The present invention relates a method and apparatus for analysis of a dielectric medium.
In certain realisations the method and apparatus is for capacitance measurement in a dielectric medium, and in particular to such a system in which correction for polarisation error at measurement electrodes can be made.
Capacitance measurement techniques are known for measuring the capacitance (or specific capacitance or dielectric constant) of liquids and suspensions, such as biological cells in ionic aqueous solutions. Known techniques involve introducing metal electrodes into the liquid and applying an excitation signal (usually sinusoidal) and measuring voltage and current using a pair of measurement electrodes. The impedance, conductivity and specific capacitance can then be calculated. At high excitation frequencies (greater than about 1 MHz) this is relatively straightforward with simple electrode and circuit configurations. However at lower frequencies, and particularly where the conductivity is high (up to 100 mS/cm or so), the electrode—liquid interface exhibits an impedance which appears in series with the impedance of interest and distorts the measurements.
EP1018025 discloses such a technique for measurement of biomass. This document describes the background to the Beta dispersion and how correction needs to be made for polarisation at measurement electrodes.
Electrode polarisation effects result largely from the charged electrodes attracting around themselves a counter layer of ions which acts electrically as a capacitor/resistor network in series with the biomass suspension that is under measurement investigation. The magnitude of the electrode polarisation effect is largely frequency dependent. Unfortunately to be on the plateau of the Beta dispersion for meaningful biomass measurement requires the use of a frequency region in which polarisation of the measuring electrodes can contribute a significant capacitance which has a material distortion on the measured capacitance. This error also varies with time as the electrode surface impedance is not stable and depends upon electrode surface current density.
In a known prior art arrangement (shown in
A further technique for dealing with the electrode polarisation capacitance error is to estimate the error from the shape of the capacitance Vs frequency curve and then subtract the error from the measured values. This technique is described in EP 1018025. This technique is possible because, at the lower end of the frequency range used for biological samples, the cell-suspension capacitance is usually relatively flat against frequency (plateau region) whereas the Electrode capacitance increases steeply as the frequency reduces. Whilst this technique works effectively in many circumstances, there are situations in which it is difficult to make an accurate estimate of the polarisation capacitance which is totally independent of the biomass characteristics.
There are other techniques for attempting to deal with the electrode polarisation error. Some of these are suitable for laboratory implementation but for various reasons not practicable for industrial on-line measurement. Electrode coatings designed to reduce the surface impedance can be effective but often do not have sufficiently long life effectiveness for typical operating conditions. Other methods such as variable geometry electrodes and differential methods using a reference electrode also have drawbacks, particularly for industrial on-line applications.
An improved technique and apparatus has now been devised.
According to a first aspect, the present invention provides a method for analysing a dielectric test medium, the method comprising:
In one embodiment, the second couple of electrodes may comprise one of the excitation electrodes and a sensing electrode. In such an embodiment, it is preferred that one of the excitation electrodes has a surface area significantly larger than the other of the excitation electrode couple. Beneficially, the larger surface excitation electrode comprises the excitation electrode in the second couple of electrodes. By significantly larger it is means that the surface area of the larger surface excitation electrode is at least 2× (more preferably at least 5×, most preferably at least 10×) the surface area of the smaller surface area electrode.
In an alternative embodiment, separate respective couples of excitation electrodes and sensing electrodes are provided, the voltage being measured across the excitation electrode couple and the sensing electrode couple and compared in order to derive a polarisation correction factor. In this embodiment, the sensing electrodes comprise first and second sensing electrodes, neither being an excitation electrode.
A first couple of electrodes comprise first and second sensing electrodes (for example a pair of electrodes); and a second couple of electrodes comprise first and second excitation electrodes for applying the excitation current to the test medium, and the measured voltages across the excitation electrodes and the sensing electrodes are compared in order to derive a polarisation correction factor.
In one realisation of the invention, the voltage is therefore measured across the excitation electrodes in addition to being measured across the second electrode couple (for example the separate pair of sensing electrodes).
In one realisation of the invention, one couple of electrodes may comprise first and second sensing electrodes; and an alternate couple of electrodes may comprise first and second excitation electrodes for applying the excitation current to the test medium, and the measured voltages across the excitation electrodes and the sensing electrodes are compared in order to derive a polarisation correction factor.
Beneficially the measured voltages are used to derive a measure of the capacitance of the medium (typically using a capacitance value corrected for by the polarisation correction factor).
The voltages are complex values having phase components. The measured voltages between the first and second electrode couples are compared to reveal the out-of-phase component between them, which is then used to derive the polarisation correction factor.
Beneficially the quadrature component of the measured voltages of the electrode couples are compared to derive the polarisation correction factor.
It is preferred that the comparison comprises derivation of a ratio of measured values.
Beneficially the correction factor is applied to correct a value calculated from the measured voltage across one of the couples of electrodes.
In a preferred realisation, one couple of electrodes comprise first and second sensing electrodes; and another couple of electrodes comprise first and second excitation electrodes for applying the test current to the test medium; the correction factor being applied to correct a value calculated from the measured voltage across the sensing electrodes.
It is preferred that the voltage across one or both of the electrode couples is measured using a high impedance device such that there is negligible current flow (preferably less than 1 uA) across one or both of the electrode couples. This minimises the effect of the polarisation at the electrode surface.
Beneficially, the correction factor derived is used to provide a corrected value for capacitance, or conductivity.
In a preferred realisation, the test medium may be a biomass medium.
According to a further aspect, the present invention provides apparatus for analysis of a dielectric test medium, the apparatus comprising:
As described in relation to the first aspect, in one embodiment, one couple of electrodes may comprise first and second sensing electrodes; and the other couple of electrodes may comprise first and second excitation electrodes for applying the excitation current to the test medium, and the measured voltages across the excitation electrodes and the sensing electrodes may be compared in order to derive a polarisation correction factor.
In an alternative embodiment the first couple of electrodes may comprise an excitation electrode couple (preferably comprising first and second respective excitation electrodes). In this embodiment the second electrode couple comprises one of the excitation electrodes and a sensing electrode. Beneficially, one of the excitation electrodes has a surface area significantly larger than the other of the excitation electrode couple. The larger surface excitation electrode comprises the excitation electrode in the second couple of electrodes.
Referring to the drawings, and particularly
The two outer electrodes 23,24 are used to drive current through the sample, whilst the two inner electrodes 25,26 are used to detect the potential drop (v) across the suspension between the inner electrodes 25,26. The potential is detected with a high impedance differential amplifier 27, such that there is virtually no current flowing across the inner electrodes 25, 26 electrode/solution interfaces. So far this is the same as with respect to the prior art configuration of
At high excitation frequencies (greater than one to a few MHz) the voltage between the excitation electrode pair 23, 24 and the voltage between the voltage sensing pair 25, 26, can be related by a simple scalar constant which would depend upon the electrode geometry. This is because at the high excitation frequencies, the impedance of the suspension/electrode interface is negligibly small compared to that of the liquid or suspension. This scalar relationship is independent of the conductivity and permittivity of the liquid or suspension being measured. This is because it is determined by the ratio of impedances with identical phase versus frequency properties.
However at lower measuring frequencies, where the impedance of the suspension/electrode interface is not negligibly small compared to that of the liquid or suspension, voltage relationship departs from the high frequency value and becomes a complex quantity. Using the electrode arrangement of the invention as shown in
The correction is derived at the same frequency as the specific capacitance or conductivity is measured, not extrapolated from a lower frequency measurement as is the case in respect of prior art techniques. This provides an improvement over prior art techniques.
The measured value of the voltages can readily be converted to values of conductivity or capacitance by means of known algorithms running on conventional processors or computer software.
Therefore, the output of amplifier 28 is fed via an integrator circuit 31 (to introduce a 90 degree phase shift) to a phase sensitive detector 32. The reference for the phase sensitive detector is taken from the output from the differential amplifier 27 measuring the excitation voltage. The output from the phase sensitive detector is passed via a low-pass filter 33 to a processor unit 34 which processes the signal to derive a value for the capacitance error due to the electrode polarisation layer. The function applied by the processor can be a linear function related to gain and offset, although more complex functions may be derived and utilised. The capacitance error is then subtracted from the measured capacitance to give the corrected capacitance.
In an alternative technique in accordance with the invention a three electrode system may be used.
As shown in
In this embodiment a second electrode couple is formed by the large surface area excitation electrode 44 and the sensing electrode 45. This electrode couple is used to detect the potential drop (v) across the suspension between the inner electrodes 44 and 45. The potential is detected with a high impedance differential amplifier 47, such that there is virtually no current flowing.
In this embodiment, because of the large surface area of the excitation electrode 44, (with respect to the excitation electrode 43) the impedance of the electrode 44 (including the contribution due to surface polarisation) is negligible compared to that of the other excitation electrode, and that of the test medium. As a result the voltage will be extremely close to that of the test medium adjacent the large electrode 44. The consequence of this is that, for practical purposes, the large electrode 44 can be used both as an excitation electrode and a sensing electrode. The signals are processed in the same manner as with respect to the earlier described embodiment.
Number | Date | Country | Kind |
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1011474.2 | Jul 2010 | GB | national |