CN113009165B - Method for controlling an analyzer - Google Patents

Method for controlling an analyzer Download PDF

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Publication number
CN113009165B
CN113009165B CN202011422103.9A CN202011422103A CN113009165B CN 113009165 B CN113009165 B CN 113009165B CN 202011422103 A CN202011422103 A CN 202011422103A CN 113009165 B CN113009165 B CN 113009165B
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Prior art keywords
heat output
temperature
reactor chamber
current
memory
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CN113009165A (en
Inventor
乌尔里希·罗滕斯坦纳
伊娃-玛丽亚·佩塔
克里斯蒂安·克莱默
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Endress and Hauser Conducta GmbH and Co KG
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Endress and Hauser Conducta GmbH and Co KG
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    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05DSYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D23/00Control of temperature
    • G05D23/19Control of temperature characterised by the use of electric means
    • G05D23/1919Control of temperature characterised by the use of electric means characterised by the type of controller
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/00584Control arrangements for automatic analysers
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05DSYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D23/00Control of temperature
    • G05D23/19Control of temperature characterised by the use of electric means
    • G05D23/30Automatic controllers with an auxiliary heating device affecting the sensing element, e.g. for anticipating change of temperature
    • G05D23/32Automatic controllers with an auxiliary heating device affecting the sensing element, e.g. for anticipating change of temperature with provision for adjustment of the effect of the auxiliary heating device, e.g. a function of time
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B1/00Details of electric heating devices
    • H05B1/02Automatic switching arrangements specially adapted to apparatus ; Control of heating devices
    • H05B1/0227Applications
    • H05B1/023Industrial applications
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • B01J2219/0006Temperature measurement of the heat exchange medium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00054Controlling or regulating the heat exchange system
    • B01J2219/00056Controlling or regulating the heat exchange system involving measured parameters
    • B01J2219/00058Temperature measurement
    • B01J2219/00063Temperature measurement of the reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00132Controlling the temperature using electric heating or cooling elements
    • B01J2219/00135Electric resistance heaters
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00193Sensing a parameter
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00193Sensing a parameter
    • B01J2219/00195Sensing a parameter of the reaction system
    • B01J2219/002Sensing a parameter of the reaction system inside the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00211Control algorithm comparing a sensed parameter with a pre-set value
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00211Control algorithm comparing a sensed parameter with a pre-set value
    • B01J2219/00213Fixed parameter value
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00211Control algorithm comparing a sensed parameter with a pre-set value
    • B01J2219/0022Control algorithm comparing a sensed parameter with a pre-set value calculating difference
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00222Control algorithm taking actions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00222Control algorithm taking actions
    • B01J2219/00225Control algorithm taking actions stopping the system or generating an alarm
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00222Control algorithm taking actions
    • B01J2219/00227Control algorithm taking actions modifying the operating conditions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00191Control algorithm
    • B01J2219/00222Control algorithm taking actions
    • B01J2219/00227Control algorithm taking actions modifying the operating conditions
    • B01J2219/00229Control algorithm taking actions modifying the operating conditions of the reaction system
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00243Mathematical modelling
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00346Heating or cooling arrangements

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Automation & Control Theory (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

The present application relates to a method for controlling an analyzer. The application relates to a method for controlling an analyzer, comprising at least the following steps: determining a limit heat output by at least the following sub-steps: repeatedly measuring the temperature of the reactor chamber by means of a temperature sensor, storing each measured temperature in a memory, repeatedly heating the reactor chamber by means of a heater with a pre-specified heat output, storing the heat output in question in the memory, determining a limiting heat output based on the highest stored heat output; measuring a current temperature of the reactor chamber; comparing the current temperature with the last stored temperature; saving the current temperature in a memory; heating the reactor chamber with the current heat output by a heater; comparing the current heat output with the limited heat output; saving the current heat output in a memory; if the current heat output is greater than the limit heat output and the current temperature is equal to the last saved temperature, an error message is output.

Description

Method for controlling an analyzer
Technical Field
The invention relates to a method for controlling an analyzer.
Background
In analytical measurement techniques, in particular in the field of water management and environmental analysis, and in industry, for example in food technology, biotechnology and pharmaceutical, and in various laboratory applications, it is very important that the concentration of analytes, such as pH, conductivity or e.g. ions or dissolved gases, in a gaseous or liquid measurement medium is measured. These measured values may be detected and/or monitored, for example, by electrochemical sensors such as potential, current, volt-ampere or charge sensors, or even conductivity sensors. These sensors are typically integrated in the analyzer.
By means of an analyzer, the total parameter, such as Chemical Oxygen Demand (COD), total Phosphorus (TP) or Total Nitrogen (TN), can be determined. For this purpose, the sample to be analyzed must be decomposed in the reactor by using a decomposition reagent and high temperature before measurement. In order to set a certain temperature in the reactor, it is necessary to measure in the reactor. Generally, this is accomplished by using a sensor as close as possible to the liquid to be heated. The reactor is typically made of glass, as glass is not electrically conductive and is highly thermally conductive, very chemically resistant, and most importantly transparent to certain wavelengths of light.
A certain overpressure occurs during the decomposition. This is particularly high in COD measurement, as the sample is decomposed at relatively high temperatures. Due to the complex structure of the reactor and the fact that glass reactors are mainly manufactured by hand, situations arise in which under cyclic loading, fine cracks develop in the glass at high temperatures, leading to leaks in the pouch for the temperature sensor. The aggressive reagent mixture, typically sulfuric acid, can then propagate through the crack and slowly damage the temperature sensor. Furthermore, damage to the temperature sensor may also occur purely due to thermal cycling stresses.
Both cases then appear as arbitrary unreliable temperature values. Because temperature represents the control variable for the reactor heating control as described above, incorrect temperature values result in uncontrolled heating of the reactor. In the best case, i.e. in the event of a broken sensor wire, the sensor indicates a very high temperature and the heating is switched off, which occurs for example via a temperature limiting switch. On the other hand, if a local short circuit occurs, the indicated temperature is too low. The reactor is then heated in an uncontrolled manner and the pressure in the reactor continues to rise until the overpressure means of the reactor reacts or the weakest point of the system yields.
Fuses or bimetallic switches are known in the art to prevent uncontrolled heating of the reactor. These can respond at a pre-specified temperature in the reactor and irreversibly or reversibly set the heating current to 0. However, the components have a certain thermal inertia, which is often too large for the fault to be intercepted, or requires considerable design effort. Furthermore, for example, fuses are produced for single use only, and thus the assembly is no longer functional after triggering.
In previous reactors, the overpressure means were intended to prevent bursting of the weakest point of the glass reactor or system and thus to prevent harm to the operator. However, the overpressure device is usually a disposable device, for example in the form of a so-called burst disk, so that failure of the component occurs due to the above-mentioned malfunction. As a result, the analyzer is disabled for a certain time, which is not acceptable for some users.
Disclosure of Invention
It is therefore an object of the present invention to provide a method for operating an analyzer that prevents the analyzer from being disabled.
This object is achieved by the method according to the invention.
The method according to the invention comprises at least the following steps:
-providing an analyzer having a reactor chamber, a heater adapted to heat the reactor chamber, a temperature sensor adapted to measure the reactor chamber, a control unit connected to the temperature sensor and the heater and having a memory;
-determining a limit heat output by at least the following sub-steps:
repeatedly measuring the temperature of the reactor chamber by means of a temperature sensor,
Saving each measured temperature in a memory,
Repeatedly heating the reactor chamber by means of a heater with a pre-specified heat output,
Saving the heat output in question in a memory,
-Determining a limiting heat output based on the highest saved heat output;
-measuring the current temperature of the reactor chamber;
-comparing the current temperature with the last saved temperature;
-saving the current temperature in a memory;
-heating the reactor chamber by a heater at the current heat output;
-comparing the current heat output with a limit heat output;
-saving the current heat output in a memory;
-outputting an error message if the current heat output is greater than the limit heat output and the current temperature is equal to the last saved temperature.
The method according to the invention may make the reactor of the analyzer non-overheated and the heater may be disconnected before overheating. This prevents the reactor from exploding or the safety valve has to be opened. With the reactor filled, uncontrolled heating is prevented, which leads to escape of highly corrosive or toxic reaction mixtures. Thus, greater safety for the user is ensured. The reliability and service life of the analyzer and the reactor are also significantly increased.
According to one embodiment of the invention, the pre-specified heat output and/or the current heat output is a heat output averaged over a pre-specified time interval.
According to one embodiment of the invention, the pre-specified heat output and/or the current heat output is greater than zero when the measured current temperature is below the target temperature.
According to one embodiment of the invention, the step of determining the limit heat output comprises the sub-step of adding a safe offset.
According to one embodiment of the invention, the step of determining the limited heat output is repeated periodically such that the limited heat output is adjusted periodically.
According to one embodiment of the invention, the step of determining to limit the heat output is repeated until at least 10 heat outputs have been saved. Preferably, the step of determining to limit the heat output is repeated until at least 100 heat outputs have been saved. Preferably, the step of determining to limit the heat output is repeated until at least sufficient heat output has been saved such that all heat output expected during the predetermined period of use has been saved.
According to one embodiment of the invention, the limited heat output corresponds to a maximum heat output of the heater.
According to one embodiment of the invention, in the step of determining the limiting heat output, repeated measurement of the temperature of the reactor chamber and repeated heating of the reactor chamber are repeated within 10 seconds. Preferably, in the step of determining the limiting heat output, the repeated measurement of the temperature of the reactor chamber and the repeated heating of the reactor chamber are repeated within 5 seconds. More preferably, in the step of determining the limit heat output, the repeated measurement of the temperature of the reactor chamber and the repeated heating of the reactor chamber are repeated within 1 second.
According to one embodiment of the invention, limiting the heat output is based on filtering the saved maximum heat output.
According to one embodiment of the invention, the filtering comprises a floating average or median filtering and is based on the last saved at least 3 thermal outputs. The filtering is preferably based on the last saved 5 heat outputs. Particularly preferably, the filtering is based on the last saved 10 heat outputs.
According to one embodiment of the invention, the memory has a ring memory, and the pre-specified heat output and the current heat output are written to the ring memory.
Drawings
The invention will be explained in more detail based on the following description and the accompanying drawings. The following description shows:
fig. 1 is a schematic diagram of an analyzer for use in a method according to the invention.
Detailed Description
Fig. 1 shows an analyzer 1 having a reactor chamber 10, a heater 11, a temperature sensor 12 and a control unit 13 connected to the temperature sensor 12 and the heater 11.
The heater 11 is adapted to heat the reactor 10. The heater 11 is, for example, a heating coil. The heater 11 is arranged around the reactor chamber 10, for example. In an alternative embodiment, the heater 11 is integrated in the wall of the reactor chamber 10. In yet another embodiment, the heater 11 is, for example, a heating resistor attached to the reactor chamber 10. In yet another alternative embodiment, the heater 11 is arranged in the reactor chamber 10.
The temperature sensor 12 is adapted to measure the temperature of the reactor chamber 10. The temperature sensor 12 is arranged, for example, in the reactor chamber 10. In an alternative embodiment, the temperature sensor 12 is arranged in the wall of the reactor chamber 10. In yet another alternative embodiment, the temperature sensor 12 is arranged on the outer wall of the reactor chamber 10.
The temperature sensor 12 is a temperature sensor measuring temperature by the principle of resistance, such as PT100, PT1000, PTC or NTC, or a temperature sensor measuring temperature by the thermoelectric effect, such as a type K, J, N or other type of thermocouple.
The control unit 13 has a memory 14. The memory 14 is, for example, a ring memory. Ring memory is understood to mean that the memory 14 has a limited storage capacity and holds data in such a way that the data held first is erased first when the memory is full. In other words, the ring memory functions according to the first-in first-out principle, also called FIFO principle.
A method for controlling the analyzer 1 according to the present invention will be described below.
First, the analyzer 1 described above is provided. This includes preparing the analyzer 1 for measurement operations. For example, reactor 10 already contains the process medium. Ideally, the process medium has been heated to a desired target temperature by, for example, heater 11. Therefore, the purpose of the control unit 13 is to intelligently control the analyzer 1 such that the temperature of the processing medium is kept constant at the target temperature for a pre-specified time or, if the user intentionally changes the target temperature, at the changed target temperature.
Next, a determination is made to limit the heat output. For this purpose, at least the following sub-steps are carried out:
As a first sub-step, the temperature of the reactor chamber 10 or of the reactor wall or of the process medium is repeatedly measured by the temperature sensor 12, depending on how and where the temperature sensor 12 is installed. For example, the temperature of the reactor chamber 10 is repeatedly measured at predetermined intervals. For example, the temperature measurement is repeated within 10 seconds. The temperature measurement is preferably repeated within 5 minutes. It is particularly preferred to repeat the temperature measurement within 1 second. In an alternative embodiment, the temperature measurement is repeated over different time periods.
Then, a substep of saving the measured temperature in the memory 14 is performed. A temperature profile can thus be established which is then used for error detection. Error detection will be discussed in detail later. Naturally, preserving the temperature means preserving a temperature value corresponding to the measured temperature.
The subsequent substep includes repeatedly heating the reactor chamber 10 by the heater 11 at a pre-specified heat output. Here, for example, as well as in the substep of temperature measurement, a pre-specified heat output is emitted by the heater 11 at pre-specified intervals and stored in the memory 14, for example, the pre-specified intervals being the same as those in the above-described temperature measurement. By preserving the heat output, the characteristics of the heat output can be generated later. Preserving the heat output is of course understood to mean preserving the heat output value corresponding to the emitted heat output.
Alternatively, the heater 11 may continuously emit a predetermined heat output. For example, the pre-specified heat output is obtained as the heat output averaged over a pre-specified time interval. The acquisition of the heat output is based on filtering the heat output within a time window. The filtering is for example an average filtering or a median filtering. For example, the filtering is floating filtering. The average filtering comprises at least 3, preferably 5, particularly preferably 10 of the last saved heat outputs. Alternatively, the filtering is based on an average of all heat output emitted over a time span. The time span for forming the average value is, for example, less than 60 seconds, preferably less than 10 seconds, particularly preferably less than 1 second. In the event of strong fluctuations in the value of the heating, the so-called heating peaks are therefore smoothed by averaging, without triggering an error message.
In a heating mode with a continuously emitted heat output, it is particularly advantageous to store the heat output based on an average value of the heat output, since the heat emitted by the heater 11 can thereby be precisely controlled.
Optionally, a sub-step of comparing the measured temperature with the target temperature is performed. If the measured temperature is below the target temperature, the pre-specified heat output is selected to be greater than zero.
In the next substep, the pre-specified heat output from the heater 11 is stored in the memory 14. This preferably occurs at the same point in time as in the temperature storage sub-step. In other words, the emitted pre-specified heat output and temperature are saved in such a way that the heat output can be precisely assigned to the corresponding measured temperature. Thus, a characteristic of the heat output and a continuous characteristic of the temperature can be established, which is subsequently used for error detection.
Next, the substep of determining a limit heat output is performed based on the highest saved heat output. This is done, for example, by comparing all saved heat outputs and defining the heat output with the highest value as the limit heat output.
Optionally, in the substep, a safe offset is added to the determined limit heat output. Thus, the limiting heat output increases the safe offset. The safe offset is based on empirical values.
Optionally, the step of determining the limit heat output is repeated until at least 10 heat outputs have been saved. This means that at least sufficient heat output has been saved such that all heat output expected during a pre-specified period of use has been saved. The prespecified usage period is understood to be the period of time necessary for performing a process, for example a so-called decomposition of the process medium. Such a period of time may be, for example, only a few minutes or a few hours.
In a next step of the method for controlling the analyzer 1, the current temperature of the reactor chamber 10 is measured.
The current temperature is then compared with the temperature last stored in memory 14. The current temperature is performed at a point in time, for example, after a predetermined time span has elapsed after the last temperature measurement stored in the memory 14.
Next, the current temperature is saved in the memory 14. If the memory 14 is a ring memory and is full, the earliest saved temperature value will be discarded and the current measured temperature saved.
The reactor chamber 10 is then heated by the heater 11 with the current heat output. As mentioned above, the heating with the current heat output may be performed continuously or intermittently, i.e. only for a limited time interval.
In the next step, the current heat output is compared with the limit heat output. It is thus determined whether the current heat output is above or below the limit heat output.
The current heat output is then saved in memory 14. If the current heat output is continuously emitted, the average current heat output may be saved, as described above. If the current heat output is only emitted during a limited time interval, the current heat output averaged over the time interval can also be saved in this case.
In a further step, an error message is output if the current heat output is greater than the limit heat output and the current temperature is equal to the last saved temperature.
In one embodiment, the step of determining the limiting heat output is repeated repeatedly. The limit heat output determined for each pre-specified usage period may be written to the memory, and the maximum value of the determined last X limit heat outputs may be used as the limit value. Therefore, the limit heat output is regularly adjusted by the control unit 13. By periodically repeating the determination of the limit heat output, the method is performed in a self-learning manner, since structural changes, for example due to aging, increased resistance of the heating coil of the heater 11, or environmental influences, such as temperature, can be taken into account in determining the limit heat output.
As described above, it is preferable to use a sufficient number of heat outputs to determine the limit heat output so that temperature fluctuations of the environment of the analyzer 1 will have been fully considered. In determining the limit heat output, therefore, temperature fluctuations of the analyzer 1 between daytime and nighttime operation, or between summer and winter operation, are preferably taken into account.
If the temperature of the reactor chamber 10 does not rise even if the heat output has been increased, there must be a temperature loss, for example due to cracks in the reactor chamber 10, or the temperature sensor 12 itself is defective, so that for example the displayed temperature is too low.
The analyzer 1 may additionally have a temperature sensor for measuring the ambient temperature. In this case, the ambient temperature may be taken into account in the error detection. For example, if the ambient temperature drops abnormally fast, it is expected that there is not necessarily an error if the heat output increases and the temperature of the reactor chamber 10 remains constant for a short period of time. In this case, the control unit 13 may output a warning signal instead of the error message.
If the operator changes the target temperature, the limit heat output must be reset and the memory 14 refilled from the point in time the set value changed and a new limit heat output determined accordingly.
By means of the present invention, an intelligent control method can be provided which prevents uncontrolled heating when filling the reactor chamber 10. Thus, the triggering of potential crack formation or overpressure protection in the reactor chamber 10 is prevented, and escape of the process medium due to a defective reactor chamber 10 is practically impossible.
REFERENCE SIGNS LIST
1 Analyzer
10 Reactor chamber
11 Heater
12 Temperature sensor
13 Control unit
14 Memory

Claims (17)

1. A method for controlling an analyzer (1), comprising at least the steps of:
-providing an analyzer (1), the analyzer (1) having a reactor chamber (10), a heater (11) adapted to heat the reactor chamber (10), a temperature sensor (12) adapted to measure the reactor chamber (10), a control unit (13) connected to the temperature sensor (12) and the heater (11) and having a memory (14);
-determining a limit heat output by at least the following sub-steps:
repeatedly measuring the temperature of the reactor chamber (10) by means of the temperature sensor (12),
Storing each measured temperature in the memory (14),
Repeatedly heating the reactor chamber (10) by means of the heater (11) with a pre-specified heat output,
Saving a specific heat output in said memory (14),
-Determining the limiting heat output based on the highest saved heat output;
-measuring the current temperature of the reactor chamber (10);
-comparing the current temperature with a last saved temperature;
-saving said current temperature in said memory (14);
-heating the reactor chamber (10) with the current heat output by the heater (11);
-comparing the current heat output with the limit heat output;
-saving the current heat output in the memory (14);
-outputting an error message if the current heat output is greater than the limit heat output and the current temperature is equal to the last saved temperature.
2. The method of claim 1, wherein the pre-specified heat output and/or the current heat output is a heat output averaged over a pre-specified time interval.
3. A method according to claim 1 or 2, wherein the pre-specified heat output and/or the current heat output is greater than zero when the measured current temperature is below a target temperature.
4. The method of claim 1 or 2, wherein the step of determining the limited heat output comprises the sub-step of adding a safe offset.
5. The method of claim 1 or 2, wherein the step of determining a limited heat output is repeated repeatedly such that the limited heat output is adjusted periodically.
6. The method of claim 1 or 2, wherein the step of determining a limit heat output is repeated until at least 10 heat outputs have been saved.
7. The method of claim 6, wherein the step of determining a limit heat output is repeated until at least 100 heat outputs have been saved.
8. The method of claim 6, wherein the step of determining a limit heat output is repeated until at least sufficient heat output has been saved such that all heat output expected during a pre-specified period of use has been saved.
9. A method according to claim 1 or 2, wherein the limited heat output corresponds to a maximum heat output of the heater (11).
10. The method according to claim 1 or 2, wherein in the step of determining a limited heat output, repeated measurements of the temperature of the reactor chamber (10) and repeated heating of the reactor chamber (10) are repeated within 10 seconds.
11. The method according to claim 10, wherein in the step of determining a limited heat output, repeated measurements of the temperature of the reactor chamber (10) and repeated heating of the reactor chamber (10) are repeated within 5 seconds.
12. The method according to claim 10, wherein in the step of determining the limiting heat output, the repeated measurement of the temperature of the reactor chamber (10) and the repeated heating of the reactor chamber (10) are repeated within 1 second.
13. The method of claim 1 or 2, wherein the limiting the heat output is based on filtering the saved maximum heat output.
14. The method of claim 13, wherein the filtering comprises a floating average filtering or a median filtering, and the filtering is based on at least 3 last saved thermal outputs.
15. The method of claim 14, wherein the filtering is based at least on 5 last saved heat outputs.
16. The method of claim 14, wherein the filtering is based at least on 10 last saved heat outputs.
17. The method according to claim 1 or 2, wherein the memory (14) has a ring memory and the predetermined heat output and the current heat output are written to the ring memory.
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Citations (1)

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JPH0783897A (en) * 1993-09-09 1995-03-31 Yamatake Honeywell Co Ltd Temperature control method for thermostatic chamber of gas chromatograph

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CN101031800B (en) * 2004-09-30 2011-01-05 爱科来株式会社 Analyzer
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