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18th International Symposium on the Application of Laser and Imaging Techniques to Fluid MechanicsLISBON | PORTUGAL JULY 4 – 7, 2016 Investigation of a self-calibration method for global rainbow refractometry Kailin Cao 1 , Xuecheng Wu 1,* , Haoyu Jiang 1 , Yingchun Wu 1, 2 , Can Li 1 , Kefa Cen 1 , and Gerard Grehan 2 1: State Key Lab of Clean Energy Utilization, Zhejiang University, Hangzhou 310027, China 2: UMR 6614/CORIA, CNRS, BP12 76801 Saint Etienne du Rouvray, France * Correspondent author: [email protected] Keywords: Global rainbow refractometry, Self-calibration, Scattering angle, Dual-wavelength laser ABSTRACT Accurate measurement and control of key parameters of droplets in the complex atomization or spray flow field play an instructive role in the mechanism study of multiphase flows and optimization of specific industrial process. Among numerous advanced optical measurement techniques for characterizing droplets, global rainbow refractometry is able to measure the size distribution and refractive index of droplets simultaneously. Temperature, concentration, solution components and any other relevant parameter can be determined according to the relationship between refractive index and target parameter. Since the information of refractive index and droplet size contained in the rainbow intensity distribution is highly sensitive to the scattering angle, accuracy of calibration for the relationship between CCD pixel column and scattering angle greatly affects the measurement accuracy. A novel self-calibrated global rainbow refractometry based on dual-wavelength laser is proposed in this paper. The angular calibration and the refractive index measurement under two wavelengths can be realised simultaneously without additional measure devices. The actual refractive indices of droplets under two wavelengths and calibration equation can be quickly and simultaneously obtained by searching the minimum of root mean square (RMS) errors between the hypothesizing refractive indices and the ones from inversion. The results of simulation and experiment show the feasibility and high precision of self calibration method for global refractometry. This self-calibrated global rainbow system was also successfully applied to measure the refractive index of water–ethanol solutions with volume concentration from 10% to 60%. What’s more, this design can be extended to calibration for one-dimensional rainbow technique. 1. Introduction Liquid atomization and spray has a broad range of applications in the energy, chemical and many other industrial fields. Accurate measurement and control of key parameters of droplets in the complex atomization or spray flow field play an instructive role in the mechanism study of multiphase flows and optimization of specific industrial process. Among numerous advanced optical measurement techniques for characterizing droplets, global rainbow refractometry (Van Beeck and Giannoulis, 1999) has been shown to be a powerful tool for its advantages in simultaneously measuring the size distribution and refractive index for both individual droplets,
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  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    Investigation of a self-calibration method for global rainbow refractometry

    Kailin Cao1, Xuecheng Wu1,*, Haoyu Jiang1, Yingchun Wu1, 2, Can Li1, Kefa Cen1, and Gerard Grehan2

    1: State Key Lab of Clean Energy Utilization, Zhejiang University, Hangzhou 310027, China 2: UMR 6614/CORIA, CNRS, BP12 76801 Saint Etienne du Rouvray, France

    * Correspondent author: [email protected]

    Keywords: Global rainbow refractometry, Self-calibration, Scattering angle, Dual-wavelength laser

    ABSTRACT

    Accurate measurement and control of key parameters of droplets in the complex atomization or spray flow field play an instructive role in the mechanism study of multiphase flows and optimization of specific industrial process. Among numerous advanced optical measurement techniques for characterizing droplets, global rainbow refractometry is able to measure the size distribution and refractive index of droplets simultaneously. Temperature, concentration, solution components and any other relevant parameter can be determined according to the relationship between refractive index and target parameter. Since the information of refractive index and droplet size contained in the rainbow intensity distribution is highly sensitive to the scattering angle, accuracy of calibration for the relationship between CCD pixel column and scattering angle greatly affects the measurement accuracy. A novel self-calibrated global rainbow refractometry based on dual-wavelength laser is proposed in this paper. The angular calibration and the refractive index measurement under two wavelengths can be realised simultaneously without additional measure devices. The actual refractive indices of droplets under two wavelengths and calibration equation can be quickly and simultaneously obtained by searching the minimum of root mean square (RMS) errors between the hypothesizing refractive indices and the ones from inversion. The results of simulation and experiment show the feasibility and high precision of self calibration method for global refractometry. This self-calibrated global rainbow system was also successfully applied to measure the refractive index of water–ethanol solutions with volume concentration from 10% to 60%. What’s more, this design can be extended to calibration for one-dimensional rainbow technique.

    1. Introduction Liquid atomization and spray has a broad range of applications in the energy, chemical and many other industrial fields. Accurate measurement and control of key parameters of droplets in the complex atomization or spray flow field play an instructive role in the mechanism study of multiphase flows and optimization of specific industrial process. Among numerous advanced optical measurement techniques for characterizing droplets, global rainbow refractometry (Van Beeck and Giannoulis, 1999) has been shown to be a powerful tool for its advantages in simultaneously measuring the size distribution and refractive index for both individual droplets,

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    and spray of polydispersed droplets. Temperature (Hom and Chigier, 2002), concentration (Wu and Wu, 2012), solution components (Zhao and Qiu, 2006) and any other characterization parameter can be determined according to the relationship between refractive index and target parameters. By analyzing the distribution of scattered light around the primary rainbow angle, rainbow technique extracts the absolute angular location and the shape of the rainbow pattern, which can be used to inverse the refractive index and the droplet size respectively. Standard rainbow technique (Roth and Anders, 1991) was firstly presented to measure a spherical single droplet or individual monodispersed droplets in a line. Later, the standard rainbow technique was progressed to the global rainbow technique (Van Beeck and Giannoulis, 1999) for measuring spray droplets. Global rainbow technique requires larger size of the pinhole and longer exposure time of the CCD camera to get superposition of rainbows from numerous droplets that are illuminated by laser. This superposition of rainbows avoids the effects of the non-sphericity of the droplets and eliminates the high-frequency component of the rainbow signals to obtain a steady and smooth rainbow structure. Recently, a one-dimensional rainbow technique (ORT-1) (Wu and Jiang, 2014) was proposed that extended a point volume measurement to a one-dimensional segment measurement by using slit apertures. Then, an alternative optical design of one-dimensional rainbow technique (ORT-2) (Wu and Promvongsa, 2015) was developed. ORT-2 aims to facilitate the angular calibration in the full image field by using Fourier domain filtering. Since the information of refractive index and droplet size contained in the rainbow intensity distribution is highly sensitive to the scattering angle, precise calibration of the relationship between CCD pixel column (pix) and scattering angle (θ) is the key part to guarantee the measurement accuracy. Acquiring global rainbow images on a set of sprays of known temperature is one of the calibration methods (Lemaitre and Porcheron, 2006). This method is susceptible to environmental perturbations, such as temperature change. The most conventional calibration process is completed by using a mirror mounted on the rotation platform (Vetrano and Gauthier, 2006), which we call as the mirror calibration method. However, errors caused by manual operation and additional precise instrument of mirror calibration method is unavoidable. When it comes to harsh industrial environments such as spray in a container, calibration for the mirror inaccessible occasions is a challenge. To solve the problem, we propose a self-calibration method based on dual-wavelength lasers for global rainbow refractometry. This method enables us to calibrate the scattering angle along with the refractive index measurement under two wavelengths illuminations.

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    2. Numerical and Experimental Methods As the material’s natural property, the refractive index changes with the wavelength of the light when other conditions keep the same. With the increase of the wavelength of the light, refractive index of common liquid is decreased, such as water and alcohol. For spray droplets illuminated by two different wavelengths of laser beams that are modulated into a coincident one, two rainbow patterns of different wavelengths can be obtained on method of appropriate signal separation. Obviously, these two rainbows correspond to the same particle size distribution and the same temperature. If the equation for the refractive index as a function of wavelength and temperature is known in advance, according to coupling relationship of refractive index between this pair of rainbows, both the calibration equation and the droplets temperature (T) might be yielded simultaneously. In this study, two vertically placed lasers of different wavelengths (e.g. λ1= 532 nm, λ2= 633 nm) are modulated to get one coincident laser beam by using a beam splitter, as shown in Fig. 1. The coincident laser beam horizontally illuminates the spray with unknown temperature.

    Fig. 1. Optical setup for the self-calibrated global rainbow refractometry.

    Two spherical lenses, one aperture and a color CCD form the imaging system for self-calibrated global rainbow refractometry. Instead of using a black-white CCD sensor to record monochromatic rainbow signals in classical global rainbow system, here a color CCD sensor is applied to record dual-wavelength scattered light signals. The mixed signals can be separated in red, green, and blue channels, so two global rainbow curves of two wavelengths can be extracted

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    respectively from the Green and Red channel, as the simulated global rainbow curves shown in Fig. 2(a). The global rainbow curves are simulated based on the Lorenz–Mie theory. The pixels corresponding to the geometric rainbow angles (pix1, pix2) can be determined by the angles where the normalized scattering light intensities reach a value of RI (RI = Irg /IMAX) before the primary rainbow maximum. Irg is the scattered light intensity corresponding to the geometric rainbow angle. IMAX is the scattered light intensity that reaches the maximum. The geometric rainbow angle, θrg only depends on the refractive index (n) that varies with the wavelength of light, as given by Eq. (1) (Hulst and Van De Hulst, 1957).

    2 21 1

    2

    4 44sin 2sin3 3rgn nn

    θ π − −− −

    = − + (1)

    As the equation for the refractive index of spray as a function of wavelength and temperature should be known in advance, here we choose deionized water whose physical characteristics have been fully studied, as given by Eq. (1) (Quan and Fry, 1995).

    6 2 1 2 6 3( , ) 1.31405 2.02 10 (15.868 0.00423 ) 4382 1.1455 10n T T Tλ λ λ λ− − − −= − × + − − + × (2)

    When the spray temperature (T) has been hypothesized, the refractive indices of calibration medium under two wavelengths (n1, n2) can be determined by Eq. (2), and geometric rainbow angles can be calculated by Eq. (1). In Fig. 2(a), pix1 and pix2 correspond to θrg1 and θrg2 respectively.

    Fig. 2. Simulated global rainbow curves under two wavelengths

    Since the calibrated angle-pixel relationship presents good linearity between the scattering angle θ and the CCD pixel, the calibration equation is usually obtained by linear fitting (θ = a + b × pix)

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    and has been shown to ensure the accuracy. By both hypothesizing the value of RI and spray temperature T, two characteristic calibration point (pix1, θrg1) and (pix2, θrg2) can be used to obtain a and b, the characterizing parameters of linear calibration equation. Then we get the dual-wavelength distributions of intensity on scattering angle, as shown in Fig. 2(b). These distributions are used for the rainbow signal processing to inverse the refractive indices (m1, m2) by using an inversion algorithm based on the modified Nussenzveig’s theory (Saengkaew and Charinpanikul, 2010). By using the non-negative least-squares algorithm, the refractive indices (m1, m2) and size distribution are inversed respectively by solving the equations, as given by Eq. (3) and Eq. (4).

    11 1( ) ( , , ) ( )I T m d D dθ θ= (3)

    22 2( ) ( , , ) ( )I T m d D dθ θ= (4)

    The intensity vector I is the scattered light intensity distribution extracted from the CCD recordings. The rainbow scattering coefficient matrix T is computed by using the modified Nussenzveig’s theory and the vector D is the size distribution of the spray droplets. The subscript numbers 1 and 2 correspond to wavelengths of λ1 and λ2 respectively. For a particular spray, its actual refractive indices under two wavelengths are definitely certain values. Any deviation either in preset value of RI or preset temperature T would lead to an error when comparing the inverse refractive indices (m1, m2) with the hypothesizing refractive indices (n1, n2). Thus actual refractive indices of droplets under two wavelengths and calibration equation can be quickly and simultaneously obtained by searching the minimum of root mean square (RMS) errors between the hypothesizing refractive indices and the ones from inversion. A typical example shows the RMS error for the case of a water spray at 25℃ under two wavelengths (λ1= 532 nm, λ2= 633 nm), as shown in Fig. 3. The actual refractive indices of deionized water under two wavelengths at each temperature can be calculated by Eq. (2). The actual value of RI here equals to 0.47, which can be obtained by locating the geometric rainbow angle in the simulated global rainbow curves. Tested water sprays at temperatures ranging 20℃–30℃ and value of RI ranging 0.44–0.49 are inspected. The preset pair of the value of RI and spray temperature T is used to obtain the hypothetical refractive indices (n1, n2) and linear calibration equation, which can be used to inverse the refractive indices (m1, m2) from the simulated global rainbow curves.

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    Fig. 3. Simulated RMS errors between the preset refractive indices and the inversion ones

    The result in Fig. 3 shows that the RMS error between inverse refractive indices (m1, m2) and the hypothetical refractive indices (n1, n2) is significantly decreased when the tested temperature and the value of RI are close to the target ones. By iteratively searching for the minimum error, accurate temperature, value of RI and the calibration equation can be obtained at the same time. The feasibility of the self-calibration method presented here is verified by the experimental setup in Fig. 4. Two vertically emitted semiconductor laser (wavelength: λ1=532 nm) and He-Ne laser (wavelength: λ2=633 nm) are transformed into one coincident laser beam by a 560 nm dichroic beam splitter (λ > 560 nm transmit; λ < 560 nm reflect). The back-scattered light of spray illuminated by the coincident laser beam is collected by Lens 1 with a diameter of 10 cm and a focal length of 16 cm. Lens 1 is placed 25 cm away from the probe volume. An aperture with a diameter of 2mm is located at the image plane of the Lens 1, in order to select and define the measured probe volume. Then the collected light passes through Lens 2 with a diameter of 10 cm and a focal length of 8 cm. Lens 2 conjugates the image focal plane of Lens 1 on the color CCD sensor, which records chromatic rainbows with a resolution of 1392 × 1040 pixels (6.45 μm/pixel)).

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    Fig. 4. Setup diagram of the experimental system.

    3. Results and Discussion A spray of deionized water is tested. A typical chromatic global rainbow image of mixed rainbow signals is shown in Fig. 5(a). Subject to the power of He-Ne laser, the image presents a yellow-green primary rainbow pattern. The mixed signals are separated in red, green, and blue (RGB) channels, as shown in Fig. 5(b) - (d). For droplets illuminated by green and red lasers, the nearly complete dark image in Fig. 5(d) shows that signal intensity in blue channel is negligible compared to the signal intensities in the other two channels.

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    Fig. 5. Original global rainbow image (a) and images extracted from the red (b), green (c), and blue (d) channels

    The filtered global rainbow curves extracted from red and green rainbow images are shown in Fig. 6, where the noise has been suppressed by fast Fourier transform (FFT) filtering. The value of RI =0.45 and temperature T=23℃ are used as the initial preset values. According to the self -calibration method presented above, we can search the minimum of RMS errors of the preset refractive indices and the ones from inversion, through iterations of correcting the preset value of RI equals to 0.47 and temperature. When iteration is finished, the final preset value of RI equals to 0.47 and temperature T equals to 20℃. The temperature measured by self-calibration method is consistent with the thermocouple readings 21.2℃, which is in the error range (±0.75%+1℃) of a k-type thermocouple. The pixels (pix1 = 206, pix2 = 122) corresponding to the final preset geometric rainbow angles ( =138.217°, =137.741°) can be positioned in the filtered global rainbow curves with the help of RI. And two characteristic calibration point (pix1, θrg1) and (pix2, θrg2) can be used to obtain the parameters of linear calibration equation, a=137.05°, b =0.00566°/pixel. The final RMS error equals to 7.67×10-5 by comparing the preset refractive indices (n1=1.33503, n2=1.33176) at 20℃ and the ones from inversion (m1=1.33511, m2=1.33183).

    Fig. 6. Dual-wavelength distributions of light intensity extracted from the green and red rainbow images. The high frequency noise on the rainbow signals was suppressed by fast

    Fourier transform (FFT) filtering.

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    The performance of this calibrated global rainbow system has been tested and verified further by the water–ethanol solutions with volume concentration from 10% to 60%. FigureFig. 7 shows chromatic global rainbow images of water–ethanol solutions. The location of the bright fringe in rainbow image shifts distinctly for solutions of volume concentration. Directly inverse the refractive indices from the extracted rainbow signals in Red and Green channels, and the measured results are shown in Fig. 8, by method of self-calibration and mirror calibration. The measurement results of these two calibration methods, shown by solid and dashed curves, fit well respectively under two wavelengths.

    Fig. 7. Chromatic global rainbow images of water–ethanol solutions with volume concentration

    from 10% to 60%, with the step of 10% FigureFig. 8 shows that the average discrepancy of refractive index between two methods of calibration is 0.0005, which is equivalent to discrepancy of scattering angle of ~0.07°.This difference might be caused by instrumental error of rotating platform under the mirror (rotating accuracy: 0.05°) and positioning deviation of geometric rainbow angles due to residual noise in the filtered rainbow curves (positioning deviation: ~0.03°). Also, these inversion results show good agreement with the reported values (Hall and Payne, 1922). For the method of self-calibration and mirror calibration, the average deviations of refractive index under each two adjacent wavelength (532nm and 589nm, 589nm and 633nm) is 0.00198 and 0.0015 respectively, which are both roughly in line with the average wavelength deviation 0.0021 at 20℃ calculated

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    by Eq. (2). But obviously this deviation of self-calibration method is closer to the theoretical calculation value than that of mirror calibration method. This one aspect demonstrates that self-calibration method achieves a higher precision than that of mirror calibration method.

    Fig. 8. Comparison of the measured refractive index by method of mirror calibration and self-

    calibration with the theoretical data for water–ethanol solutions at 20℃. Note that when obtaining both the calibration equation and the refractive index measurement under two wavelengths, self-calibrated system only works for the liquids with a prior relationship between refractive index and wavelength, temperature. A different way of putting it, liquids (such as deionized water) whose physical parameters have been fully studied, can be used as calibration medium to complete the angular calibration for rainbow refractometry without additional precise measure device for angle, temperature or refractive index. 4. Conclusion In conclusion, by use of the natural shift of rainbow pattern under two wavelengths, the relationship between scattering angles and pixels are calibrated in parallel to the measurement of the refractive indices under two wavelengths. We call this method a self-calibrated global rainbow refractometry. The feasibility of this method has been tested by simulation and experiment, and the results show that it is an efficient and accurate calibration method for global rainbow system. This method spares the rainbow refractometry from extra

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    angle or temperature measuring instrument. It can apply to mirror inaccessible occasions, and may even be extended to calibration for one-dimensional rainbow technique.

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    Hulst, H. C. and H. C. Van De Hulst(1957). Light scattering by small particles, Courier Corporation.

    Lemaitre, P., E. Porcheron and G. Gréhan, et al. (2006) Development of a global rainbow refractometry technique to

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    Quan, X. and E. S. Fry (1995) Empirical equation for the index of refraction of seawater. Appl Optics 34: 3477-3480.

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    Wu, X., H. Jiang and Y. Wu, et al. (2014) One-dimensional rainbow thermometry system by using slit apertures. Opt

  • 18th International Symposium on the Application of Laser and Imaging Techniques to Fluid Mechanics・LISBON | PORTUGAL ・JULY 4 – 7, 2016

    Lett 39: 638-641.

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