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High resolution optical refractometer for dispersion measurement in UV-NIR

range

Article  in  The European Physical Journal Special Topics · February 2008

DOI: 10.1140/epjst/e2008-00537-x

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Eur. Phys. J. Special Topics 154, 159–163 (2008)


c EDP Sciences, Springer-Verlag 2008 THE EUROPEAN
DOI: 10.1140/epjst/e2008-00537-x PHYSICAL JOURNAL
SPECIAL TOPICS

High resolution optical refractometer for dispersion

measurement in UV-NIR range
J. Pluciński
Department of Optoelectronics and Electronic Systems, Gdansk University of Technology,
ul. Narutowicza 11/12, 80-952 Gdansk, Poland

Abstract. A high resolution optical refractometer for dispersion measurement in

the UV-NIR range is described. Using this refractometer, refractive index of a
range of liquid samples, such as aqueous solutions of sugars, salts and alcohols,
was measured as a function of wavelength in the range from 300 nm to 920 nm
with accuracy better than 10−5 . So accurate results can be used for improvement
of resolution of OCT measurements conducted in biological samples.

1 Introduction

The knowledge of the dispersion of the refractive index in a wide range of wavelength is neces-
sary in many fields of science and technology. An important field where the deep knowledge of
the dispersion is essential is systems based on the measurement of the optical path length. This
group contains precise interferometers for physical or chemical measurements, especially those
used in optical coherence tomography (OCT). The resolution of measurement of the optical
path length increases if the spectral bandwidth of the optical source used in the OCT increases
and its central wavelength decreases. Recent availability of supercontinuum light sources has
resulted in OCT systems achieving resolution about 1 µm [1]. However, a very precise compen-
sation of dispersion in the measured medium is needed in order to attain this resolution. Such
compensation can only be performed if the refractive index of the medium is known with high
resolution, necessitating the use of a high resolution optical refractometer for UV-NIR range.

2 Theory

The absolute refractive index n of a medium is defined as the ratio of the speed of light in
vacuum c to the wave’s speed in the medium v [2]:

n = c/v = f(λ). (1)

For most media n, known also as the phase refractive index, depends on wavelength λ. A group
delay dispersion D is the basic parameter describing dispersive properties of optical materials.
It can be determined from the function n = f(λ) as follows:

D = −[λ0 2 /(2πzc)](d2 ϕ(t)/dω 2 ) = −(λ0 /c)(d2 n/dλ2 ), (2)

where z is the thickness of sample, λ0 is the central wavelength, ω is the angular frequency,
ω0 is the central angular frequency, ϕ is the phase of the optical wave.
160 The European Physical Journal Special Topics

Computer

Reference detector Ir
I4
I1 I2 I3

Light source Monochromator Coupler Detector 1 Detector 2 Detector 3 Detector 4

Chopper
Fibre optic
Optical fibre bundle

Cuvette
Moving stage
Pure water Sample
∆d
Mirror 1 Mirror 2
nw θ ns ∆ϕ

Fig. 1. Block diagram of the refractometer.

Longitudinal resolution ∆z
of an OCT system without dispersion compensation can be

expressed using parameter D as [1]:

 2 2  4
 2

d ϕ(ω) ∆ω 2πcz(∆λ)2
∆z ≈ ∆z 1 + = ∆z 1 + D , (3)
dω 2 ω0 2 4λ20

where ∆z is the resolution of the OCT system for nondispersive materials.

Expression (2) shows that if D = 0 we get compensation for the quadratic phase distortion,
(d2 ϕ/dω 2 )ω0 , of a large-bandwidth optical radiation. Similarly to the problem of generating
ultrashort optical pulses, full compensation of the dispersion in ultrahigh resolution OCT sys-
tems needs compensation not only the quadratic phase distortion, but also the cubic phase
distortion, (d3 ϕ/dω 3 )ω0 [3].
The function n = f(λ) from which the quadratic phase distortion, (d2 ϕ/dω 2 )ω0 , (and para-
meter D), the cubic phase distortion, (d3 ϕ/dω 3 )ω0 , and even higher order phase distortions can
be determined is well known for many substances (e.g. for glasses and other materials used in
optics). Also, the refractive index of water (i.e. the basic substance of life forms) nw in respect
to wavelength, temperature, and mass density is accurately known [4,5].
During measurements by OCT systems (e.g. to needs of biology, medicine, the paper-making
industry) the optical radiation very often propagates not through pure water but through aque-
ous solutions of different chemical substances. The dispersion properties of these solutions differ
from those of the water. Absolute measurements of the refractive index of solutions with the
high accuracy are not an easy task – the difference between refractive indexes of a solution
and clear water is much easier. This difference can be measured by measurement of changes of
direction of optical radiation (described by Snell’s law) crossing the border between to media
having different refractive indexes.

3 The measurement system

The block diagram of the measurement system is shown in Fig. 1. The Xenon lamp produces
the light whose spectrum spans from near UV to near IR. The light, modulated by the chopper,
enters the monochromator, from which it is coupled to an Y-type optical fibre coupler. The
reference detector placed in one of the output ports of the coupler measures the optical power
incident on the sample. The light emerging from the other port is collimated by an off-axis
paraboloidal mirror 1 and passes through the cuvette divided into two triangular parts by a
quartz glass plate. The first part of the cuvette is filled with reference liquid (pure water)
 36th Winter School on Wave and Quantum Acoustics 161

Aqueous solution of sucrose (10 000 ppm) Aqueous solution of ethanol (10 000 ppm)
4.86
1.56 y = 1.193083E-20x6 - 4.604190E-17x5
4.84
y = 4.789156E-21x6 - 2.298393E-17x5 + 7.255686E-14x4 - 5.974128E-11x3
1.54 + 4.511215E-14x4 - 4.658536E-11x3 4.82 + 2.719236E-08x2 - 6.534256E-06x
4.80

∆n (x10-4)
∆n (x10 )

1.52 + 2.693148E-08x2 - 8.405093E-06x + 1.125111E-03

-3

+ 2.587086E-03 4.78
1.50 4.76
1.48 4.74
4.72
1.46
4.70
1.44 4.68
300 400 500 600 700 800 900 300 400 500 600 700 800 900
Wavelength [nm] Wavelength [nm]

Fig. 2. Refractive index difference between Fig. 3. Refractive index difference between aqueous
aqueous solution of sucrose (10 000 ppm) and solution of ethanol (10 000 ppm) and pure water.
pure water.

while the second part contains the measured liquid. The beam leaving the cuvette is focused by
mirror 2 in such a way that the focused spot coincides with the end face of a fibre optic bundle
consisting of four fibres which is attached to a translation stage. The power in these fibres is
measured by detectors 1 ÷ 4 (connected to the computer).
The measurement of the refractive index is based on Snell’s law. The difference of refractive
indices ∆n of measured and reference liquids (∆n = ns − nw ) changes the direction of the beam
emerging from the cuvette, causing the displacement ∆d of the focused spot. Signals I1 ÷ I4
from detectors 1 ÷ 4 are used to determine ∆d (e.g. if the spot is located between the fibres
connected to detector 1 and 2, ∆d is calculated by the computer from signal (I2 −I1 )/(I2 +I1 )).

3.1 Calibration

The system calibration was carried out in four steps.

In the first step the power incident on each detector as a function of the spot displacement
was determined. The fibre optic bundle was shifted by the translation stage. The measurements
were performed with pure water filling both parts of the cuvette. The calibration wavelength was
589.3 nm.
Following, in the second step, the spot displacement versus ∆n was measured for samples
whose refractive index was known with high accuracy (i.e. glycerol solutions) [5]. The measured
sensitivity ∆n/∆d was 2.50 · 10−6 1/µm.
Finally, in the third step, the cuvette was filled with pure water again, and the spectral
characteristic of signals (Ii+1 − Ii )/(Ii+1 + Ii ) (i = 1 ÷ 3) and (I1 + I2 + I3 + I4 )/Ir were
measured (Ir is the signal from reference detector – see Fig. 1). These characteristics were used
to reduce the errors caused by differences between the spectral characteristics of detectors.

3.2 Measurement

Using this refractometer, the refractive index of a broad range of aqueous solutions of well-
known substances like sucrose, fructose, sodium chloride, ethanol, glycerol, ethylene glycol was
measured in range 300 ÷ 920 nm with spectral resolution better than 0.5 nm. Accuracy of the
refractive index measurements was 10−5 while the resolution was 2 · 10−6 . The measurement
range of the refractive index is 1.33 ÷ 1.34 at wavelength 589 nm (from refractive index of
pure water to refractive index of pure water +0.01), and can be changed by moving the stage.
Example results are shown in Fig. 2 and Fig. 3. Samples from a paper mill and chemical pulp
mill were also investigated by this system [6].
Measured refractive index difference ∆n can be conveniently expressed in a polynomial
form:
∆n(λ) = c0 + c1 λ + c2 λ2 + c3 λ3 + c4 λ4 + c5 λ5 + c6 λ6 + · · · (4)
162 The European Physical Journal Special Topics

Table 1. Coefficients ci of formula (4) for 10 000 ppm aqueous solutions of selected substances
(λ in nm).
Substances c0 [×10−3 ] c1 [×10−6 ] c2 [×10−9 ] c3 [×10−12 ] c4 [×10−15 ] c5 [×10−18 ] c6 [×10−21 ]
Sucrose 2.587086 −8.405093 26.93148 −46.58536 45.11215 −22.98393 4.789156
Fructose 2.856365 −15.01617 60.72488 −131.9992 160.2554 −102.4289 26.87140
Sodium chloride 5.205842 −28.21006 102.0161 −203.9943 232.6602 −141.9084 35.95467
Ethanol 1.125111 −6.534256 27.19236 −59.74128 72.55686 −46.04190 11.93083
Glycerol 2.609706 −14.14396 57.32404 −124.2230 149.9040 −95.06769 24.72307
Ethylene glycol 1.737519 −7.329807 26.81796 −52.73504 57.92670 −33.51065 7.969041

where, for convenience reasons, wavelength λ is expressed in nanometres. The coefficients

c0 ÷c7 , obtained from measurement results of 10 000 ppm aqueous solutions are given in Table 1.
For concentrations other than 10 000 ppm, we can obtain ∆n(λ) assuming that ∆n is
proportional to the concentration, which is true for small concentrations, i.e. smaller than few
percents. Adding the refractive index of pure water nw to ∆n we obtain refractive index of the
solution ns from which we can determine phase distortion ϕ(λ) (and group delay dispersion D
given by (2)).

4 Conclusion
Presented measurement method can be used for high resolution, high accuracy measurement
of the refractive index of aqueous solutions of a broad range of substances, particularly for
solutions where the concentration level is very low.
The refractometer can also be very useful for measurements of concentrations of these
substances and for their identification. The obtained resolution of the refractive index makes
this method competitive with an interferometric method without the need for tuned coherent
light sources. Values of the refractive index measured in a broad range of wavelength and
with high resolution allow us to implement advanced dispersion compensation techniques in
ultrahigh resolution OCT systems using configurations similar to those used in ultrashort
pulse systems (i.e. employing complex set-ups of prisms and diffraction gratings) [3]. The
measurement results will be useful also for designers of those measurement systems in which
ultrashort optical pulses propagate through aqueous solutions of measured substances (see
Table 2) – e.g. in time-of-flight spectroscopy [8].

This study was partially supported by Finland’s Ministry of Education, the Polish Ministry of Science
and Higher Education under the grant No. 3 T11B 009 27, and by Gdansk University of Technology
under the BW and DS grants.

References
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 36th Winter School on Wave and Quantum Acoustics 163

3. R.L. Fork, C.H. Brito Cruz, P.C. Becker, C.V. Shank, Opt. Lett. 12, 473 (1987)
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