Evaluation of a Novel Tubular Sample Holder for Dielectric Measurements with Abdulnour’s Method André Rotavaa, Luiz E. P. Borgesb, Maurício H. C. Diasa, José C. A. Santosa a b Electrical Engineering Department Chemical Engineering Department Military Institute of Engineering – IME Rio de Janeiro, Brazil {rotava, luiz, mhcdias, araujo}@ime.eb.br Abstract—This paper assesses the accuracy of a rectangular waveguide pierced by a tubular load sample holder for measuring liquid materials at high temperatures with a formulation based on Abdulnour’s method. The measurement technique is derived from the transmission line method. The sample holder is adapted from a section of a rectangular waveguide pierced by a tubular load for high temperature measurements at 2.45 GHz. Simulations of the loaded sample holder are carried out with CST Microwave Studio® for several values of sample permittivity. The accuracy of the technique is evaluated by comparing these values to those obtained from Abdulnour’s extraction model. It is shown that by properly choosing a set of calibration standards the technique can be quite accurate. Keywords— permittivity measurements; high temperature measurements; transmission line method; Abdulnour’s method I. INTRODUCTION during measurements. However, it was found that it is not fully compliant with measurements at the frequency range of interest, i.e., at low microwave spectrum, due dimensional problems. Related to that, there come all the difficulties of measuring liquid materials with this technique, particularly, but not exclusively, at very high temperatures. The traditional transmission line method is not appropriate for the purposes of this work, both for measuring liquid materials, and for measuring materials at high temperatures. In order to overcome these problems, different types of sample holders and techniques were investigated. In this context, a variant of the transmission line method developed by Abdulnour et al. [2] which uses a double layered cylindrical sample holder confined in a rectangular waveguide was of interest. Although their apparatus is not adequate for high temperature measurements, their formulation is quite simple and has been shown to be very precise. Measuring dielectric properties of liquid materials at high temperatures poses a series of challenges. Although the fundamentals of any permittivity measurement method can be applied, many technical issues arise from their effective use at very high temperatures, i.e., temperatures well above room temperature. Thermal isolation between material under test (MUT) and measuring setup, heat dissipation, thermal expansion, and temperature monitoring are just some of them. The sample holder introduced by Nishikata [3] brought more flexibility to the measurement system. His apparatus propitiates easy handling of the sample, especially for liquid materials, and has a considerable potential for high temperature applications. In fact, with some slight modifications, considering thermal isolation between sample and measuring setup, and proper heat dissipation, this sample holder can be used for the purposes of the current work. At the Military Institute of Engineer (IME), a recent work lead by the Microwave Group has dealt with this kind of measurements. The main interest was on high temperature permittivity measurements of liquid materials at a frequency range around 2.45 GHz. As part of this effort, an evaluation of the coaxial probe method has been performed [1]. In this context, some national oil samples were measured at temperatures up to 180°C. One of the greatest difficulties in dielectric measurements when a discontinuity in a transmission line is present is to solve the inverse problem, i.e., to extract the dielectric permittivity of the MUT from the measured S-parameters of the sample holder. So far, a number of approaches have been proposed [2][3][4][5]. The problems with these techniques lie in their intrinsic complexity, the relatively long CPU time for their computation, and various convergence difficulties for some of them. The coaxial probe method is known to be very appropriate for measuring liquid materials. However, since the probe must be in direct contact with the sample, measurements are limited to temperatures dictated by the probe, which usually are not too high. The free space method has also been investigated for the purposes of this work. The great advantage of this method is that the MUT does not make contact with the measuring setup In this paper we investigate if the approximate analytical formulation derived in [2] would still be valid for a sample holder similar to that presented in [3]. Section II presents the fundamental concepts of Abdulnour’s method. Section III describes the tubular sample holder in use. Section IV explains the methodology to assess the accuracy of the modified sample holder with Abdulnour’s formulation. Section V presents some significant results of this evaluation. And Section VI concludes the work. II. ABDULNOUR’S METHOD The measurement technique described in [2] is based on the scattering analysis of a cylindrical sample inserted in a rectangular waveguide. The sample can be confined in a dielectric cylindrical tube, as shown in Fig. 1. For the sample holder in question, it is not possible to obtain a complete analytical solution for extracting the permittivity of the MUT (εMUT). On the other hand, the direct problem, which consists of determining the S parameters of the tubular structure, given the permittivities of the tube and of the MUT, can be analytically formulated and numerically solved. In [2], a combination of the boundary integral equation technique with a modal expansion approach is used to specifically equate the direct problem. Fig. 2. Typical diagram of S21 as a function of the relative permittivity of the MUT. It must be emphasized that the extraction model proposed in [2] is not a proper analytical solution for the problem, but an approximation. Even though, in general, it allows reproducing the actual response with great precision. Abdulnour et al. [2] state that for waveguides with a useful frequency range between 8 and 26 GHz, if 1.2 < f ⁄ fc < 1.8, where fc is the waveguide cutoff frequency, and D1 < a ⁄ 5, the method’s approximation error is always better than 1%. III. Fig. 1. Top (a) and front (b) view of a rectancular waveguide with a dielectric tube containing a sample of material under test. Fig. 2 shows a typical diagram of the forward scattering parameter S21 obtained from the solution of the direct problem for various values of the relative permittivity of the MUT. It is found that the geometrical locations of the real and imaginary parts of εMUT (ε′MUT and ε″MUT, respectively) resemble circular arches in the complex plane of S21. In this example, the sample holder is composed of a WR90 waveguide section (a = 22.86 mm, b = 11.43 mm), and the tube has relative permittivity εt = 4.5, inner diameter D1 = 1.08 mm, and outer diameter D2 = 1.732 mm. The analysis frequency is f = 8 GHz. A detailed geometrical analysis of the diagram of Fig. 2 allows one to deduce simple analytical equations that express ε′MUT and ε″MUT directly as a function of the S21 parameter of the cylindrical obstacle [2]. These equations constitute an approximate analytical solution for the inverse problem, i.e., for directly extracting the relative permittivity of the MUT from the sample’s scattering parameters. In Abdulnour’s technique, at least three solutions to the direct problem must be known for computing the unknown parameters of its extraction model. In a traditional calibration procedure, one’s would need three standards, or materials, whose permittivities are known beforehand. THE TUBULAR SAMPLE HOLDER DEFINITION In Abdulnour’s method, the sample is completely confined within the waveguide. This leads to a series of practical difficulties for adapting this technique to high temperature measurements. Besides the problem of heating the sample without affecting the measurement setup, it would be necessary to disconnect the sample holder from the setup to load, unload, or replace the sample. This would substantially increase measurement errors. A similar solution, but with a few improvements to the previous sample holder, was presented in [3]. The cylindrical sample is made to pierce through the center of the wider walls of the rectangular waveguide, without making contact with them. To avoid escaping microwave energy, the holes at the waveguide walls are followed by metallic sleeves, or chimneys, which in practice act as circular waveguides with cutoff frequency well above the effective bandwidth of the rectangular waveguide. Fig. 3 shows a sketch of the described sample holder. The tubular load is composed by a cylindrical tube of linear, isotropic, and homogeneous dielectric material, entirely filled with the material under test. Fig. 3. Rectangular waveguide pierced by tubular load. The main advantage of this sample holder is that one can load, unload, or replace the MUT through the holes without disconnecting the waveguide joints. In the analysis performed in [3], the S parameters of the sample holder are rigorously formulated in terms of the modal scattering coefficients of the cylindrical object, a complex and costly solution. The dimensions that specify the sample holder of Fig. 3 are shown in Fig. 4: a, b and L are the width, height and length of the rectangular waveguide; HC and DC are the internal height and internal diameter of the chimneys; D1 and D2 are the internal and external diameters of the dielectric tube, respectively. The structure is symmetric, i.e., the tubular load is centered at the waveguide. The thickness of the waveguide walls and the extensions of the tubular load outside the chimneys do not interfere with the electromagnetic response of the device. remaining values of S21 to extract the corresponding relative permittivity of the MUT (εo). This process is illustrated in Fig. 5. Comparing the input and output permittivities, we can check if Abdulnour’s formulation can reproduce the response of the sample holder’s model. The errors are expressed in three forms: ET = ε o − ε i ε i • Real part error: E R = (ε o′ − ε i′ ) ε i′ • Imaginary part error: E I = (ε o′′ − ε i′′) ε i′′ • Total error: Fig. 5. Methodology of evaluation. Fig. 4. Dimensions for specifing the sample holder. Since the sample holder is meant to be used in a frequency band around 2.45 GHz, it was built upon a WR340 waveguide standard, with dimensions a = 86.36 mm and b = 43.18 mm. The effective bandwidth of this waveguide goes from 2.2 to 3.3 GHz. Additional modifications were made to allow precise positioning of the dielectric tube and thermal isolation from the measurement setup that do not affect the electromagnetic behavior of the measurement system. IV. METHODOLOGY The primary objective of this work is to use Abdulnour’s method with the modified sample holder. For this to be possible, the accuracy of the method must be assessed. The idea behind this is to evaluate how Abdulnour’s extraction model reproduces the actual relation between the MUT’s permittivity and the tubular load S parameters. So, to reach that objective, the following methodology is adopted. Firstly, we obtain, with CST Microwave Studio® [6], the sample’s S21 parameters relative to a large set of relative permittivity values of the MUT (εi), in a given frequency. Then, with Matlab®, we arbitrarily pick three of these solutions to determine the coefficients of the model equation proposed in [2]. Also in Matlab®, that equation is applied to the The results are organized in graphical format, according to some error intervals, on a complex Cartesian plane. In the following figures, the crosses indicate de tubular load’s S21 parameter obtained from CST, and the small black circles indicate the three points used for determining Abdulnour’s extraction model. The blue arches represent the calculated model, by mapping constant ε′MUT and constant ε″MUT values into the complex plane of S21. The precision for each simulation point is indicated by the color of the cross, according to the following legend: • Lilac → ER < 1% and EI < 1%; • Red → ER > 1% or EI > 1% and ER < 5% and EI < 5%; • Green → ER > 5% or EI > 5%. V. RESULTS A. Single Frequency Evaluation Fig. 6 shows the evaluation of the sample holder described in Section III. The first observation about this figure is that the extraction model does not agree equally with the sample holder response for all values of MUT’s relative permittivity. In this example, the simulation was at f = 2.5 GHz; with (typical value for laboratorial glass); L = 100 mm; D1 = 10 mm; D2 = 12 mm; HC = 25 mm; DC = 14 mm; ε′i = 1, 3, 5...21; and ε″i = 0, 2, 4...20. The three MUT relative permittivity values used for computing the extraction model coefficient are ε1 = 1, ε2 = 1 – j20 and ε3 = 21. εt = 4.6 – j0.017 B. Swept Frequency Evaluation Fig. 7(d) shows the evaluation of the same sample holder at 2.5 GHz, with ε1 = 21 – j20, ε2 = 9 – j20 and ε3 = 15 – j10. Fig. 8 repeats the analysis for the frequencies of 2 and 3 GHz. It is noticed that the region of error below 1% changes when the frequency sweeps from 2 to 3 GHz. Fig. 6. Precision evaluation of the sample holder at 2.5 GHz.. At first, depending on the expected permittivity value for the MUT, Fig. 6 may indicate that Abdulnour’s modeling is not adequate for representing the sample holder in question. However, by changing the three points that determine the extraction model, the precision of the method can change substantially. This is shown in Fig. 7. It can be noticed that it is possible to generate an adequate extraction model for different ranges of MUT permittivities by properly choosing the calibration standards for the extraction model. Although this may restrict the use of the technique for measuring a broad range of arbitrary materials, this limitation may be overcome in the case of high temperature measurements. In fact, the extraction model can be tuned for a specific material by using its low temperature permittivity as reference. As this case shows, the precision of the extraction model is not maintained when the frequency of analysis is changed, if the three calibration permittivity values are kept constant. In other words, if at a certain frequency of analysis one specific trio of permittivities generates a model with good precision for a given interval of εMUT, this will not be guaranteed for other frequencies. If a certain precision level is required for a broad band of frequencies, the choice of the calibration standards for the sample holder must be subject to further analysis. C. A Case Study for Methanol One way to ascertain if the choice of ε1, ε2 and ε3 is adequate for the interval of εMUT of interest is through simulation. Fig. 9 shows the simulation of a measurement with methanol, in which were used ε1 = 21 – j20, ε2 = 9 – j20 e ε3 = 15 – j10. In the figure, the red curves represent the methanol’s theoretical relative permittivity and the blue ones represent the approximate response from the extraction model. (a) (b) (c) (d) Fig. 7. Precision evaluation of the sample holder at 2.5 GHz by switching the points for calculating the extraction equation coeficients (a) ε1 = 1, ε2 = 3 – j4 and ε3 = 5 – j6, (b) ε1 = 1 – j10, ε2 = 1 – j14 and ε3 = 5 – j20, (c) ε1 = 21, ε2 = 15 and ε3 = 21 – j6, (d) ε1 = 21 – j20, ε2 = 9 – j20 and ε3 = 15 – j10. In this example, it is noticed that the approximation was good along the entire frequency band of interest, which validates the choice of ε1, ε2 e ε3 for calibrating the sample holder in this case. VI. CONCLUSION In this work, an alternative approach for permittivity measurements of liquid materials with a tubular sample holder was evaluated. (a) Abdulnour’s method [2] was used. Although it was developed for the analysis of a sample holder that is not suitable for high temperature measurements, it comprises a very simple solution for the reverse problem, i.e., for computing MUT permittivity from measured S parameters. We investigated if Abdulnour’s extraction model could be applied to a sample holder made of a cylindrical sample piercing through the walls of a rectangular waveguide, with a WR340 standard. The sample holder was thoroughly simulated for various values of sample permittivity. The approximation errors were computed for each point of simulation. The results were represented in a graphical format. (b) Fig. 8. Precision evaluation of the sample holder changing the simulation frequency from (a) 2 GHz to (b) 3 GHz. It was found that by properly choosing calibration standards it’s possible to apply Abdulnour’s extraction model to the proposed tubular sample holder with good accuracy. ACKNOWLEDGMENT The authors would like to thank Petrobras for the financial funding to this work. REFERENCES [1] [2] (a) [3] [4] [5] (b) [6] Fig. 9. Simulation of measurement of (a) real and (b) imaginary parts of the relative permittivity of methanol. Santos, J. C. A., Dias, M. H. C., Aguiar, A. P., Borges, I., e Borges, L. E. P. Using the coaxial probe method for permittivity measurements of liquids at high temperatures. Journal of Microwaves and Optoelectronics, v. 8, p. 78S-91S, 2009. Abdulnour, J., Akyel, C., e Wu, K. 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