WO2020223749A1 - Procédé de vérification de l'état d'un capteur de temperature d'un capteur de densité - Google Patents

Procédé de vérification de l'état d'un capteur de temperature d'un capteur de densité Download PDF

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Publication number
WO2020223749A1
WO2020223749A1 PCT/AT2020/060177 AT2020060177W WO2020223749A1 WO 2020223749 A1 WO2020223749 A1 WO 2020223749A1 AT 2020060177 W AT2020060177 W AT 2020060177W WO 2020223749 A1 WO2020223749 A1 WO 2020223749A1
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WIPO (PCT)
Prior art keywords
temperature
phase transition
sensor
density
reference material
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PCT/AT2020/060177
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German (de)
English (en)
Inventor
Gerhard Murer
Original Assignee
Anton Paar Gmbh
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Publication of WO2020223749A1 publication Critical patent/WO2020223749A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K15/00—Testing or calibrating of thermometers
    • G01K15/005—Calibration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
    • G01K11/06—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using melting, freezing, or softening
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • G01N9/002—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
    • G01N9/002—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis
    • G01N2009/006—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis vibrating tube, tuning fork

Definitions

  • the invention relates to a method for checking the status of a temperature sensor of a density sensor according to claim 1, as well as a density measuring device for determining the density of a fluid according to claim 16.
  • the state of the art includes density meters for liquids and gases for laboratory applications and various evaluation methods, e.g. from AT 516420 B1 - relating to the decay behavior - and AT 515552 B1 - relating to the viscous correction - known.
  • density measuring devices usually consist of a density sensor with an integrated temperature sensor, a (solid-state) thermostat for
  • Temperature setting of the density sensor and measurement sample electronic and mechanical components for operating the density sensor and the thermostat, an electrical supply unit, a digital evaluation unit for determining, displaying and outputting the density and temperature measurements and the variables derived therefrom, as well as a housing that encloses the elements mentioned .
  • the calibration and adjustment of the density sensor is therefore usually two-stage: First, the temperature sensor integrated in the density sensor is calibrated with an external reference temperature measuring device that is calibrated to international temperature standards. For this purpose, the reference temperature sensor is introduced into the density sensor in a suitable manner. The thermostat is then used to gradually approach temperatures in the measuring range of the density meter, wait for the isothermal state and record the temperature difference between the integrated temperature sensor and the reference temperature sensor. Carrying out the temperature calibration and adjustment requires not only a suitable reference temperature measuring device but also corresponding specialist knowledge. If this is done incorrectly, there is a risk of incorrect adjustments and damage to the density sensor.
  • the characteristic curve of the integrated temperature sensor is then adjusted by adapting at least one adjustment constant so that the recorded deviations from the reference temperature sensor are minimal and the temperature measured values of the integrated temperature sensor match the measured values of the reference temperature sensor within the required specifications.
  • the thermostat can have its own temperature sensor, this is also adjusted if necessary.
  • the density sensor can be calibrated and adjusted using density standards traceable to international standards.
  • the two-stage adjustment and calibration described above is not only necessary for a new device, but also at suitable calibration intervals during the service life of the Density meter necessary. Since these measures are associated with considerable effort and the density measuring device is not ready to measure during this time, the calibration intervals cannot be selected as short as desired. If a significant change in the sensor characteristics occurs within the calibration interval, there is a risk of measurement errors and corresponding consequential damage.
  • the state of the art for the traceable calibration of temperature sensors is to introduce them into suitable devices in which temperature fixed points are realized by phase transitions of pure substances, and thus to calibrate the temperature sensors at these temperature fixed points, as for example in US 4244207 A or KR 101486731 B1 is described.
  • the temperature fixed points are determined by the International Temperature Scale from 1990 (ITS-90).
  • Comparative calibrations can be carried out using traceable, calibrated reference temperature sensors.
  • the reference temperature sensor and the temperature sensor to be calibrated are placed in a suitable device, the temperature of which is adjustable and which is able to produce isothermal conditions at the set temperature points.
  • the difference between the indications of the reference temperature sensor and the temperature sensor to be calibrated is determined and, if necessary, an adjustment of the temperature sensor is carried out, the latter usually being carried out by recalculating the adjustment constants.
  • the object of the invention is therefore to remedy the known disadvantages and to provide a method or a density measuring device which enables the status of a temperature sensor of a density sensor, in particular a density sensor installed in the density measuring device, to be checked during operation of the density measuring device without the need for a longer downtimes are required for this and the risk of damage to the density sensor is avoided.
  • the invention solves this problem with a method for checking the status of a temperature sensor of a density sensor, in which at least one reference material built into the density sensor or several reference materials are used as temperature reference, which undergo a phase transformation at precisely defined temperatures.
  • the density sensor comprises a housing, in the interior of which a flexural oscillator is arranged,
  • the density sensor comprises a temperature control unit for heating and / or cooling the density sensor, which is in thermally conductive contact with the housing of the density sensor,
  • a temperature sensor is arranged in the vicinity of the flexural oscillator in such a way that the temperature of the flexural oscillator can be detected
  • At least one reference material is arranged in the vicinity of the flexural oscillator, the at least one reference material having at least one phase transition in the heating and / or cooling area of the temperature control unit, and
  • At least one phase transition sensor for detecting the phase transition of the at least one reference material is arranged in the vicinity of the reference material (4), and
  • the density sensor is heated or cooled at least until a phase transition occurs in the at least one reference material, in particular until the at least one reference material has undergone a phase transition
  • phase transition measurement temperature measured at the detected time of the onset of the phase transition is determined in the time profile of the temperature recorded by the temperature sensor
  • Such a temperature calibration run can be carried out almost as often and automatically, for example at night, during longer work breaks or while the thermostat is operating through a phase transition range. This practically eliminates the risk of measurement errors caused by an undetected change in the sensor characteristics of the integrated temperature sensor.
  • the temperature sensor integrated as standard in the density sensor remains unaffected and is therefore ready for use in the entire temperature measuring range.
  • a temperature control unit is understood to be a device such as a solid-state thermostat with Peltier elements, with which the density sensor can be heated or cooled. Not only is the density sensor heated, but also the flexural transducer built into its interior and also the components such as the temperature sensor, the reference material and the phase transition sensor, such as the temperature sensor, the reference material and the phase transition sensor, which are arranged in the vicinity of the flexural oscillator, for example in the interior of the density sensor or outside the housing of the density sensor.
  • the heating and / or cooling range of the temperature control unit is understood to be that temperature range within which or between its upper and lower limit temperatures a heating or Cooling of the density sensor can be made by means of the temperature control unit.
  • a particularly simple and exact detection of the onset of the phase transition in the reference material can be ensured if the heating and / or cooling of the density sensor is carried out with a defined temperature gradient, in particular with a defined linear temperature ramp.
  • a particularly simple correction of the temperature measured by the temperature sensor can be achieved if the deviation of the phase transition measurement temperature measured by the temperature sensor or a value derived therefrom from the phase transition reference temperature is used to correct the temperature measured by the temperature sensor.
  • a particularly reliable variant of a method according to the invention for checking the state of a temperature sensor of a density sensor which advantageously also enables the temperature sensor to be recalibrated, can be provided if
  • the density sensor is heated and / or cooled in succession with at least two different heating and / or cooling rates
  • phase transition sensor for each heating and / or cooling rate the onset of the phase transition of the at least one reference material is detected by means of the phase transition sensor
  • phase transition measurement temperature measured at the detected point in time of the onset of the phase transition is determined
  • an extrapolation is carried out to a specified heating and / or cooling rate, in particular to a specified reference temperature, preferably by means of linear regression analysis,
  • the extrapolated phase transition measurement temperature is compared with the phase transition reference temperature specified for the respective reference material, and
  • a correction value for correcting the temperature measured by the temperature sensor is determined on the basis of the deviation determined.
  • a method according to the invention can advantageously also be used to improve the accuracy of a density measurement value determined by means of the density sensor, in that the correction value is used for a density determination for the correction of the temperature measured by the temperature sensor when the density sensor is heated and / or cooled again.
  • the density sensor is successively heated with at least two different heating and / or cooling rates
  • phase transition sensor for each heating and / or cooling rate the onset of the phase transition of the at least one reference material is detected by means of the phase transition sensor
  • phase transition measurement temperature measured at the detected point in time of the onset of the phase transition is determined
  • phase transition measurement temperature determined by the temperature sensor at the onset of the phase transition and the respective heating and / or cooling rate
  • a time constant for adjusting the different time behavior of the temperature sensor, the at least one phase transition sensor and the at least one reference material is calculated and
  • the determined time constant is used in the event of renewed heating and / or cooling of the density sensor for the correction of the temperature curve measured by the temperature sensor, the determined time constant being added or subtracted to the respective measurement times of the temperature curve so that the measurement times are shifted or a delay element, especially first order, is used for correcting the time behavior.
  • a particularly rapid statement about a possible deviation of the temperature sensor can be provided if - for each heating and / or cooling rate, the phase transition measurement temperature measured by the temperature sensor at the detected time of the onset of the phase transition is stored as a temperature sensor reference temperature, and
  • phase transition measurement temperature currently measured by the temperature sensor at the detected point in time at the onset of the phase transition is determined
  • phase transition measurement temperature currently measured by the temperature sensor is compared with the temperature sensor reference temperature stored for the respective heating and / or cooling rate, and
  • a correction value for correcting the temperature measured by the temperature sensor is determined again.
  • a temperature sensor reference temperature for comparison with the currently measured phase transition measurement temperature for heating and / or cooling rates for which no temperature sensor reference temperature has yet been stored, it can advantageously be provided that for the comparison with the phase transition currently measured by the temperature sensor -Measuring temperature at a current heating and / or cooling rate, based on the temperature sensor reference temperature stored for specified heating and / or cooling rates, a temperature sensor reference temperature for the current heating and / or cooling rate is derived, in particular interpolated or extrapolated.
  • a particularly reliable detection of the onset of the phase transition can be guaranteed if the change in a physical variable of the at least one reference material, in particular the temperature, the speed of sound, the density, the thermal conductivity or the electrical conductivity, is detected by means of the phase transition sensor as the onset of the phase transition .
  • a particularly reliable detection of the onset of the phase transition can be achieved by the time course of the change in a physical variable of the at least one reference material, which is changed by the phase transition in the reference material, in particular the temperature
  • the speed of sound, the density, the thermal conductivity or the electrical conductivity is measured by means of the phase transition sensor.
  • phase transition sensor offer the advantage that they can be designed in such a way that no significant additional costs arise for the density sensor.
  • a particularly exact detection of the onset of the phase transition can be achieved if the onset of the phase transition is determined as the intersection of the tangents or regression lines of the time curve of the physical variable measured by the phase transition sensor before and during the phase transition.
  • the onset of the phase transition is detected for each reference material, in particular by means of at least one phase transition sensor, preferably by means of a separate phase transition sensor for each reference material,
  • phase transition measurement temperature measured by the temperature sensor or a value derived therefrom is compared with a phase transition reference temperature predetermined for the respective reference material
  • the correction value for correcting the temperature measured by the temperature sensor is determined on the basis of the, preferably selected, deviations determined for the respective reference materials.
  • a check of the condition of a temperature sensor of a density sensor with particularly favorable reference materials for installation in a density sensor can be provided if water, gallium and / or indium are used as reference material.
  • the density sensor is heated or cooled at a heating or cooling rate with an increase amount or a decrease amount of 0.1 to 20 K / min and / or
  • That the heating or cooling of the density sensor is carried out in a range from at least 0.5 K below the phase transition reference temperature to at least 0.5 K beyond the end of the phase transition.
  • a particularly exact density determination by means of a density sensor checked according to the invention can be ensured if, in the course of the check for assessing the deviation of the phase transition measurement temperature or a value derived therefrom from the phase transition reference temperature, a threshold value of less than 0.05 K, in particular less than 0.02 K is used.
  • a further improvement in the accuracy of the density measurement by means of a density sensor or density measuring device checked according to the invention can be ensured if
  • the temperature control unit comprises a temperature control unit temperature sensor, the temperature control unit temperature sensor being used to determine the time profile of the temperature in the immediate vicinity of the density sensor and
  • the invention further relates to a density measuring device for determining the density of a fluid.
  • the density measuring device comprises the following components:
  • a density sensor with a housing, in the interior of which a flexural oscillator is arranged,
  • a temperature sensor being arranged in the vicinity of the flexural oscillator in such a way that the temperature of the flexural oscillator can be detected
  • the temperature sensor is designed to measure the time course of the temperature of the flexural oscillator
  • At least one reference material being arranged in the vicinity of the flexural vibrator, the at least one reference material having at least one phase transition in the heating and / or cooling area of the temperature control unit, and
  • phase transition sensor is arranged in the vicinity of the reference material, which is designed to detect the phase transition of the at least one reference material
  • a temperature control unit for heating and / or cooling the density sensor which is in thermally conductive contact with the housing of the density sensor and is designed to heat or cool the density sensor at least until a phase transition occurs in the at least one reference material, in particular up to the at least one reference material has undergone a phase transition
  • a control and evaluation unit which is connected to the temperature control unit, the phase transition sensor and the temperature sensor and which is designed to control the temperature control unit and upon detection of the onset of a phase transition of the at least one reference material by means of the phase transition sensor
  • phase transition measurement temperature measured at the detected point in time of the onset of the phase transition or a value derived therefrom in the time profile of the temperature recorded by the temperature sensor and to use a phase transition which is specified for the at least one reference material, in particular stored in the control and evaluation unit Compare reference temperature and
  • phase transition measurement temperature measured by the temperature sensor or a value derived therefrom from the phase transition reference temperature.
  • the temperature control unit is designed to heat and / or cool the density sensor with a defined temperature gradient, in particular with a defined linear temperature ramp.
  • a particularly compact and robust design of a density sensor which can be checked by means of a method according to the invention, can be provided if the temperature sensor, the flexural vibrator and the at least one reference material are arranged in the interior of the density sensor at a distance from one another in such a way that the temperature sensor and the flexural vibrator are not influenced remain from a heating and / or cooling of the at least one reference material.
  • phase transition sensors for use in a density measuring device according to the invention that detect the phase transition particularly precisely and at the same time inexpensive variants can be provided if the phase transition sensor is also used is designed to detect the change in a physical variable of the at least one reference material, in particular the temperature, the speed of sound, the density, the thermal conductivity or the electrical conductivity, as the onset of the phase transition or, if the phase transition sensor is designed, the temporal course of the change a physical quantity of the at least one reference material that is changed by the phase transition in the reference material, in particular the speed of sound, the density, the thermal conductivity or the electrical conductivity, or if the phase transition sensor is a temperature sensor connected to the reference material in a thermally conductive manner for measuring the course over time the temperature of the at least one reference material is formed.
  • a physical variable of the at least one reference material in particular the temperature, the speed of sound, the density, the thermal conductivity or the electrical conductivity
  • phase transition sensors can be used that either directly detect the occurrence of a change in the measured physical variable as the onset of the phase transition or the onset of the phase transition is determined from the time course of the measured physical variable determined by the phase transition sensor.
  • B calculated by the control and evaluation unit.
  • Disadvantageous influences on the onset of the phase transition in the reference material can be avoided by arranging the at least one reference material in a hermetically sealed container, in particular with walls made of glass, plastic or metal, in the interior of the density sensor.
  • a density measuring device which enables a particularly precise check of a temperature sensor of the density sensor, can be provided if several reference materials are arranged in the interior of the density sensor, with provision being made in particular that a separate phase transition sensor is arranged in the interior of the density sensor for each reference material.
  • Particularly inexpensive reference materials in the temperature measuring range of the density measuring device can be provided if water, gallium and / or indium is provided as the reference material.
  • the temperature control unit comprises a temperature control unit temperature sensor which is designed to determine the time profile of the temperature in the immediate vicinity of the density sensor and is connected to the control and processing unit, and
  • control and processing unit is designed to carry out a method according to the invention for checking the state of the temperature control unit temperature sensor for the temperature control unit temperature sensor.
  • An advantageous possibility for checking the status of a temperature sensor of a density sensor without the need for an external reference temperature measuring device can be provided by using at least one reference material, which has at least one phase transition and is arranged in the interior of a density sensor, for checking the status of a temperature sensor of the density sensor according to a method according to the invention.
  • a program for carrying out a method according to the invention for checking the status of a temperature sensor of a density sensor can advantageously also be stored on a data carrier and can thus be used to retrofit existing density measuring devices.
  • 1 shows a section from an exemplary embodiment of a density measuring device according to the invention with a density sensor according to the invention
  • 2 shows an embodiment of a temperature calibration method based on the phase transitions of a reference material at three different heating rates
  • phase transition measurement temperature 3 shows an exemplary embodiment of an extrapolation of the phase transition measurement temperature to a predetermined heating rate or reference temperature.
  • FIG. 1 schematically shows a section of an embodiment of a density measuring device 200 according to the invention with a density sensor 100 comprising a flexural oscillator 2 and a housing 1, which is shown in cross section as a dotted line in the embodiment in FIG. 1.
  • the flexural oscillator 2 is, for example, melted into the housing 1, which in FIG. 1 has the shape of a tube and consists of glass.
  • Such a flexural oscillator 2 arranged in the housing 1 is known, for example, from AT 516420 B1 and is designed as a hollow U-tube with two equally long, clamped legs that is filled with the sample to be examined.
  • the housing 1 can be filled with protective gas or evacuated.
  • the housing 1 encloses an interior 10 of the density sensor 100 and a temperature sensor 3 and a reference material 4 are arranged in the interior 10.
  • the temperature sensor 3 is arranged in Fig. 1 at a short distance from the flexural oscillator 2, so that the temperature sensor 3 can directly measure the time profile of the temperature of the flexural oscillator 2 and thus also the temperature of a sample contained in the flexural oscillator 2 or flowing through the flexural oscillator 2.
  • the temperature sensor 3 and / or the reference material 4 and / or the phase transition sensor 5 can also be attached to the outside of the housing 1 of the density sensor 100, for example glued.
  • a factory calibration of the temperature sensor 3, in which an external calibration device is introduced into the flexural oscillator 2, can optionally be carried out so that the dependence of the temperature measurement by the temperature sensor 3 on the distance from the flexural oscillator 2 can be examined and taken into account.
  • the reference material 4 is located in a container 41 which is designed as a hermetically sealed capsule and which is arranged in the area of the free, non-clamped end of the flexural oscillator 2.
  • a container 41 typically has walls made of thin-walled glass, metal or plastic, and the interior of the container 41 is free of interfering foreign substances and has a sufficient internal volume so that adverse effects on the phase transition temperature are avoided are. This means that the internal volume of a container 41 is significantly larger than the volume of the respective reference material 4.
  • the reference material 4 has at least one phase transition in the heating and / or cooling area of the temperature control device 6, i.e. in that temperature range within which the density sensor 100 can be heated or cooled by means of the temperature control unit 6.
  • this is a range between -60 and 200 degrees C.
  • a reference material 4 with at least one phase transition in that temperature range in which the density determination of the density of a fluid by means of the density sensor 100 can be carried out with sufficient accuracy can also be selected.
  • this is a range from -20 ° C to 100 degrees C.
  • the reference material 4 serves as a temperature reference integrated in the density sensor 100 for a temperature calibration of the density sensor 100.
  • phase transition sensor 5 is arranged in the interior 10 in Fig. 1, which is connected to the reference material 4 e.g. is coupled.
  • the phase transition sensor 5 is a temperature sensor which is connected to the reference material 4 in a manner that conducts heat well, for example by gluing or fusing, and is designed to measure the temperature of the reference material 4 over time.
  • the phase transition sensor 5 can also be designed, for example, to detect the change in a physical variable, for example the speed of sound, the density, the thermal conductivity or the electrical conductivity, which occurs in the reference material 4 when the phase transition occurs.
  • a physical variable for example the speed of sound, the density, the thermal conductivity or the electrical conductivity, which occurs in the reference material 4 when the phase transition occurs.
  • An ultrasonic sensor for example, can be used as such a phase transition sensor 5, which determines the transit time of a sound pulse through the reference material 4 and derives the propagation speed of the sound pulse in the reference material 4 therefrom.
  • the phase transition sensor 5 can also be designed to measure the time course of the change in a physical variable of the reference material 4, for example the speed of sound in the reference material 4, the density, the thermal conductivity or the electrical conductivity of the reference material 4, which is caused by the phase transition in the reference material 4 is changed, which will be discussed in more detail below.
  • phase transition sensor 5 and the associated container 41 with the reference material 4 are designed in a similar design to the integrated temperature sensor 3 and opposite the temperature sensor 3 in the area of the free end of the flexible oscillator 2 at a predetermined distance of preferably 0.1 to 2 millimeters from the Flexural oscillator 2 arranged. This is done, for example, by a thin-walled support structure made of glass or metal with the lowest possible heat capacity, which is attached to the housing 1 of the density sensor 100.
  • phase transition sensor 5 and the reference material 4 are arranged in Fig. 2 at the same distance from the flexural oscillator 2 as the integrated temperature sensor 3. This means that the time behavior of the integrated temperature sensor 3 and the reference material 4 is similar and its phase transition has a sufficient distance from the integrated temperature sensor 3 no effect on this or on the flexural oscillator 2. This means that the reference material 4 is positioned in such a way that it does not influence the temperature sensor 3 integrated as standard in the density sensor 100.
  • the temperature sensor 3 and the container 41 with the reference material 4 are arranged in the region of the free end of the flexural oscillator 2, on both sides of the flexural oscillator 2, opposite one another.
  • a temperature control unit 6 surrounds the housing 1 of the density sensor 100, which is designed as a solid-state thermostat and rests on the housing 1 following the shape.
  • Peltier elements or a spiral-shaped heating wire of the temperature control unit 6 are in contact with heat-conducting or heat-storing metal plates, so-called temperature control elements.
  • the temperature control unit 6 is therefore in thermal conduction contact with the housing 1 of the density sensor 100 and heats and / or cools it.
  • the density meter 200 is insulated from the outside, also with regard to the surface of the device and the electronics and in order to avoid heat losses.
  • the temperature control unit 6, designed as a solid-state thermostat in FIG. 1, generally surrounds the housing 1 of the density sensor 100 to a large extent. In most cases, however, a viewing window remains free for checking the filling of the oscillating vibrator 2.
  • a method according to the invention or a density measuring device 200 according to the invention also works in principle with density sensors 100 with a flexural oscillator 2 made of metal and a metal body or housing enclosing this, but glass oscillators and enclosing glass bodies are preferably used.
  • the temperature sensor 3 and the phase transition sensor 5 are shown in FIG. 1 in a preferred position in the interior 10 of the enveloping housing 1 of the density sensor 100.
  • at least one additional additional sensor is shown in FIG. 1 in a preferred position in the interior 10 of the enveloping housing 1 of the density sensor 100.
  • Temperature control unit temperature sensor 7 can be used to control the temperature control unit 6 or the solid-state thermostat. This can also be, for example, temperature regulating unit temperature sensors which also monitor the ambient temperature and / or the temperature of the measuring device housing of the density measuring device 200.
  • a reference material 4 is arranged in the interior 10 of the density sensor 100, but a plurality of reference materials 4 can also be arranged in the interior 10.
  • a single phase transition sensor 5 can be provided for detecting the phase transitions of all reference materials 4, or a separate one for each container 41 with a respective reference material 4
  • Phase transition sensor 5 If several containers 41 are arranged in the interior 10 of the density sensor 100, several containers 41 can each contain the same reference material 4, for example to determine the onset of the phase transition of the respective reference material 4 particularly precisely. Alternatively, different containers 41 can contain different reference materials 4, so that a number of different phase transitions in the heating and / or cooling area of the temperature control unit 6 or the measuring area of the density sensor 100 are available for a temperature calibration.
  • a reference oscillator can also be arranged in such a density sensor 100.
  • a density measuring device 200 according to the invention further comprises a control and evaluation unit 8, which is designed to carry out and evaluate density measurements as well as to carry out a checking method according to the invention, which will be discussed in more detail below.
  • the density of the fluid is derived from a control and evaluation unit 8, for example from the frequency of the oscillation of the flexural oscillator 2 filled with a fluid to be examined, as is the case, for example, in FIG. B. is described in AT 515552 B1. Any mechanisms for generating the oscillation and decreasing the frequency of the oscillation are known from the prior art, for example by means of magnets and current-carrying coils, but also, for example, by striking the oscillator.
  • the control and evaluation unit 8 is connected to the temperature control unit 6 and controls it. Furthermore, the control and evaluation unit 8 is connected to the temperature sensor 3 and the phase transition sensor 5, and possibly with a temperature control unit temperature sensor 7, so that the measurement data from the sensors are transmitted to the control and evaluation unit 8 and can be evaluated by it.
  • the control and evaluation unit 8 can also have a display which is arranged on the measuring device housing of the density measuring device 200, so that a user can access data, e.g. desired threshold values, or warnings can be displayed to him.
  • An excitation and sensor device of the control and evaluation unit 8, which set the oscillating vibrator 2 filled with the fluid to be examined vibrating comprises in the exemplary embodiment in FIG. 1 piezo elements 9a, 9b that excite the vibrating vibrator 2 to a forced oscillation close to its natural frequency .
  • This procedure is known from AT 516420 B1, for example.
  • two piezo elements 9a, 9b are schematically in the area of the clamping of the legs, which on the one hand excite the oscillation and on the other hand decrease the frequency.
  • a method according to the invention for checking the status of a temperature sensor of a density sensor 100 or a density measuring device 200 runs according to the following scheme: First, the density sensor 100 is heated or cooled by means of the temperature control unit 6 until it enters the reference material 4 or, if necessary, all reference materials 4 Phase transition occurs or has been passed through by these. This can be beneficial also take place during a density measurement process when the temperature of the sample is approaching the measurement temperature.
  • phase transition sensor 5 or, if applicable, several phase transition sensors 5 determine the onset of the phase transition for the reference material 4 or several reference materials 4.
  • phase transition measurement temperature T mess measured by the temperature sensor 3 when the onset of the phase transition is detected is determined by the control and evaluation unit 8 in the profile of the temperature of the flexural oscillator 2 recorded by the temperature sensor 3.
  • the phase transition measurement temperature T mess determined in this way is then compared with a phase transition reference temperature T so n predetermined for the at least one reference material 4 for the onset of the phase transition.
  • This predetermined phase transition reference temperature T so n can be available, for example, for different heating and / or cooling rates and / or reference temperatures and can be stored, for example, in the control and evaluation unit 8 or also entered by the user of the density measuring device 200.
  • phase transition measurement temperature T measured value for example a to a predetermined heating and or cooling rate or a predetermined reference temperature extrapolated phase transition measurement temperature T extrap, with the predetermined phase transition reference temperature T soN be compared .
  • a comparison can be carried out, for example, by a comparator, but also by suitable software present in the control and evaluation unit 8 of the density measuring device 200.
  • the control and evaluation unit 8 also determines the deviation of the phase transition measurement temperature T mess measured by the temperature sensor 3, or a value derived therefrom, from the phase transition reference temperature T SON .
  • the Control and evaluation unit 8 If the deviation of the phase transition measurement temperature T mess measured by the temperature sensor 3, or of the value derived therefrom from the phase transition reference temperature T so n, exceeds a predetermined threshold value, the Control and evaluation unit 8, a message can be issued to the user that, for example, a recalibration of the temperature sensor 3 is required.
  • Predefined threshold values of this type can, for example, also be stored in the control and evaluation unit 8, or can be entered by the user on the density measuring device 200.
  • 0.02 K for density measuring devices 200 which provide values with a 5-digit accuracy
  • 0.05 K for density measuring devices 200 with a 4-digit accuracy can be used as threshold values for assessing the deviation.
  • an external reference temperature measuring device can be dispensed with, as a result of which the checking of the density measuring device 200, in particular during the period of use, is considerably simplified for the users.
  • the check with an external reference temperature measuring device requires not only this but also corresponding specialist knowledge and is associated with the risk of damaging the density sensor 100 in the process.
  • the invention avoids these problems.
  • a check can be carried out almost as often and automatically, for example even during a density measurement. This practically eliminates the risk of measurement errors caused by an undetected change in the sensor characteristic of the integrated temperature sensor 3.
  • the temperature sensor 3 integrated as standard in the density sensor 100 remains unaffected and is therefore ready for use in the entire temperature measuring range of the density meter 200.
  • the components necessary for the application of the method according to the invention in the density sensor 100 can be designed in such a way that no significant additional costs arise for the density sensor 100.
  • phase transition temperature ranges of the reference material 4 or the reference materials 4 are passed through with the temperature control unit 6 or the thermostat at various suitable heating rates.
  • the comparison of the phase transition Reference temperatures T so n with the respective phase transition measurement temperature T mess of the integrated temperature sensor 3 thus takes place in the course of suitable temperature ramps.
  • the temperature ramp is linear heating or cooling with a constant heating or cooling rate over a predetermined period of time, i.e. with a constant temperature gradient understood.
  • the phase transition sensor 5 is designed as a temperature sensor that is thermally coupled to the reference material 4 and determines the time profile of the temperature of the reference material 4, as has already been described in connection with FIG. 1.
  • the thermal time constants of the integrated temperature sensor 3 and the integrated reference material 4 or the reference materials 4 can, however, differ from one another. This can be seen in FIG. 2, where the time profile of the measured values of the integrated temperature sensor 3 is shown as a dash-dotted line and the time profile of the measured values of the phase transition sensor 5 is shown as a solid line.
  • the measured values of the two sensors differ from one another, since the temperature sensor 3 heats up faster in the exemplary embodiment shown than the reference material 4, as a result of which the phase transition sensor 5 measures lower values than the temperature sensor 3 at a respective measurement time.
  • temperature ramps can be run through with at least two different heating rates or rates of change and an extrapolation of the input signal of the phase conversion to a specified heating rate or a specified reference temperature can be carried out.
  • FIG. 2 shows by way of example how the temperature calibration is carried out with a reference material 4.
  • the phase transition region of the reference material 4 is passed through in the example in FIG. 2 with three different heating rates or temperature rise rates of 1 K / min, 2 K / min and 3 K / min.
  • the measured values of the integrated temperature sensor 3 and the phase transition sensor 5, which is a further temperature sensor, are recorded.
  • the point in time at which the phase transition begins is determined by the control and evaluation unit 8. This can for example, by determining and cutting the tangents of the measurement signal recorded by the phase transition sensor 5 before the phase transition and during the phase transition, which are shown in dashed lines in FIG.
  • phase transition measurement temperatures T mess determined by the integrated temperature sensor 3, calculated by the control and evaluation unit 8, respectively, in FIG. 2 these are the temperatures T 3 , T 2 and Ji for the three different heating rates the basis of further calculation.
  • the phase transition measurement temperature T mess measured by the integrated temperature sensor 3 is adjusted to a heating rate or rate of rise of, for B. 0 K / min, ie a predetermined reference temperature, extrapolated (see Fig. 3).
  • a suitable, for example linear, relationship the phase transition measurement temperature T mess measured by the integrated temperature sensor 3 is adjusted to a heating rate or rate of rise of, for B. 0 K / min, ie a predetermined reference temperature, extrapolated (see Fig. 3).
  • a suitable, for example linear, relationship the phase transition measurement temperature T mess measured by the integrated temperature sensor 3 is adjusted to a heating rate or rate of rise of, for B. 0 K / min, ie a predetermined reference temperature, extrapolated (see Fig. 3).
  • at least two data points or phase transition measurement temperatures T mess are required.
  • the regression lines are determined with at least two points and these intersect with one another. The point of intersection then gives the point in time of the phase transition and the temperature T meas measured by the temperature sensor at this point in time. Any complex algorithms for data analysis are possible here in order to determine the individual T meas .
  • the calculation is carried out, for example, via a compensation calculation by minimizing the possibly weighted deviation squares.
  • This procedure is, for example, at https://de.wikipedia.org/wiki/Methode_der_kleinsten_Quadrate (last accessed on 2.5.2019), and https://en.wikipedia.org/wiki/Least_squares (last accessed on 2.5.2019).
  • the relationship between the individual T does not necessarily have to be linear here.
  • the individual measured values for the individual T are measured against the respective heating rate dQ / ⁇ t plotted and extrapolated to a heating rate of zero Kelvin / minute.
  • the approach y ax + c, which reflects a linear behavior of the temperature values, can be used, for example.
  • the extrapolated temperature of the integrated temperature sensor at a rate of increase of 0 K / min, the deviation from the nominal value of the phase transition reference, ie the phase transition reference temperature, can be determined.
  • the regression line is then formed accordingly.
  • Table 1 Phase transition measurement temperatures T mess at the respective heating rate Dq / ⁇ t, extrapolated measurement temperature T extrap at 0 K / min, phase transition reference temperature T s 0M and deviation T extrap - T SoN
  • Table 1 shows an example of the process of calculating the deviation of the phase transition measurement temperature measured by the integrated temperature sensor 3 extrapolated to a rate of increase of 0 K / min.
  • the phase transition measurement temperatures T mess of the integrated temperature sensor 3 assumed in Table 1 at the respective point in time of the phase transition result in a linearly extrapolated phase transition measurement temperature T extrap of the integrated temperature sensor 3 of 29.71 ° C at a heating rate or rate of increase of 0 K / min. From this, the deviation of the integrated temperature sensor 3 of -0.05 K from the setpoint value of the phase transition reference, ie the phase transition reference temperature T So n of 29.76 ° C., is calculated.
  • this deviation is greater than the specified error limits of the temperature measurement of the density sensor 100, i. greater than the stored threshold value for the deviation, this deviation can be eliminated by calculating a correction value and thus used for an adjustment of the temperature sensor 3.
  • This adjustment can advantageously also take place over a larger temperature range with a plurality of reference materials 4 and corresponding adjustment constants. To minimize this deviation, adjustment constants of the integrated temperature sensor 3 can be recalculated, for example.
  • the temperature output of the temperature sensor 3 is thus corrected.
  • this correction value can optionally be used when the density sensor 100 is heated again, e.g. a density determination can be used to correct the temperature measured by the temperature sensor 3.
  • This process can be carried out both automatically and user-controlled. For example, a warning message can be displayed to the user or an acoustic warning signal can be emitted if the deviation exceeds the predefined threshold value.
  • phase transition reference temperature T SoN the phase transition reference temperature T SoN . If a significant temperature difference is determined between the temperature determined by the integrated temperature sensor 3 and the temperature determined by the reference temperature measuring device, it may be necessary to correct the stored phase transition reference temperature T Soii .
  • an external reference temperature measuring device can be dispensed with, as a result of which the calibration and adjustment of the density measuring device 200, in particular during the period of use, are significantly simplified for the users.
  • the calibration with an external reference temperature measuring device requires, in addition to this, corresponding specialist knowledge and is associated with the risk of damaging the density sensor 100 in the process.
  • the invention avoids these problems.
  • a temperature calibration run can be carried out almost as often and automatically, for example at night, during longer work breaks or while the temperature control unit 6 or the thermostat is operating through a phase transition range. This practically eliminates the risk of measurement errors caused by an undetected change in the sensor characteristic of the integrated temperature sensor 3.
  • a time constant calibration is carried out prior to the implementation of a checking method according to the invention, as described above, in order to align the thermal time constant of the integrated temperature sensor 3 with that of the phase transition sensor 5 and the reference material 4 or reference materials 4. This means that the different time behavior during tempering, i.e. during heating or cooling, the temperature sensor 3, the phase transition sensor 5 and the reference material 4 are adjusted to one another.
  • the time behavior of the integrated temperature sensor 3, the phase transition sensor 5 and the reference material 4 can be adjusted, for example, by digital signal processing. This can be done, for example, in that the faster element is dynamically delayed by digital delay elements.
  • the time constant required for this is calculated as follows for the exemplary embodiment shown in FIG. 2: First, the density sensor 100 is successively operated with at least two different heating rates, in the exemplary embodiment there are three different heating rates, heated. For each heating rate, the onset of the phase transition of the at least one reference material 4 is detected by the control and evaluation unit 8 by means of the phase transition sensor 5, for example as described above, and the temperature measured by the temperature sensor 3 when the onset of the phase transition is detected, ie the phase transition measurement temperature T mess , determined.
  • the control and evaluation unit 8 sets a time constant t to adjust the different heating behavior of the temperature sensor 3 and the phase transition sensor 5 and the reference material 4 or of the reference materials 4 calculated.
  • the integrated temperature sensor 3 heats up more quickly because the phase transition measurement temperature T mess measured by the integrated temperature sensor 3 at the time the phase transition occurs increases as the temperature rise rate or heating rate increases. From this, for example, a first-order delay element with a time constant t of
  • T AT meas / A (A / At) for temperature sensor 3 can be calculated.
  • higher-order digital delay elements can also be used, in which case the time constant calibration and determination of the time constants are correspondingly more complex.
  • the integrated temperature sensor 3 has a time behavior that is sufficiently similar to the time behavior of the phase transition sensor 5 with the reference material 4.
  • This delay element can be implemented digitally, ie by delaying the temperature signal of the temperature sensor 3 with a first-order delay element, or this delay is taken into account when evaluating the phase transition measurement temperature T mess . If such a time constant calibration has been carried out, a calibration run with only one heating rate or temperature rise rate is sufficient to determine the deviation of the phase transition measurement temperature T mess of the integrated temperature sensor 3 from the phase transition reference temperature T SON of the reference material 4. The difference between the digitally delayed measured value of the phase transition measurement temperature T mess of the integrated temperature sensor 3 at the onset of the phase transition to the phase transition reference temperature T soN corresponds directly to the deviation of the integrated temperature sensor 3.
  • the temperature sensor 3 is first checked, as described above. For each heating rate, the phase transition measurement temperature T mess that was measured by the temperature sensor 3 at the point in time at which the onset of the phase transition was detected is stored as the temperature sensor reference temperature T ' mess in the control and evaluation unit 8.
  • control and evaluation unit 8 compares the currently measured phase transition measurement temperature T mess with the stored value of the temperature sensor reference temperature T ' mess of the integrated temperature sensor 3 when using the phase transition that was previously stored for the current heating rate.
  • a warning by the control and evaluation unit 8 can for example be given or will be displayed and, optionally after a confirmation by the user, a new temperature calibration, as described above, are performed.
  • the method of temperature calibration with the integrated phase change temperature reference has so far only been shown for a reference material 4. If several reference materials 4 are installed, the integrated temperature sensor 3 is calibrated at the corresponding phase transition reference temperatures. The processes are the same for each reference material 4 as described above. For any recalculation of the adjustment constants of the integrated temperature sensor 3, several or all of the available correction values are used.
  • the density sensor 100 can, for example, be heated or cooled at a heating or cooling rate with an amount of increase or amount of decrease of 0.1 to 20 K / min.
  • the heating or cooling of the density sensor 100 advantageously takes place in a range of at least 0.5 K below the phase transition reference temperature to at least 0.5 K above the final temperature of the phase transition, so that the reference material 4 or possibly all reference materials 4 at least one Have gone through phase transition.
  • the temperature control unit 6 can optionally include a temperature control unit temperature sensor 7, with which the time profile of the temperature in the immediate vicinity of the density sensor 100 is determined.
  • the temperature control unit temperature sensor 7 is connected to the control and Evaluation unit 8 connected so that a temperature calibration can also be carried out for the temperature control unit temperature sensor 7 as in one of the exemplary embodiments described above.
  • the temperature sensor 3 instead of the time profile of the temperature of the flexural oscillator 2, the temperature sensor 3 or in addition to it, the time profile of the temperature in the immediate vicinity of the housing 1 of the density sensor 100 is determined.
  • the temperature measured by the temperature control unit temperature sensor 7 is then determined for the respective current heating rate and compared with the phase transition reference temperature T soN . If a predefined threshold value is exceeded by the deviation of these two temperatures, a correction value for the temperature control unit temperature sensor 7 can be determined as described above. All of the exemplary embodiments of a method according to the invention described above for the temperature sensor 3 integrated in the density sensor 100 can also be used for the temperature control unit temperature sensor 7.

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Abstract

L'invention concerne un procédé de vérification de l'état d'un capteur de température d'un capteur de densité (100), - le capteur de densité (100) comprenant un boîtier (1) dans l'espace intérieur duquel est disposé un résonateur de flexions (2), - le capteur de densité (100) comprenant une unité de régulation de température (6) destinée à chauffer et/ou refroidir le capteur de densité (100), laquelle unité de régulation de température est en contact de conduction de chaleur avec le boîtier (1) du capteur de densité (100), - un capteur de température (3) étant disposé à proximité du résonateur de flexions (2) de façon à pouvoir détecter la température du résonateur de flexions (2), au moins un matériau de référence (4) étant disposé à proximité du résonateur de flexions (2), l'au moins un matériau de référence (4) comportant au moins une transition de phase dans la plage de chauffage et/ou de refroidissement (6) de l'unité de régulation de température (6) et - au moins un détecteur de transition de phase (5) est agencé à proximité du matériau de référence (4) pour détecter une transition de phase de l'au moins un matériau de référence (4), a) le capteur de densité (100) étant chauffé ou refroidi au moins jusqu'à ce qu'une transition de phase commence dans l'au moins un matériau de référence (4), en particulier jusqu'à ce qu'une transition de phase s'est déroulée dans l'au moins un matériau de référence (4), b) le tracé dans le temps de la température du résonateur de flexions (2) étant mesuré au moyen du capteur de température (3), c) le commencement de la transition de phase de l'au moins un matériau de référence (5) étant détecté au moyen du détecteur de transition de phase (5), d) la température mesurée de transition de phase (Tmess) à l'instant détecté du commencement de la transition de phase étant déterminée dans le tracé dans le temps de la température détectée par le capteur de température (3), e) la température mesurée de la transition de phase (Tmess) mesurée par le capteur de température (3) ou une grandeur dérivée de celle-ci étant comparée à une température de référence de transition de phase (Tsoll) pour le commencement de la transition de phase, prédéfinie pour l'au moins un matériau de référence et f) l'écart entre la température mesurée de la transition de phase (Tmess) ou un grandeur dérivée de celle-ci et la température de référence de transition de phase (Tsoll) étant déterminé.
PCT/AT2020/060177 2019-05-03 2020-04-30 Procédé de vérification de l'état d'un capteur de temperature d'un capteur de densité WO2020223749A1 (fr)

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CN114558343B (zh) * 2022-02-28 2023-05-05 中国科学院长春应用化学研究所 一种真空升华提纯装置

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