Sensors and Actuators B 123 (2007) 594605

Fiber optic sensing of liquid refractive index

Argha Banerjee b , Sayak Mukherjee b , Rishi Kumar Verma c , Biman Jana d , Tapan Kumar Khan d , Mrinmoy Chakroborty d , Rahul Das d , Sandip Biswas b , Ashutosh Saxena a , Vandana Singh b , Rakesh Mohan Hallen d , Ram Swarup Rajput b , Paramhans Tewari a , Satyendra Kumar b , Vishal Saxena a , Anjan Kumar Ghosh a,c , Joseph John a,c , Pinaki Gupta-Bhaya d,
a

Department of Electrical Engineering, Indian Institute of Technology Kanpur, Kanpur 208016, India b Department of Physics, Indian Institute of Technology Kanpur, Kanpur 208016, India c Laser Technology Program, Indian Institute of Technology Kanpur, Kanpur 208016, India d Department of Chemistry, Indian Institute of Technology Kanpur, Kanpur 208016, India Received 10 April 2006; received in revised form 28 September 2006; accepted 28 September 2006 Available online 13 November 2006

Abstract An optical ber, partially stripped of its cladding is shown to sense refractive index of a liquid in which the uncladded sensing region is immersed, to a high degree of precision and over a wide range of refractive index. The slope of sensor response is found to be non linear, can have either sign and can change sign at around refractive index of the ber. The sensitivity of the sensor to refractive index change is dependent on cladding thickness and is a maximum at an intermediate thickness value. It is insensitive to the presence of absorption at the wavelength at which refractive index is being measured and to the chemical nature of the solute. Experiments designed to show that cladding modes are responsible for sensing are described. 2006 Elsevier B.V. All rights reserved.
Keywords: Liquid refractive index sensor; Fiber optic refractive index sensor; Refractive index sensitivity of uncladded ber; Uncladded optical ber as sensor

1. Introduction The measurement of refractive index (RI) is important in a variety of applications. Various methods for its measurement have been described [1,2]. Refraction of light by turbid colloidal dispersions has been of interest to physical chemists for more than 50 years [35]. Yet, only a few reports have appeared hitherto on the systematic measurement of RI increment of colloidal spheres. The classical methods of RI measurement from critical angle and Brewster angle data run into difculty for absorbing and turbid liquids [622]. The analysis of light scattering and turbidity spectroscopic data of polymeric or particulate suspension requires RI values of suspended particles [23]. RI determination of suspended particles requires RI data of turbid suspensions. In bio-sensing there is a need to measure small RI changes in small volumes of liquid. Traditional bulk refractometers are then

Corresponding author. Tel.: +91 512 2597372; fax: +91 512 2597436. E-mail address: pinaki@iitk.ac.in (P. Gupta-Bhaya).

not appropriate. Their size and weight are inconvenient in this and other applications. In view of the above, development of alternative sensors of RI, viz., those based on optical ber is relevant. A ber based RI sensor can be very compact in size and be made suitable for remote sensing. It is usable for liquids or polymer composites, needs only a small volume and can be adapted to be chemical sensors. Optical ber has also been used as a sensor of absorption [2427]. Metal-coated bers using surface plasmon resonance [28,29] and in-ber Bragg grating (FBG) [30,31] have been used as highly sensitive RI sensing devices. Tapering of ber and stripping of the ber cladding have been used to make optical ber a sensitive sensor of RI [3236]. Untapered, fully cladded bers with thin lms deposited on them have also been used as RI sensors [37,38]. A ber stripped of cladding has been layered with adsorbent material deposited by Solgel technique to make it a sensor of chemicals that get adsorbed on the adsorbent layer and modify its RI [3945]. Optical ber has been used as a vehicle for carrying light in experiments designed to sense RI, but not directly as a sensor of RI [46,47]. A few reports

0925-4005/$ see front matter 2006 Elsevier B.V. All rights reserved. doi:10.1016/j.snb.2006.09.063

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refer to the signicance of the cladding of a ber in the context of its use as a sensor [4853]. In this report, we describe experimental results on RI sensing by a low cost plastic cladded plastic ber and a silica ber with a plastic coating that forms a protective layer on the silica cladding. This layer is not quite a formal cladding, but its removal shows a measurable sensitivity of output light intensity to the change of RI of the test liquid. In the rest of the paper, we refer to this plastic layer as the cladding of the silica ber. The cladding of these two bers have been stripped to different thickness to make the bers sensitive to RI of the environment. The effect of variation of cladding thickness and the effect of mode scrambling highlight the role of cladding modes in RI sensing. The inuence of light absorption by solute and that of its chemical nature on RI measurement are also investigated. 2. Methods 2.1. Measurement system The experimental setup is shown in Fig. 1. A laser beam ( = 633 nm) obtained from a Melles-Griot (25LHP-213230) Helium Neon Laser is chopped by a Stanford Research System optical chopper at 900 Hz. The chopped light beam falls on a beam splitter (Melles Griot) which splits the beam into a reference and a sample beam that emerge in perpendicular directions. The sample beam passes through a sensor ber, with cladding etched to different extents, immersed in the uid of interest. The beam falls on two separate matched photodetectors whose output currents are converted into proportional voltages. The photodiode is appropriately biased to minimize noise. The two voltages are then fed into two separate Stanford Research System (SR 830) Lock-in-Ampliers. The ratio of their outputs is calculated in a personal computer that is interfaced to the Lockin-Ampliers in a Labview environment. We have performed experiments with a reference beam that directly falls onto a photodiode without passing through a ber or has passed through a fully cladded ber. Experiments performed with both these options give mutually consistent results. The system is veried to be linear within a certain range of light intensity in which we perform experiments. A typical measurement lasts for about 15 min. Total number of data points over which averaging is done is 20/min.

2.2. Fiber specication The plastic cladded plastic ber (SH 4001, Super Eska Fiber, ber diameter: 1.00 mm and core diameter: 0.98 mm, RI of core = 1.492 and of cladding = 1.402) was obtained from Mitsubishi Rayon Co., Ltd., Tokyo, Japan. This ber is a step index ber and is referred to as PCP ber. A silica ber was purchased from Electro-optical Products Division, International Telephone and Telegraph Corporation (ITT), Roanoke, VA, USA (T-1227). It is a graded index ber, has a core thickness 50 (5) m, a glass outer diameter (sum of core and cladding thickness) 125 (6) m, core axial RI 1.48 (nominal) and a numerical aperture 0.230.28. A second layer made of plastic forms a protective coating on top of the silica cladding. This ber is referred to as PCS ber. 2.3. Fiber etching In experiments described in this paper, the optical ber is uncladded to different cladding thickness. As a result, the evanescent eld in the core cladding interface interacts with the surrounding liquid. The PCP ber is uncladded mechanically by careful use of a razor. The plastic coating of the PCS ber is removed by immersing a part of the ber in concentrated sulphuric acid. The degree of cladding removal is dependent on the length of the time of immersion of the ber in acid and is monitored by measurement of the ber thickness by an optical microscope tted with a digital camera. The magnied image of the ber is rened for more accurate edge detection by an image processing software. The thickness of the ber image is then measured by counting the number of pixels between the two edges using manufacturer provided thickness of the untreated ber as reference. A schematic diagram of an optical ber whose sensing region is partially stripped of cladding is given in Fig. 2. Typical total length of ber used is 30 cm. Typical length of the uncladded region is half of the total length. The PCS ber has an outer buffer jacket which cannot be removed by simple mechanical means. Sulphuric acid etching removes the buffer jacket rst and then proceeds to etch the hard plastic layer that coats the silica cladding. It is not possible to stop etching right where the jacket alone has been removed and the hard plastic layer is intact. As a result, we have not measured the thickness of the ber with the plastic layer intact. A change in ber thickness as a result of etching indicates a change in the

Fig. 1. Schematic experimental arrangement.

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Fig. 2. Schematic diagram of an optical ber sensor of refractive index whose sensing region is stripped to different cladding thickness.

thickness of the plastic layer. We nd that the ber treated in sulphuric acid for 16 h shows a ber thickness of 120 m which is the thickness of silica core and silica cladding (the manufacturer specication for this thickness is 125 6 m). Etching for 16 h removes the plastic layer completely. In this report, observations made as a function of ber thickness are interpreted as having been made as a function of thickness of the plastic layer. Data on known refractive indices of solutions of fructose, magnesium sulphate, copper sulphate and sucrose are obtained from CRC Handbook of Chemical and Engineering Data [54]. The data are reported at = 589 nm. 3. Results and discussions 3.1. Sensor response to RI change Let Isig denote the output intensity from the uncladded ber immersed in the liquid under test and let Iref be the intensity of the reference beam. The experimental indicator of the value of the RI of the liquid under test is the ratio R= Isig . Iref

Fig. 3. Plot of change in intensity ratio R as a function of change in refractive index n, tted with an exponential growth function. 2 of t are indicated. The origin with respect to which the s are calculated is sucrose solution of concentration 5% (w/v). Fiber: PCP.

water or the most dilute solution in a given family of samples as reference, measured using PCP bers, are given in Figs. 36. These four plots differ from each other because the ber preparations are different. The degree of cladding removal (a point we elaborate on later) and the surface smoothness vary because of mechanical scrapping used for cladding removal. However, in each of these plots the slope R/n is positive (henceforth called positive slope) and the experimental data points are tted very well (with 2 very close to unity) by an exponential growth function, R = A exp(n/B) + C, where A, B, C are constants. The values of these constants for each gure are given in Table 1. These numbers demonstrate that the sensitivity of the measured intensity ratio to RI change increases with increasing RI of test liquid. Fig. 7(a) displays data obtained on PCS ber etched for 16 h, a linear plot with (R/n) < 0 (henceforth called negative

We have uncladded the sensing bers by mechanical or chemical etching and experimentally determined the variation of R with changes in RI of the liquid. The results of the experiments are plotted in Figs. 311. The characteristics of the slopes of these plots are discussed in the next subsection. 3.1.1. Non linearity and sign of slope A plot of the intensity ratio as a function of RI of test liquids shows a non linear functional dependence. The values of RI used in these plots are literature values, determined by other more direct techniques, viz., critical angle measurements. The reference liquids of known refractive indices that we use are aqueous (aq.) sucrose solutions (n = 1.33591.3999) (54) and aq. glycerol solutions (n = 1.38971.4735) (54). The plots of R, the change in intensity ratio as a function of n, the change in RI, with pure

Fig. 4. Plot of change in intensity ratio R as a function of change in refractive index n, tted with an exponential growth function. 2 of t are indicated. The origin with respect to which the s are calculated is sucrose solution of concentration 3% (w/v). Fiber: PCP.

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Fig. 5. Plot of change in intensity ratio R as a function of change in refractive index n, tted with an exponential growth function. 2 of t are indicated. The origin with respect to which the s are calculated is sucrose solution of concentration 2% (w/v). Fiber: PCP.

Fig. 6. Plot of change in intensity ratio R as a function of change in refractive index n, tted with an exponential growth function. 2 of t are indicated. The origin with respect to which the s are calculated is glycerol solution of concentration 44% (w/v). Fiber: PCP.

Fig. 7. (a) Plot of change in intensity ratio R as a function of change in refractive index n, tted with an exponential decay function. 2 of t are indicated. The origin with respect to which the s are calculated is water. A straight line t with the specied 2 is obtained. Fiber: PCS. (b) Plot of intensity ratio at different values of liquid refractive index (nl ) to show the rise in intensity ratio at high refractive index that follows an initial decrease with a minimum at nl = nber the monotonic decrease at nl < nber is shown in (a), which is performed with a different ber preparation of the same ber. Fiber: PCS.

slope). In this ber preparation, the cladding is fully removed, the remaining ber thickness being 120 m. The plots in Fig. 7(a and b) are obtained from two different experiments done with two different preparations of the PCS ber under conditions of etching time that give negative slope in both. The magnitudes of the intensity ratio and the slopes differ. Even though the PCS ber shows a negative slope when it is fully uncladded
Table 1 Parameters of exponential t of graphs in Figs. 37(a) Figure Fig. 3 Fig. 4 Fig. 5 Fig. 6 A 0.01518 (0.00672) 0.01077 (0.00162) 0.10544 (0.05287) 0.19912 (0.02500)

by sulphuric acid etching for 16 h (Fig. 7), a positive slope is found when etching time is shorter and the cladding thickness is larger (Fig. 11). These statements about positive and negative slopes refer to experiments with liquids whose refractive indices are below that of the ber. According to Fresnel equation only a negative slope should be observed in these liquids.

t 0.02729 (0.00552) 0.03449 (0.00240) 0.05574 (0.02079) 0.03456 (0.00160)

y0 0.01432 (0.00874) 0.00969 (0.00203) 0.10759 (0.05432) 0.18521 (0.04075)

The equation tted is: y = A exp(x/t) + y0 .

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Fig. 8. Plot of intensity ratio as a function of refractive index of fructose and sucrose solution pairs with very close refractive index. The continuous line displays the polynomial (degree 5) t obtained with sucrose data points. Fiber: PCP.

In order to extend the range of liquid RI above that of the ber, we have to use non-aqueous solvents. Whereas, either PCP or PCS ber can be used with aqueous solutions, the latter alone can withstand non-aqueous solvents, e.g., dimethyl sulfoxide (DMSO) and nitrobenzene. Fig. 7(a and b) display data taken on aqueous solutions below the ber RI and nonaqueous solvents above the ber RI using a PCS ber sensor whose cladding is completely removed by sulphuric acid etching for 16 h. We observe a monotonic decrease followed by an increase in Fig. 7(a and b), the change in the sign of slope occurring (Fig. 7(b)) at a RI of the liquid that equals the RI of the ber (n = 1.48). To summarize, we nd that R/n, i.e., the slope of R versus n plots, is a strong function of (a) the type of ber used, PCP or PCS, (b) the extent of cladding removal and (c) the range

Fig. 10. (a) Plot of intensity ratio as a function of refractive index of aq. solutions of copper sulphate and fructose, to evaluate effect of optical absorption on refractive index measurements. The continuous line displays the polynomial t (degree 3) of the fructose data points. Fiber: PCP. (b) Plot of intensity ratio as a function of refractive index of aq. solutions of copper sulphate and fructose, to evaluate effect of optical absorption on refractive index measurements. The continuous line displays the polynomial t (degree 3) of the copper sulphate data points. These data are obtained at signicantly higher solute concentration than those of (a). Fiber: PCP.

of RI being measured. It can be either positive or negative and switches sign at around ber RI. 3.1.2. Relation to literature reports In this subsection, we relate the observations summarized above to existing literature reports. Wong et al. [32] observe insignicant response of a tapered fully cladded multimode plastic optical ber to a RI change in the range 1.331.47 followed by a signicant increase of normalized intensity from 1 to 14 as RI changes from 1.47 to 1.50. Kumar et al. [33] observe experimentally that the output light intensity of a multimode optical ber whose sensing region is stripped of cladding and is tapered, when plotted as a function of n2 (nl is liquid RI being l sensed) is a straight line with a negative slope. The measure-

Fig. 9. Plot of intensity ratio as a function of refractive index of fructose and magnesium sulphate solution pairs with very close refractive index. The continuous line displays the polynomial t (degree 5) of fructose data points. Fiber: PCP.

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Fig. 11. Plot of sensitivity to refractive index change as a function of the thickness of the ber (PCS). The thickness of the ber (and of cladding) decreases along the positive X direction. For each thickness the ratio of the intensity ratios in air to that in water is measured. This ratio is taken as a measure of sensitivity to refractive index change and is plotted as relative sensitivity on the Y-axis. The ber with smallest thickness (16 h etching) registers a decrease in intensity ratio from air to water. All other bers register an increase.

ments cover a range of RI values from that of liquid water (1.33) to that of the ber core (1.45). Villiatoro et al. [34] use a ber with cladding intact and a tapered region that senses RI. The transmission shows a relatively steady light output upto a RI determined by the waist diameter followed by a rapid fall at a high RI (1.4). Afromowitz and Lam [35,36] use a ber with stripped cladding to measure RI of a thin layer of epoxy resin which is overlaid on it and nd that the output light intensity of the sensor shows a negative slope. Spenner et al. [37] measure RI of thin lms deposited on a fully cladded ber using the dependence of the phase velocity of the guided modes on the RI of the lm. Cusano et al. [38] use a fully cladded single mode ber to monitor RI of polymer-based composites deposited on the ber. They make measurements with liquid samples for purposes of calibration. The quantity that monitors the RI of the liquid is the intensity of reected light at the liquidber interface. They observe, just as we do (Fig. 7) a negative slope in the RI range 1.371.48, the ber RI and a positive slope when RI of test liquid exceeds that of ber (1.48). Their results, as well as ours are consistent with the prediction of Fresnel equation. In their case the incident light falls on the ber surface from outside, whereas in our measurement light is incident from within the ber. Reected light intensity as calculated by Fresnel equation is insensitive to this difference in direction of incidence. Several experimental reports on ber optic chemical sensors use adsorbent layers deposited on the ber core as sensors of adsorbed chemicals which modify the RI of the adsorbent layers [3945]. Cherif et al. [39] report a rapid decrease of optical power at a higher RI (1.4) of the adsorbent layer preceded by a comparatively steady response at lower values of RI. The switchover from a steady response to a rapid decrease occurs at a RI that depends on the angle of incidence. Abdelghani et al. [40] studied a PCS ber coated with porous silica deposited

by solgel method as a sensor of chemicals that are adsorbed on the porous silica layer. Chemicals with higher index of refraction than porous silica, when adsorbed, lower its RI and an increase in output light intensity is observed. Chemicals with lower values of RI show opposite behaviour. This report like those of Cherif et al. [39] and Kumar et al. [33] show a negative slope of the sensor sensitivity. Durana et al. [48] in a simulation study on a ber with varying cladding thickness nd that the output optical power decreases at each cladding thickness when the medium changes from air to a high RI oil. The magnitude of decrease is cladding thickness dependent. The simulation is entirely based on Ray theory which includes tunneling rays. Kumar [55] in our laboratory simulated light propagation in a at ber using wave theory and observed a sharp increase in light output above a RI of 1.40, below which the sensor shows comparatively poor response. Amongst the reports cited above, that of Wong et al. [32] is the only one to report a positive slope in the range of liquid RI below that of the ber, in agreement with our results. They use a fully cladded but tapered ber. Their results are relevant to our observations because tapering and stripping of the cladding are qualitatively similar modications. In an experiment [46] in which the ber is not used directly as a sensor, two bers, the same bers cut into two parts, are aligned such that light emerging from the rst passes though the liquid under test and then enters the second. Not all of the light intensity that leaves the rst enters the second. As the beam emerges out of the rst ber, the light beam refracts, the angle of refraction depends on the liquid RI. The light intensity output of the second ber is then a measure of the RI of the intervening liquid. The experimentally veried [46] prediction of the theory of this experiment is that the output power, at the outlet of the second ber, increases with increasing RI of the liquid. The experiments with cladding fully stripped in the sensing region are very close to this experiment. We observe (Figs. 36, 810) in agreement with the theory and experiment of Brown et al. [46] an increase of light output with increasing RI of liquid, a positive slope. Our observation of a non linear dependence of output light intensity on RI of test liquid is in agreement with those of Wong et al. [32], Kumar et al. [33], Cherif et al. [39] and Kumar [55]. 3.1.3. Range The measurements discussed above (Figs. 37) show that the bers used in this report are sensitive RI sensors in the whole range 1.331.56, below and above the ber RI. This observed sensitivity to a broad RI range is in agreement with the ndings of Kumar et al. [33] and Cusano et al. [38]. In contrast, Wong et al. [32] found no signicant response to change of RI in the range 1.331.47 and a signicant sensitivity only in the range n = 1.471.50. The results of a recent theoretical study [55] in our laboratory are similar to those of Wong et al. [32]. 3.1.4. Precision The relative standard error (( of R)/ R) of a typical measurement of intensity ratio is not signicantly dependent on the value of the ratio. It is typically 103 to 104 for the PCP ber with a positive slope and is much larger, typically 101 for the

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Table 2 Data on relative standard error of measurement of change in intensity ratio ( R) in different bers identied by gure numbers in which data obtained with a particular ber is displayed Figure Fig. 3 Fig. 4 Fig. 5 Fig. 6 Fig. 7(a) Value of standard error () 1.994E4 9.912E5 4.244E5 5.850E4 2.230E2 Change in intensity ratio ( R) 0.00928 0.03157 0.00458 0.01759 0.02429 0.03093 0.59330 0.06812 0.09076 Range of refractive index n in each of the following is 0.0106 1.34031.3509 1.37961.3902 1.34031.3509 1.38931.3999 1.34031.3509 1.36001.3706 1.48291.4735 1.34171.3523 1.35941.3700 Value of (/ R) 2.15E2 6.30E3 2.16E2 5.63E3 1.74E3 1.37E3 9.86E4 3.27E1 2.45E1

The range of refractive index used for calculation of sensitivity is indicated.

PCS ber with a negative slope. Precision of n measurement depends on this noise gure alone and is found to be about 105 to 106 (for n = 1) for a ber with a positive slope and 103 for a ber with a negative slope. The precision is larger at large n, because as pointed out earlier, R/ n becomes larger as n increases. The data on precision is given in Table 2. We conclude that RI measurement to a precision in the fth place of decimal is possible with this sensor. The evaluation of precision is based on standard error of mean and not standard deviation. This is justied because the mean value measures the bulk RI and the calibration curve is based on bulk RI values of standard liquids. The reproducibility of the mean as given by standard error of mean is therefore a measure of experimental precision. A large part of standard deviation arises from uctuation of RI around the mean value (bulk RI) in the thin liquid layer surrounding the sensor region of the ber. Literature reports on ber optic sensors with overlaid thin layers [3545] show that these sensors sense RI change very close to the ber surface. Kumar [55] in our laboratory has also observed in his simulation studies that the output power is signicantly modied by a thin layer of a different RI overlaid on the ber surface. This is understandable in view of the short range of evanescent ber sensing. We note that our experiments are as precise as the ones that determine the standard values used to draw a calibration curve. Any higher precision in our experiments would have been useless. 3.1.5. Accuracy The technique described in this paper is not a direct measurement of RI as is, for example, the methods that use critical angle or Brewster angle. The accuracy of this method is entirely dependent on that of the reported RI values used in calibration. 3.2. Sensor response to chemical nature of solute It is necessary that we conrm an anticipated result that the intensity ratio (R) senses RI alone and is entirely independent of the chemical nature of the solute. This anticipation may not hold in the presence of signicant adsorption of solute onto the

sensor surface. Fig. 8 shows the intensity ratio data of a solution of fructose and that of sucrose of nearly equal RI [54]. In the solution pairs chosen for this comparative study, the refractive indices are very close, but not always identical. We have taken care of these non-identical values by tting the values of R as a function of RI for sucrose solution by a polynomial and plotting the corresponding values of fructose solution on the same graph. We nd that the intensity ratio (R) as a function of RI of both the sucrose and fructose solutions are distributed with very small deviations around the plot of the polynomial that ts the data of sucrose solutions best. The deviations of both these families from the polynomial plot are small and comparable and do not increase with increasing solute concentration. Any difference between fructose and sucrose solutions arising from their chemical differences would show dependence on solute concentration. We note that the concentrations of fructose solutions studied range from 0.112 to 2.613 M and those of sucrose solutions range from 0.059 to 1.375 M. The ratio of the highest and the lowest concentration is 25 in both cases and the highest concentrations are fairly large in magnitude. Any difference arising from the chemical nature of solutes would show up, if it indeed exists, at large concentration values used in these experiments. The deviations of the experimental intensity ratio (R) values of sucrose solutions around the plot of the best-t polynomial obtained with data of sucrose solution are, in increasing order of RI, within 3, 2, , , 3, and those of fructose solutions are within , 3, , 2, 3, . The fact that the deviations around the plot of the best-t polynomial are (i) small, (ii) random, (iii) present for both fructose and sucrose solutions and (iv) solute concentration independent at even high salt concentrations, support the contention that the sensor senses RI alone and is not sensitive to the chemical nature of the solute. Identical conclusion is reached from measurements on matched pair of magnesium sulphate solution and fructose solution. The concentrations of fructose solutions studied ranges from 0.340 to 1.878 M and those of magnesium sulphate solutions range from 0.201 to 2.027 M. The ratio of the highest and the lowest concentration is 6 and 14, respectively. The highest concentrations are fairly large for both solutes. The maximum concentration

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of magnesium sulphate studied is so large that ion adsorption is a possibility, but even if it is there, no signicant effect is noticed in the sensing of RI. The experimental intensity ratio (R) of Fructose solutions are tted with a polynomial which is displayed in Fig. 9 and the experimental values of magnesium sulphate solutions are plotted on the same graph. The deviations of the experimental intensity ratio values of magnesium sulphate solutions around the plot of the best-t polynomial are, in increasing order of RI, within 2, , 2, , , and those of fructose solutions are within , , 2, 2, 3, . 3.3. Effect of absorbance(n ) on RI(n ) sensing Meeten and co-workers [16,17,1921] report errors in determination of RI of optically absorbing and turbid uids by critical angle and Brewster angle measurement, the classical methods for determination of RI. The error in transmission mode is shown to be much larger than that in the corresponding reection mode. A method is described for analyzing the data of specular optical reectance at the interface between the uid and the glass prism as a function of the angle of incidence (from the glass prism side) by detailed tting with the theoretical equations to obtain the real and imaginary refractive indices of the uid. The method succeeds for absorbing and some, not all, turbid uids. In view of this difculty with the critical angle method, it is important that other sensors be investigated to nd out about their usefulness for absorbing and turbid uids. We report our investigation on the effect of optical absorbance on RI measurement with the ber sensor. In order to investigate the effect of absorbance of a liquid on the measurement of its RI at a wavelength where absorption is signicant, one would have to make a comparative measurement of the intensity ratio in two liquids with identical values of RI but one of them would have to be absorbing while the other would not absorb, at the wavelength of interest. It is not possible to choose this liquid pair for the comparative measurement referred to above, if we insist that they must have identical RI at a wavelength where one of them absorbs. The values of RI of an absorbing liquid within the absorption band are not reported [54] perhaps because of errors of measurements in standard methods that use critical and Brewster angle data [16,17,1921]. We have chosen a solution pair of copper sulphate and fructose in water, whose refractive indices at 589 nm are identical. This would imply that at 633 nm the refractive indices would be nearly identical, if not identical within errors of measurements. At 589 nm, copper sulphate solution does not absorb. The literature value of RI used for comparison with that of fructose solution at the same wavelength (589 nm) where neither of them absorb is therefore not complicated by the problem of having simultaneous absorbance. We now describe experimental results of this comparative study. The graphical display of the results are given in Fig. 10(a and b). As has been done in the comparison between fructose and sucrose solutions, we t the experimental values of intensity ratio (R) as a function of RI of one of the two liquids (fructose solutions in Fig. 10(a) and copper sulphate solutions in Fig. 10(b)) and plot the experimental values of the other liquid on the same graph. In Fig. 10(a) the deviations around the

graph tted with a polynomial are within, in increasing order of RI, , 2, 4 for copper sulphate solutions and within 2, 3, for fructose solutions. In Fig. 10(b) the corresponding gures are 2, , , for copper sulphate solutions and 2, , for fructose solutions. We conclude that the measurement of RI by the technique we describe is not signicantly inuenced by the presence of absorption. Several reports have appeared in the literature on ber optic evanescent eld absorption sensor [2427]. These papers, however, do not refer to the inuence of absorption on RI sensing. Gupta et al. [27] show the inuence of launching condition and geometry of the sensing region on the sensitivity of the absorption sensor. High sensitivity is achieved by launching power into a ber having tapered sensing region. Absorption sensitivity is small, ideally zero if light is launched horizontally into the ber as we do in our experiments. This is predicted theoretically by Ruddy [25] and is experimentally veried by Gupta et al. [27]. It is thus not surprising that we do not observe any difference in intensity ratio of an absorbing solution and its non-absorbing counterpart (measured at a wavelength within the absorption band), which share the same RI value at a wavelength slightly outside the absorption band. Any optical effect because of the medium is entirely due to refraction. It would be interesting to do these experiments under different launching conditions, for which absorption is sensed. 3.4. Effect of cladding thickness on RI sensing The experiments described below demonstrate the important role played by the cladding of an optical ber in sensing RI. (a) The PCS ber is etched with sulphuric acid for different lengths of time in order to remove its cladding to different extents. When the PCS bers so prepared are used to sense RI, we nd that their RI sensitivities depend signicantly on cladding thickness. Fiber etched for 16 h shows a negative slope in the plot of intensity ratio (R) as a function of RI. This ber shows a steady response after being dipped in water for a few days. The slope is found to be negative right after etching and continues to be so, with change in magnitude until a steady state is attained. Fiber etched for 8 h shows an initial negative slope, which turns positive with time and reaches a steady state with a positive slope. Fibers etched for 2, 4 and 6 h show positive slopes very early. The slope remains positive in steady state. In all ve cases, the time taken to achieve steady state is around 72 h, beyond which the response changes very slowly. In the PCP ber in sharp contrast, a steady response is observed right after the cladding is removed by a razor. The fully cladded original ber is found not to sense RI. (b) The intensity ratios for ve PCS bers with different cladding thickness (etched for different lengths of time 2, 4, 6, 8 and 16 h) were compared in order to investigate the effect of cladding thickness on sensitivity to RI sensing. The ratio of the intensity ratio in water to that in air is taken as a measure of sensitivity. The plot (Fig. 11) of this measure of sensitivity as a function of cladding thickness shows a max-

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Fig. 12. Plot of sensitivity to refractive index change as a function of cladding thickness for PCP ber. The rst point is for fully cladded ber. Cladding thickness decreases along the positive X direction. The numbers on the X-axis indicate the serial number of experimental points. For each thickness the ratio of the intensity ratio of 24% (w/v) to 20% (w/v) fructose solution is measured. This ratio is indicated as relative sensitivity on the Y-axis. It is a measure of the sensitivity of the ber sensor to change in refractive index.

imum of positive sensitivity at an intermediate value. We note that the rst four bers show a positive slope whereas the fth ber (etched for 16 h) shows a negative slope. The same effect has been seen in a parallel study with the PCP ber. A rise in RI sensitivity followed by a fall is observed as the ber is subjected to successive removal of cladding and perhaps also the core by application of a razor. Here the ratio of the intensity ratio (R) of 24% aq. fructose solution to that of 20% aq. fructose solution is taken as a measure of sensitivity. In this study, however, the diameter of ber at different stages of ber slicing was not monitored. Since the cladding thickness is only 2% of the ber diameter, we believe that part of the core was also sliced out in later slicing stages. Fig. 12 shows the results. The initial rise in sensitivity, we believe in view of our experience with the PCS ber, owes its origin to an optimal removal of cladding material. We now refer to a literature report, a simulation study, which when interpreted in terms of dependence of RI sensitivity on cladding thickness, gives results that are in agreement with the experiments described above. Durana et al. [48] in a paper on bending losses in bers, report simulation studies in a ber of a given extent of bending, as a function of cladding thickness in both air and oil. RI of oil equals that of the ber cladding. The output light intensity is small when the ber is immersed in oil and is independent of cladding thickness. This is so because the equality of the refractive indices of oil and ber cladding makes the cladding thickness virtually innite. Since no optical inhomogeneity is encountered, light rays refracted out of the core propagate into the oil without undergoing reection. An output intensity whose magnitude is small and is independent of cladding thickness, is therefore expected and is observed. In air, as the cladding thickness is increased the output light intensity initially increases and then decreases

asymptotically to the constant output intensity found in oil. As the cladding thickness is increased for a certain ber length, the light rays undergo fewer reections and thus fewer transmission coefcients have to be considered. In addition, all of these rays are tunneling at the cladding-air interface and almost all of this power is reected back to the cladding. After reaching a maximum, output power starts decreasing. Rays start being refractive at the cladding-air interface, that is they are no longer tunneling and a lot of power is transmitted to the air. This transmission of power to the air is stronger than the power gained by the ber as a consequence of reducing the number of transmissions and the overall energy balance is negative. These results, when interpreted in terms of dependence of RI sensitivity (oil versus air) on cladding thickness, suggest that as cladding thickness increases, one will observe an increase in sensitivity which reaches a maximum and then decreases. Importance of cladding in determining the sensitivity of a ber sensor has been referred to, in a few other publications. In a humidity sensor described by Khijwania et al. [49] original ber cladding was replaced by a chemically synthesized cladding, The thickness of the latter was found to determine the sensor sensitivity. An optimal thickness maximizes sensitivity. Lower core diameter also enhances sensitivity. Deparis et al. [50] showed the dependence of the -ray induced radiation loss of a ber on cladding to core thickness ratio. Turan and Petrick [51] studied the effect of ber optic cladding on the sensitivity of phase modulated ber optic sensor. Okamoto and Yamaguchi [52] in a study of an optical wave guide sensor that uses a single coupling prism to study optical absorption, demonstrated that the sensitivity of the sensor depends on the thickness of both cladding and waveguide layer. Ansari et al. [53] studied single mode optical waveguide with PbCl2 as a sensitive cladding layer for Chlorine sensing. They observed only slight changes in sensitivity with variation of cladding thickness. 3.5. Cladding modes and RI sensing (a) In order to investigate the role of cladding modes in RI sensing, we have studied the effect of mode scrambler on this sensitivity. This study has been done with both the PCS and the PCP bers. The mode scrambler was placed 10 cm before the sensing region. The mode scrambler increases core-cladding coupling and radiation of cladding modes. The rst effect will increase RI sensitivity, the second effect will decrease it, if cladding modes are the dominant sensors of RI. In Fig. 13, we compare the effect of mode scrambling on a PCS ber etched for 4 h with that on a PCS ber etched for 8 h. The ratio of the two experimental intensity ratios, that in water to that in air, is taken as a measure of sensitivity of the sensor to RI change. The rst of this pair has a larger cladding thickness and a larger RI sensitivity as seen in Fig. 11. We therefore anticipate and also experimentally observe a larger effect of mode scrambling on RI sensitivity of the rst ber (etched for 4 h). Also in both bers we see an initial increase followed by a decrease in sensitivity as mode scrambler is progressively tightened. Fig. 14 shows the result of change in sensitivity of the PCP ber with a

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Fig. 13. Plot of sensitivity to refractive index change as a function of number of turns on mode scrambler for PCS bers, etched for 4 and 8 h. For a given number of turns on mode scrambler, the ratio between the intensity ratio of water to that of air is designated as relative sensitivity on the Y-axis. This ratio is taken as a measure of the sensitivity of the sensor to refractive index change.

(b) The role of the cladding modes in determining the sign of the slope of sensor signal to increase in RI, is highlighted in the following experiment. As already noted in Section 3.4(a), the PCS ber when etched in sulphuric acid for 8 h, shows a negative slope initially but after remaining dipped in water, the slope eventually becomes positive after passing through zero slope at some stage. When the same experiment is repeated with a long ber length (300 cm) preceding the etched sensing region, we nd that the slope is not only negative immediately after etching, but changes very little and remains negative for a very long time (100 h). A shorter ber (30 cm) in the same length of time reaches a steady state positive slope, starting from an initial negative slope. Since cladding modes dissipate during propagation through a long ber length, this experiment relates the presence of cladding modes to the observation of a positive slope of sensor response to increase in RI. 4. Conclusion The light output of an optical ber stripped of its cladding is shown to be a sensitive indicator of the RI of a liquid in which the uncladded sensor region is immersed. The characteristics of the ber sensor, in particular the slope of the sensor output signal to RI change have been investigated. As a result of these investigations, we conclude that these sensors are easy to fabricate and handle, are highly sensitive to RI change (precision to fth place of decimal), can be used with a small liquid volume, are sensitive over a wide range of RI (1.331.56) and are insensitive to light absorption at the frequency at which RI is being measured. These features make them useful in some applications where bulk refractometers are inconvenient. Cladding modes are closely related to the sensing of RI. Their manipulation by adjustment of cladding thickness and ber length preceding the sensor region modies sensor response. Acknowledgements We are indebted to Drs. O.P.Katyal, S.C. Agarwal, Bansilal, A. Pradhan, David, Krishna Kumar, K.K. Sharma, P. Gupta, P.K. Chatterji, R. Sharan, V.K. Singh, Ms. Nina Joseph, Messers Maharaj Singh, Sudhansu Kumar, A. Sivabalan, Babloo Kumar, Peeyush Sahay and A.K. Verma of Indian Institute of Technology Kanpur, Kanpur, India and Drs. T.K. Alex and K. Kanakaraju of the Laboratory for Electronic and Optical Systems (LEOS), Indian Space Research Organisation, Bangalore, India. This work is based on a part of the Ph.D. thesis of T.K.K, the M.Tech thesis of R.K.V. and M.Sc. theses of AB, SM, BJ, RKD, MC and SB, submitted to Indian Institute of Technology Kanpur. Financial support from Indian Space Research Organisation (ISRO-IITK programme). Defence Research and Development Organisation, New Delhi, Ministry of Human Resource Development, New Delhi and Indian Institute of Technology Kanpur are gratefully acknowledged.

xed cladding thickness as a function of the degree of mode scrambling. In this experiment, the ratio of two experimental intensity ratios, that in 20% aq. sucrose solution to that in 12% aq. sucrose solution, is taken as a measure of sensitivity. The results are qualitatively the same as those shown in Fig. 13. In this experiment, the mode-scrambler was fabricated in-house in order to suit the ber thickness of the PCP ber, which was too thick for the Newport mode-scrambler. In these experiments, the slope of the sensor response to increase in RI is always positive, with and without the modescrambler.

Fig. 14. Plot of sensitivity to refractive index change as a function of number of turns on mode scrambler for PCP ber for a given cladding thickness. For a given number of turns on mode scrambler, the ratio between the intensity ratio of 20% (w/v) sucrose solution to that of 12% (w/v) sucrose solution is designated as relative sensitivity on the Y-axis. This ratio is taken as a measure of the sensitivity of the sensor to refractive index change.

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Ashutosh Saxena has obtained BTech degree in Electrical Engineering (EE) from IIT, Kanpur. He is Graduate student in EE from Stanford University, USA. Vandana Singh has obtained PhD degree in Physics from G.B.P. University of Agriculture and Technology, Pantnagar, India. She is Senior Project Scientist from Samtel Center for Display Technology, IIT Kanpur; area: organic exible printable electronics. Rakesh Mohan Hallen has obtained PhD degree in Chemistry from IIT, Kanpur. Ram Swarup Rajput is a member in Technical Staff IIT, Kanpur. Paramhans Tewari is a member in Technical Staff IIT, Kanpur.

Biographies
Argha Banerjee has obtained MSc degree in Physics from Indian Institute of Technology (IIT), Kanpur. He is Graduate student in Theoretical Physics from Tata Institute of Fundamental Research, Mumbai, India. Sayak Mukherjee has obtained MSc degree in Physics from IIT, Kanpur. He is Graduate student in Theoretical Physics from Virginia Tech, Blacksburg, USA. Rishi Kumar Verma has obtained BE degree in Electronics and Communication from MMMEC Gorakhpur, India. He is MTech in Laser Technology from IIT, Kanpur. He is Scientist at Defence Bio-engineering and Electromedical Laboratory (DEBEL), Bangalore, India; area: ber optic sensors. Biman Jana has obtained MSc degree in Chemistry from IIT, Kanpur. He is Graduate student in Theoretical Physical Chemistry, Solid State and Structural Chemistry Unit, Indian Institute of Science, Bangalore. Tapan Kumar Khan has obtained PhD degree in Chemistry from IIT, Kanpur. He is Assistant Professor in Blanchette Rockefeller Neurosciences Institute, Rockville, MD, USA. Mrinmoy Chakroborty has obtained MSc degree in Chemistry from IIT, Kanpur. He is Graduate student in Chemistry from Carnegie Mellon University, USA; area: electronic structure of high valent complexes of biological relevance. Rahul Das has obtained MSc degree in Chemistry from IIT, Kanpur. He is Graduate student in Chemistry from Rice University, USA; area: stochastic processes in complex systems. Sandip Biswas has obtained MSc degree in Physics from IIT, Kanpur. He is Graduate student in Theoretical Particle Physics from University of Hawaii, USA.

Satyendra Kumar has obtained MSc degree in Physics from University of Roorkee. He has obtained PhD degree in Physics from IIT, Delhi. He has gained Research experience at Ecole Polytechnic, Paris and Pennsylvania State University, USA. He is Professor of Physics in IIT, Kanpur; area: thin lms. Vishal Saxena has obtained BTech and MTech degrees in EE from IIT, Kanpur. He is Principal Research Engineer in Department of EE, IIT, Kanpur; area: instrumentation. Anjan Kumar Ghosh has obtained BTech degree in EE from IIT, Khargpur and MS in EE from SUNY, StonyBrook, USA. He has obtained PhD degree in EE from Carnegie Mellon University, USA. He is a member in Technical Staff, Bell Labs, Taught at Iowa State University, USA; Nanyang Technological University, Singapore. He is a Professor in EE Department in IIT, Kanpur. Currently he is Visiting Professor in Department of ECE, Oklahama University. Tulsa, USA; senior member of IEEE, area: optical information processing, optical communications, photonic sensors, instrumentation. Joseph John has obtained BSc in Engineering from College of Engineering, Thiruvananthapuram, University of Kerala, India. He has obtained MTech in EE, IIT, Kanpur; PhD degree in EE, Birmingham University, UK. He is Scholar of the Commonwealth Fund; Professor in EE Department, IIT, Kanpur; area: photonics, instrumentation. Pinaki Gupta-Bhaya is Natural Sciences Tripos, BA (Hons), MA from Cambridge University, England. He has obtained PhD in Chemistry from Columbia University, New York. He is Post Doctoral Fellow from Max Planck Institute f r u Biophysikalische Chemie, G ttingen, Germany. He is Professor in Chemistry o Department, IIT, Kanpur; area: physical chemistry.