• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a method for determining the filling quality of a bending oscillator, the oscillator tube of which flows through the measuring fluid. According to the invention, the relationship between the viscosity-dependent density of the measuring fluid and the quality and / or damping of the oscillator tube, preferably the amplitude and / or phase of a natural vibration, is determined by the relationship between the dynamic viscosity and the damping and / or quality the measurement fluid is determined and these values are used to create an adjustment curve or table which represents the functional relationship between a parameter relevant for the quality and / or damping of the bending oscillator and the viscosity of the measurement fluid that is measured during measurement of the measurement fluid Bending oscillator with a separate, additional or additional measuring device at least one measured value for the dynamic viscosity of the measuring fluid is determined that in the course of measuring the measuring fluid with the bending oscillator at least one measured value for the relevant parameter, preferably the density of the measuring fluid, determine t is determined by the obtained measured value for the viscosity on the adjustment curve or in the adjustment table or determined function value with the function value, which determines or determined by the obtained value for the quality and / or damping on the adjustment curve or table is, and that the result of this comparison is evaluated in terms of the presence of a filling error or used to determine a possible filling error of the bending oscillator.
    公开号:AT516302A1
    申请号:T50726/2014
    申请日:2014-10-10
    公开日:2016-04-15
    发明作者:Wolfgang Dr Belitsch；Stefan Dipl Ing Dr Rossegger；Robert Dipl Ing Dr Amsüss
    申请人:Anton Paar Gmbh；
    IPC主号:
    专利说明:

    The invention relates to a method for determining the filling quality of a bending oscillator, whose oscillator tube is flowed through by the measuring fluid, and to an apparatus for carrying out the method according to the preamble of patent claim 14.
    The primary object of the invention is the detection of gas bubbles in the filling of a bending vibrator, which are located in the sample liquid to be measured and would lead to an incorrect measurement result. For this purpose, the fact is exploited that gas bubbles in the sample liquid cause not only a change in the resonance frequency but also a change in the quality of the vibration system.
    The measurement of the density of fluid media with a flexural vibrator is based on the fact that the vibration of a hollow body filled with a sample to be examined depends on the filling of the vibrator tube, i. from the mass or when the volume is constant, from the density of the filled medium.
    An insertable measuring cell contains the oscillatory structure, namely a hollow, U-shaped bent, glass or metallic tubular body. This is electronically excited to an undamped oscillation. The two legs of the U-shaped tube form the spring elements of the oscillator. The natural frequency of the U-shaped vibrator tube is only affected by that part of the sample that actually participates in the vibration. This vibrating volume V is bounded by the stationary vibrating nodes at the clamping points of the vibrator tube. If the vibrator tube is filled with the sample at least up to the clamping points, the same well-defined volume V always participates in the vibration and the mass of the sample can therefore be proportional to their density are assumed. Overfilling of the vibrator beyond the clamping points is irrelevant to the measurement. For this reason, the oscillator can also measure densities of fluids that flow through the vibrator.
    For example, the excitation of the legs of the U-shaped tube against each other. This results in certain resonant frequencies for the oscillator, in which the system preferably oscillates.
    The density of the liquid thus determines the specific frequencies at which the U-shaped tube oscillates. Using precision glass tubes or metal tubes, their harmonic properties vary depending on the density and viscosity of the liquid. The resonance frequencies are varied by suitable excitation and decrease of the
    Vibrations evaluated and determined from the period of the density of the filled fluid sample. The transducer is calibrated with fluids of known density to make the measurements evaluable.
    Such density oscillators or bending oscillators have been known for a long time and are produced in various embodiments with regard to excitation and decay of the oscillation. (for example with magnetic coils and magnets, piezoelectric elements, capacitive measurement ...)
    1 shows schematically such a bending oscillator 11.
    Here, the vibration is generated by a magnet 7 directly on the oscillator tube 3, which interacts with an opposing coil 6. A second combination of coil 5 and magnet 4 is mounted on the other leg 2 of the U-shaped tube for the decrease of the formed vibration. 9 denotes an evaluation unit.
    Excitation and acceptance can also take place here by means of piezoelectric elements, for example, the elements are mounted in such a way that they do not lie in a nodal point of the vibrations of the vibrator which are examined, but can also for example take place close to the clamping point.
    The excitation of the oscillator to oscillations is effected by means of, for example, a digital excitation amplifier, which is connected in a control circuit with the acceptance signal, e.g. regulated to the maximum amplitude and thus to the natural vibration of the bending oscillator. The control and evaluation electronics here measure the signals, e.g. Amplitude, frequency and phase angle, between excitation and decrease signal or other parameter representative of the quality of the vibrator and thus of the damping of the system.
    The frequencies characteristic of the oscillator depend on the material of the oscillator tube 1 and its geometry, in particular the diameter of the U-shaped tube 1, the length of the legs 2, 3, the bending radius and thus also the distance between the two legs 2, 3 to each other
    At a certain temperature, to calculate the density of the vibration period, consider a hollow body of mass m elastically suspended on a spring at spring rate R. Its volume V is filled with a fluid of density p. For the period P of this system in the fundamental mode, the following applies:
    (1) this results in reshaping for the density:
    (2) with the adjustment constants A and B. These contain the spring rate R of the oscillator, its void mass and the volume of the fluid which participates in the oscillation. A and B are therefore apparatus constants or adjustment values of an individual oscillator. They can be determined from two measurements of the oscillation period of the oscillator filled with fluids of known different density, normally air and water or special calibration standards. The behavior of the vibrator and thus also the constants A and B are, however, viscosity-dependent. Thus, the above-determined density value can or must be provided with a viscosity correction as a rule.
    It is known that the damping of the bending momentum is mainly influenced by the viscosity and the homogeneity of the sample. Assuming that there is no filling error, a correct functional relationship between the viscosity and the quality of a resonant oscillation can be found with the correct construction and dimensioning of the oscillator.
    The influence of the dynamic viscosity (η) on the viscosity-dependent density measurement error (Kv (η) = Δρ (η) / p) in the measurement of the density of the sample liquid to be investigated is also known and shown in FIG. Fig. 2 shows the course of the measurement error of the bending oscillator due to the viscosity.
    In commercially available flexural vibrators, this dependence is used for the viscosity correction of the density reading (see, for example, AT 400 767 B, EP 0 487 499 A2, US 5,339,258). All of these corrections are based on the relationship between the quality of the vibrator and the viscosity of the transducer fluid.
    As a measure of the attenuation often the quality factor (quality factor Q) is used, by definition, it can be determined for a resonant oscillation at resonant frequency fres and associated half-width of the resonant curve Δ fFwHM of the oscillator by Q = fres / ΔfFWHM. The quality factor is thus a measure of the damping of the oscillator and indirectly proportional to this. Frequently, not only density meters are used for extended characterization of samples, but also other measuring instruments or sensors, such as sound velocity meters or viscosity meters. For combination measurements with different sensors, the measurement results of the one sensor can be made available to the second sensor or its evaluation unit, for example, via an interface. Furthermore, the sensors can also be operated with a single evaluation and display unit. The calculation unit then has the measured values of both sensors directly available.
    For example, a rotational viscometer for determining the dynamic viscosity of fluid samples is known in which the sample is first fed to a flexural vibrator 11 for the measurement of density and subsequently to a viscosity meter 12. A common evaluation and display unit 9 processes the signals from oscillator and viscosity sensor and displays both viscosity and density of the fluid being tested.
    Fig. 3 shows schematically such a rotational viscometer.
    However, the flexural vibrator 11 illustrated in FIG. 3 can also be used in combination with other sensors, such as rotational viscometers or sensors, which determine the viscosity via the vibration of membranes (MEMS).
    According to the invention, a method of the type mentioned is characterized by the features specified in the characterizing part of patent claim 1. It is envisaged that the relationship between the viscosity-dependent density of the measuring fluid and the quality and / or damping of the vibrator tube, preferably the amplitude and / or phase of a natural vibration, is determined by determining the relationship between the dynamic viscosity and the damping and / or quality of the measuring fluid and with these values an adjustment curve or -tabeile is created, which represents the functional relationship between a decisive for the quality and / or the damping of the Bevelwingers parameters and the viscosity of the measuring fluid that in the course of measuring the measuring fluid with the bending vibrator with a separate, further or additional measuring device at least one measured value for the dynamic viscosity of the measuring fluid is determined, that in the course of the measurement of the measuring fluid with the bending oscillator at least one measured value for the relevant parameter, preferably the density of the measuring fluid, is determined by denha The measurement value for the viscosity on the adjustment curve or in the adjustment table-related or specific function value agrees with the function value that is determined or determined by the obtained measurement value for the quality and / or damping on the adjustment curve or parts, and that the result of this comparison is evaluated with regard to the possible presence of a filling error or used to determine a faulty filling error of the bending oscillator.
    A device according to the invention is characterized in that the device has a measuring unit in the form of a bending oscillator 11, which determines the viscosity-dependent density value of the measuring fluid flowing through the oscillator tube, that the device additionally has a unit for determining the values of the dynamic viscosity of the measuring fluid, that these two measuring units are connected to an evaluation unit connected, which determines the viscosity-dependent density values from the quality and / or attenuation of the oscillator tube of the bending oscillator, and that the evaluation unit contains a Justierkurve or -tabeile, which Justierkurveoder- tabeile the previously determined functional relationship between a decisive for the quality or damping of the bending oscillator parameters and contains or represents the dynamic viscosity of the measurement fluid.
    In this way, a value for the dynamic viscosity of the filled fluid can be made available to the flexural vibrator for examining the filling quality and the viscosity of the fluid to be examined, which is known from the measurement, is used to investigate the filling quality of the flexible oscillator or of the system.
    The method is based on the effect that the attenuation is mainly influenced by the viscosity and the homogeneity of the sample. Assuming that there is no filling error, a correct functional relationship between viscosity and quality can be found, given the correct construction and dimensioning of the oscillator.
    With known reference viscosity of the sample can thus be given a deviation from the expected quality, which is directly proportional to the probability of filling error.
    The Füllfehlererkennung then takes place in several steps: 1. In an evaluation at least one Justierkurve is deposited, which brings a characteristic of the quality and / or damping of the bending oscillator reading with the dynamic viscosity of the fluid in a functional context, eg. a dependence of the square root of the quality on the dynamic viscosity. The calibration curve can be determined with standards of known viscosity and / or density or calculated for the linear regions for a transducer by simulation; it is also possible to deposit only one value table. 2. A separately operating, external, further measuring unit is used to determine the viscosity value of the fluid to be examined and this is provided for the detection of the filling quality of the vibrator of the evaluation unit of the bending oscillator or the common evaluation unit. 3. At least one characteristic of the attenuation characteristic of the fluid to be examined is measured, wherein the fluid to be examined is examined with the bending oscillator. 4. From the comparison of the measured value, which is representative of the quality / attenuation of the oscillator, with the measured value, which is determined in the density measurement with the bending oscillator, one can judge the extent to which a blasenfreiebzw. of inhomogeneities free filling of the vibrator is present. 5. For the comparison of the two values, a maximum allowable deviation for a specific accuracy for the actual measurement of the density measured value can be predefined. Optionally, if the measured value deviates from the expected value, a warning is issued and the user is prompted to refill the measuring system.
    Beforehand, in a first step for adjustment by means of samples with known values or adjustment standards, the dependence of the quality or one derived therefrom
    Size determined by the density and viscosity. This dependency is represented as a function and stored, as shown in FIG. This dependency can also be stored as a value table or adjustment table in the evaluation unit.
    Thus, each vibrator can be provided with an adjustment function which represents the relationship between a parameter representative of the quality / attenuation of the vibrator and the viscosity.
    The measurement of the quality of the fundamental or also of a harmonic of the oscillator can take place in a known manner in different ways, such as phase rotation, decay measurement amplitude measurement, amplitude modulation, bandwidth measurement of the resonance or period measurement in two different natural frequencies of the vibration system.
    This adjustment function is provided in the evaluation unit of the device according to the invention. With such an evaluation unit, the measurement takes place, in which a measured value for the quality and a measured value for the viscosity is determined and the distance, if necessary a distance measure, which is determined by these two measured values on the adjusting curve or in the adjustment table. Examples of adjustment curves for different resonant frequencies are Fig. 4 zuentnehmen.
    The further steps can take place at least in different ways.
    For example, as shown in FIG. 5, multiple measurements may be used to establish a tolerance band within which the measurements for the attenuation and / or quality of an unknown sample liquid to be measured and for a given or measured viscosity must lie.
    Justification measurements on a plurality of samples give an error interval for each measurement point of the calibration curve. The measured value resulting from the measurement of the unknown sample liquid is checked to see whether it lies within the defined tolerance band. If this measured value is outside, it indicates that the filling quality of the vibrator is outside the defined range.
    A particularly preferred embodiment of this procedure proposes to use the purely statistical z value for checking this tolerance band.
    The z-value allows you to take a sample from a sample and calculate how many standard deviations it is above or below the mean. In addition, the standard deviation of the individual measuring points is determined when creating the adjustment curve. The z-value results from the actual measured value of the quality Q or the parameter P representative of the damping / damping of the oscillator as a function of the viscosity Eta - the functional value of the determined or calculated quality Q as a function of the viscosity and describes the deviation a reading as a multiple of the standard deviation.
    Compared to known methods of bubble detection, the proposed one is very simplified and less error-prone, since it reduces the decision parameters necessary for it to one, namely the reference viscosity.
    4 shows an example of the course of the quality for different
    Oscillation frequencies of the oscillator as Q = ί (η).
    Fig. 5 shows measured values lying inside and outside the tolerance band and makes it possible to decide whether filling errors are present over the z-result (multiple of the standard deviation G).
    Depending on the mode used and the required accuracy of the bubble detection, the viscosity used or the value of the viscosity used as the measured value must not be known very precisely. In general, an error < 10% is sufficient for the determined viscosity value. This viscosity can therefore also be measured with simple means. Furthermore, this approach speeds up the detection of bubbles because it requires no further information and can be used at the beginning of the densitometry. Online monitoring is possible.
    This procedure has the advantage that even during filling and without calculation of a density value with known viscosity, the measured data can be used directly for checking the filling quality.
    At the z-value one also recognizes how well the oscillator tube is filled and receives an immediate statement until the z-value for the desired accuracy of the measurement is correct. Here one can easily determine empirical limits. Since the density measurement of the smallest bubbles is often not very heavily influenced, one can determine the limits here from the desired accuracy of the density measurement. 1. A further possibility of evaluation is that an adjustment curve takes place, as shown in FIG. 2, wherein Kv = F (n) is determined with different density and viscosity standards.
    This adjustment function is a direct adjustment function that directly correlates the density error of the bending oscillator with the viscosity. 2. A density correction value Kd is determined from the measurement of the attenuation or a derived quantity. Here, not only one parameter is measured, but the parameter is translated into the below 1) determined function with another adjustment curve.
    For example, by plotting the error Delta Rho to Rho as a function of goodness, one obtains a parabola relationship that looks approximately as shown in Fig. 6: 3. A density correction value Kv is calculated from the value measured by the viscometer and from the adjustment curve, respectively of the bending oscillator used (adjustment measurements with different viscosity standards) 4. The values Kd, determined from the adjustment function of the quality of a natural vibration, and Kv are compared with each other. If they do not agree within a predetermined limit, a fill error warning is issued. For example, it may be determined that the amount of difference Kd-Kv must not exceed a certain value, for example, Kd-Kv < 0.0001.
    This, too, ensures that the quality of the oscillator correlates with the actual viscosity of the filled medium and that inhomogeneities in the filling of the oscillator do not distort the measured value.
    Determining the filling quality in the SVM:
    Of course, the filling in the viscometer presented above may also be inadequate and the viscosity value determined may not correspond to the facts. Thus, the tested viscosity value of the sample is erroneous and, in the second presented method, there is a discrepancy between the two correcting values for the density although the filling of the vibrator has been done correctly.
    This can be checked, for example, by determining the actual viscosity of the fluid from the quality of the oscillator via the adjustment curve in the evaluation unit.
    In addition, when combined with a viscosity measurement, the plausibility of the viscosity measurement can be tested. A possible coarse sensing error, or more generally, a miscibility of viscosity, can be identified by the inverse method (see Figure 7).
    For this, a second harmonic or any other mode would have to be examined and measured as described in the above-mentioned methods. From the functional relationship can be deduced from a quality so on the viscosity. If the curve is not unique, the combination of two measurements can also determine the correct viscosity value to use. If the determined viscosity from the quality of the first self-oscillation investigated agrees with that of a second mode investigated, then it can be assumed that the filling error is to be found in the viscometer or in the incorrectly measured viscosity value and the bending oscillator is correctly filled.
    A combination of the methods thus leads to a reliable detection of whether the difference lies in the viscosity measurement. If the grades of two different natural oscillations (for example, fundamental and first harmonic) do not match, it is likely that the fill error is in the density cell.
    权利要求:
    Claims (16)
    [1]
    1. A method for determining the filling quality of a bending oscillator, whose oscillator tube is flowed through by the measuring fluid, characterized in that - determines the relationship between the viscosity-dependent density of the measuring fluid and the quality and / or damping of the oscillator tube, preferably amplitude and / or phase of a natural vibration is determined by determining the relationship between the dynamic viscosity and the damping and / or quality of the measuring fluid and with these values an adjustment curve or tabeile is created that the functional relationship between a relevant for the quality and / or the damping of the Bevelwingers parameters and the viscosity of the Reproduces at least one measured value for the dynamic viscosity of the measuring fluid during the measurement of the measuring fluid with the bending oscillator with a separate, additional or additional measuring device, that in the course of measuring the measuring f at least one measurement value for the relevant parameter, preferably the density of the measurement fluid, is determined with the flexible oscillator, that the function value determined by the obtained measurement value for the viscosity on the adjustment curve or in the adjustment table corresponds to the function value determined by the measured value obtained for the quality and / or damping on the adjustment curve or parts is conditional or determined, and that the result of this comparison is evaluated with regard to the possible presence of a filling error or used to determine a possible filling error of the bending oscillator.
    [2]
    2. The method according to claim 1, characterized in that the measurement of the viscosity and the quality is performed independently, but in particular simultaneously, with different or independent measuring instruments.
    [3]
    3. The method according to claim 1 or 2, characterized in that based on the Justierkurve or adjustment table is checked to what extent is predetermined by those of them on the Justierkurve or their in the calibration table determined function values and, if this deviation is exceeded, for the presence of Füllfehlers, in particular Presence of bubbles or inhomogeneities in the measuring fluid is detected.
    [4]
    4. The method according to any one of claims 1 to 3, characterized in that - the adjustment curve is determined with standards of known viscosity and / or density, and / or - that in particular linear areas of the relationship are calculated by simulation, or - that a predetermined table of values for Is held available.
    [5]
    5. The method according to any one of claims 1 to 4, characterized in that the measured values for the viscosity and the quality and / or attenuation of the bending oscillator associated evaluation are supplied, in which optionally the Justierkurven and / or the adjustment table stored or stored.
    [6]
    A method according to any one of claims 1 to 5, characterized in that the adjustment curve or adjustment table is in the form of a predetermined functional relationship between the viscosity values and the quality values, attenuation values or density error values, e.g. a square root context, be created or made available.
    [7]
    7. The method according to any one of claims 1 to 6, characterized in that for determining the quality and / or the damping of the bending oscillator values for the fundamental and / or at least one harmonic are used.
    [8]
    Method according to one of claims 1 to 7, characterized in that a tolerance band for the values lying on the adjustment curve or in the adjustment table is determined and checked by multiple measurements, if the values of the measurement fluid for the damping and / or quality and / or viscosity are functionally assigned values are within the tolerance band and, if appropriate, recognized on a proper filling.
    [9]
    A method according to any one of claims 1 to 8, characterized in that - density and / or viscosity adjustment measurements are made on a variety of standards to determine an error interval for each function value of the adjustment curve or value of the adjustment table, respectively; the value resulting from the measurement of the measurement fluid is checked as to whether it lies within the tolerance band defined thereby.
    [10]
    10. The method according to any one of claims 1 to 9, characterized in that derrein statistical Z-value is used for the verification of the tolerance band.
    [11]
    A method according to any one of claims 1 to 10, characterized in that by using the Z-value a sample value is taken from a sample and it is calculated how many standard deviations the sample value is above or below the mean value, wherein when the calibration curve or -tabeile also the standard deviation of the individual measuring points is determined.
    [12]
    12. Method according to one of claims 1 to 11, characterized in that the adjustment of the adjustment curves and / or the adjustment tables with different density and viscosity standards is carried out and as a result a direct adjustment function or adjustment table is obtained which determines the density error of the bending oscillator with the viscosity in sets a functional relationship, wherein a density correction value Kd is calculated from the measurement of the attenuation or a quantity derived therefrom.
    [13]
    Method according to one of claims 1 to 12, characterized in that - an adjustment curve or parts is determined with different density and viscosity standards, which relates the density error of the bending oscillator with the viscosity, - that a density correction value (Kd) from the attenuation or quality is determined, - that a density correction value (Kv) is determined from the value measured with the viscometer, and - that the values Kd, determined from the adjustment function of the damping of a natural vibration and the correction values (Kv), are compared with one another.
    [14]
    14. Device for determining the filling quality of the oscillator tube through which the measuring fluid flows, in particular for carrying out the method according to one of claims 1 to 13, characterized in that - the device has a measuring unit in the form of a bending oscillator 11 which determines the viscosity-dependent density value of the measuring fluid flowing through the oscillator tube, the device additionally has a unit for determining the values of the dynamic viscosity of the measuring fluid, that these two measuring units are connected to an evaluation unit which determines the viscosity-dependent density values from the quality and / or attenuation of the oscillating tube of the flexible oscillator, and the evaluation unit determines an adjustment curve or -tabeile contains which Justierkurveoder- tabeile the previously determined functional relationship between a decisive for the quality or damping of the bending oscillator parameters and the dynamic viscosity of the Me ssfluids contains or reproduces.
    [15]
    A flexural vibrator according to claim 13 or 14, characterized in that the comparator is formed by a distance measuring unit which determines the distance between the measured values and / or the distance of the measured values from the adjusting curve or from the functional values contained in the adjusting table.
    15. Bending oscillator according to claim 14, characterized in that - the evaluation unit has a comparison unit for the measured values or values, which were determined on the one hand for the dynamic viscosity and on the other hand for the quality and / or damping of the bending oscillator.
    [16]
    16 bending vibrator according to one of claims 13 to 15, characterized in that the comparison unit, a display unit for the comparison result and / or for the degree of agreement or the distance between the on the Justierkurvebzw. in the adjustment table for the viscosity values of the values obtained for the quality and / or attenuation and lying on the adjustment curve or in the adjustment table is connected.
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    同族专利:
    公开号 | 公开日
    CN105628550A|2016-06-01|
    AT516302B1|2016-06-15|
    EP3006916A1|2016-04-13|
    CN105628550B|2019-10-01|
    US20160103053A1|2016-04-14|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ATA50726/2014A|AT516302B1|2014-10-10|2014-10-10|Method and device for determining the filling quality of a bending vibrator|ATA50726/2014A| AT516302B1|2014-10-10|2014-10-10|Method and device for determining the filling quality of a bending vibrator|
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