 can be selected independently of the composition of the calibration gas mixture 15. Response functions 32, 33, and 34 are specified as measurement operating parameters 45 for the gas analyzer 10 in a fourth step 140 (not shown in detail).

[0038] The third embodiment of the required setup method 100 performed on the gas analyzer 10 Figure 3 The diagram is schematically shown. The gas analysis apparatus 10 is configured as a gas chromatograph 11 and includes a separation device 12 connected to a detector 20, which is in turn coupled to an evaluation unit 60. The detector 20 is configured to send a measurement signal 29 to the evaluation unit 60, which can be processed by a subroutine 66 stored thereon in a computer program product 65. The setting method 100 is described in detail below. Figure 3 The implementation shown is based on the fact that the first, second, third, and fourth steps 110, 120, 130, and 140 have been effectively performed, for example, like Figure 1 or Figure 2As described. Therefore, there are a first response function, a second response function, and a third response function 31, 32, 33, which are specified in the evaluation unit 60 as the measurement operating parameter 45.

[0039] Step 510 is executed, in which measurement operation 47 is performed, examining multiple running substance samples 16, either consecutively or sequentially, that have varying components 17. Measurement operation 47, in which the components 17 of the running substance samples 16 are examined, is performed substantially periodically. Here, the first response function, second response function, and third response function 31, 32, and 33, designated as measurement operation parameters 45 in step 4140, are used. Measurement data 49, i.e., the corresponding components 17 of the running substance samples 16, for the first, second, and third substance sample components 21, 22, and 23, are at least temporarily stored and transmitted to the machine learning algorithm 68 in step 610. For this purpose, the upper-level control unit 70 is connected to the evaluation unit 60 via communication data link 48. The determined measurement data 49 can be transmitted via the data interface of the display unit 62 and / or the evaluation unit 60. The machine learning algorithm 68 is constructed as a neural network and runs on the upper-level control unit 70. A subroutine of computer program product 65 also runs on the upper-level control unit 70, which implements the setting method 100. Machine learning algorithm 68 is at least functionally coupled to or belongs to computer program product 65. In the sixth step 160, the measurement data 49 generated and stored in the fifth step 150 is used as a training dataset for machine learning algorithm 68. Additionally, measurement data 49 from other gas analysis devices 10 with the same structural design can also be used. Therefore, the training dataset can be derived from the measurement data 49 of step 150 and external measurement data. Machine learning algorithm 68 is implemented to establish a modified transformation function 40 by training with measurement data 49. Specifically, the coefficients 44 belonging to transformation function 40 can be updated. Transformation function 40 has a dimension number 42 corresponding to the number of device parameters 26 in device parameter dataset 25, as exemplarily in... Figure 1 As shown in the diagram. The modified transformation function 40 is sent to the evaluation unit 60 in the sixth step 160. Based on the modified transformation function 40, at least the third and fourth steps 130 and 140 of the setup method 100 can be re-executed, thereby accurately determining the first response function, the second response function, and the third response functions 31, 32, and 33. The transformation function 40 can be automatically improved through the fifth and sixth steps 150 and 160. In particular, when operating multiple gas analysis devices 10, their calibration accuracy can therefore be improved via machine learning.

[0040] Similarly, according to Figure 3In the embodiment, a seventh step 170 is performed, in which a calibration gas mixture 15 is supplied to the gas analysis apparatus 10. The calibration gas mixture 15 used in the seventh step 170 has a second substance sample component 22 of known concentration. In addition to the second substance sample component 22, the calibration gas mixture 15 has another calibration gas 18, which is not part of the substance sample components 21 and 23 to be measured. The seventh step 170 is essentially similar to... Figure 1 The first step 110, as shown, determines a comparison value 56 for the response factor. The comparison value 56 lies on a straight line representing the zero point of the comparison response function 57. The second response function 32 for the second material sample component 22 is similarly constructed as a straight line with zero points. With proper calibration performed in the first to fourth steps 110, 120, 130, 140 of the required setup method 100, a minimum deviation 59 exists between the second response function 32 and the comparison response function 57, preferably zero. The setup method 100 further includes an eighth step 180, in which the minimum deviation 59 between the second response function 32 and the comparison response function 57 is determined. Because the second response function 32 and the comparison response function 57 are constructed as straight lines with zero points, the deviation 59 can represent the angle or slope difference between them. For example, when they are second-order polynomial functions, third-order polynomial functions, or higher-order polynomial functions, the deviation 59 will have a different form in other designed comparison response functions 57 or second response functions 32. Furthermore, the deviation 59 in step 180 is compared with a boundary value not shown in detail. When the amount of deviation 59 exceeds the boundary value, a warning 61 is sent. Warning 61 can be sent via display unit 62 and / or data interface 64. The boundary value can be specified by the user or computer program product 65. Steps 170 and 180 essentially represent experimental verification of the second response function 32 specified in step 140. Therefore, this setup method 100 is suitable for self-monitoring.

[0041] When the calibration gas mixture contains a first and second substance sample component 21, 22 of known concentration, the calibration gas mixture 15 used in steps 170 and 180 can also be the calibration gas mixture 15 from step 110. The calibration gas mixture 15 containing two substance sample components 21, 22 can, in many cases, be manufactured in a simple manner with improved accuracy. Steps 170 and 180 can be additionally performed similarly for a third substance sample component 23, thus providing another feasible option for verification. The more substance sample components 21, 22, 23 of known concentration the calibration gas mixture 15 contains, the more cross-checks of response functions 31, 32, 33 can be performed, which improves reliability. Thus, the complex calibration gas mixture 15 in the claimed setup method ensures improved reliability when calibrating the gas analyzer 10. Simultaneously, the gas analyzer 10 can be calibrated for multiple substance sample components 21, 22, 23 using the claimed setup method 100. The gas analyzer 10 and the upper control unit 70 belong to system 50 for determining the composition of the substance samples 15, 16 delivered to the gas analyzer 10.

Claims

1. A setting method (100) for a gas analysis device (10), which comprises a detector (20) and can be set up and operated by means of a plurality of device parameters (26), comprising the following steps: a) providing the gas analysis device (10) and determining at least a first response factor (28) for a first substance sample component (21) by means of a calibration gas mixture (15) and determining at least a first response function (31) using the first response factor (28); b) detecting a device parameter data set (25) comprising at least one of the current device parameters (26) and linking the device parameter data set (25) to the first response function (31); c) determining a second response function (32) for a second substance sample component (22) by means of a transformation function (30) on the basis of the first response function (31); d) defining at least the second response function (31, 32) as a measurement operating parameter (45) for the gas analysis device (10); wherein the transformation function (30) can be set using the device parameter data set (25).

2. The setting method (100) according to claim 1, characterized in that the transformation function (30) is a multidimensional transformation, the number of dimensions (42) of which corresponds to the number of device parameters (26) in the device parameter data set (25).

3. The setting method (100) according to claim 1 or 2, characterized in that in step c) the second response function (32) is also determined on the basis of a general relative response function (52) with respect to the first response function (31).

4. The setting method (100) according to any one of claims 1 to 3, characterized in that the calibration gas mixture (15) is implemented without the second substance sample component (22).

5. The setting method (100) according to any one of claims 1 to 4, characterized in that the first and / or the second response function (31, 32) is designed as a linear function, a quadratic function, a cubic function and / or a piecewise chain function.

6. The setting method (100) according to any one of claims 1 to 5, characterized in that in step c) a third response function (33) is also determined for a third substance sample component (21, 22, 23) and in step d) the third response function is specified as a measurement operating parameter (45).

7. The setting method (100) according to claim 6, characterized in that the number of response functions (31, 32, 33) specified in step d) exceeds the number of components in the calibration gas mixture (15).

8. The setting method (100) according to any one of claims 1 to 7, characterized in that ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ The device parameters (26) comprise a dose size, a substance sample temperature, a substance sample pressure, an ambient pressure, a detector voltage, a dose size, a gain factor, a detector response function, a physical property of at least one substance sample component, a chemical property of at least one substance sample component, a thermal conductivity of at least one substance sample component, an ionization cross section of the at least one substance sample component and / or a structure-related information of the gas analysis device.

9. The setting method (100) according to one of claims 1 to 8, characterized in that The setting method (100) further comprises the following steps: e) performing a measurement operation (47) with the gas analysis device (10) by means of a determined response function (31, 32, 33) and storing measurement data (49); f) using the measurement data (49) as input for a machine learning algorithm (68) and determining a modified transformation function (30).

10. The setting method (100) according to one of claims 1 to 9, characterized in that The setting method (100) further comprises the following steps: g) determining a comparison value (56) for at least one response factor and determining a comparison response function (57) for the second substance sample component (22); h) determining a deviation (59) between the comparison response function (57) and the second response function (32) and outputting a warning (61) if the amount of the deviation (59) exceeds a boundary value.

11. The setting method (100) according to one of claims 1 to 10, characterized in that At least one of the steps c) to h) is performed on a superordinate control unit (70) which is connected to the gas analysis device (10) by means of a communication data link (48).

12. A computer program product (65) designed for receiving and processing measurement values of a first response factor (28) and for determining response functions (31, 32, 33), characterized in that The computer program product (65) is designed to perform at least one setting method (100) according to one of claims 1 to 11.

13. An evaluation unit (60) for determining a composition (17) of a substance sample (15, 16) by means of a plurality of response functions (31, 32, 33), the composition being delivered to a gas analysis device (10), and the evaluation unit (60) being equipped with a computer program product (65) for specifying the response functions (31, 32, 33), characterized in that The computer program product (65) is designed according to claim 12.

14. A gas analysis device (10) for determining the composition of a substance sample (15, 16) having a plurality of substance sample components (21, 22, 23), the gas analysis device comprising a detector (20) and an evaluation unit (60), wherein The gas analysis device (10) can be set up and operated by means of a plurality of device parameters (26), characterized in that The evaluation unit (60) is designed according to claim 13.

15. A system (50) for determining the composition of a substance sample (15, 16) having a plurality of substance sample components (21, 22, 23), the system comprising a superior control unit (70) connected via a communication data link (48) with an evaluation unit (60), wherein The superordinate control unit (70) is designed for determining at least a second response function (32) with a first response function (31), characterized in that The superordinate control unit (70) is designed for determining at least a second response function (32) with a first response function (31), characterized in that The superordinate control unit (70) is configured to perform at least step c) of the setting method (100) according to any one of claims 1 to 11.

Images