Abbe's Refractometer

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Abbes
Refractometer


Name:-Mangaljit Singh Abhijit Sanjeev
Entry No:-2014PHA2208 Entry No:-2014PHA2202

M.Tech in Applied Optics
Indian Institute of Technology, Delhi

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Aim:-

To find refractive index of the given liquid samples using Abbes refractometer.

Apparatus:-

Abbes refractometer, temperature controller, light source, cotton and liquid
samples.

Theory:-

The Abbe instrument is the most convenient and widely used refractometer, Fig:-1
shows a schematic diagram of its optical system.

Fig:- 1
Schematic diagram of optical system[1]

The sample is contained as a thin layer (~0.1mm) between two prisms. The upper
prism is firmly mounted on a bearing that allows its rotation by means of the side
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arm shown in dotted lines. The lower prism is hinged to the upper to permit
separation for cleaning and for introduction of the sample. The lower prism face is
rough-ground: when light is reflected into the prism, this surface effectively
becomes the source for an infinite number of rays that pass through the sample at
all angles. The radiation is refracted at the interface of the sample and the smooth-
ground face of the upper prism. After this it passes into the fixed telescope. Two
Amici prisms that can be rotated with respect to another serve to collect the
divergent critical angle rays of different colors into a single white beam that
corresponds in path to that of the sodium D ray. The eyepiece of the telescope is
provided with crosshairs: in making a measurement, the prism angle is changed
until the light-dark interface just coincides with the crosshairs. The position of the
prism is then established from the fixed scale. Thermosetting is accomplished by
circulation of water through the jackets surrounding the prism.

Fig:-2
Inside view of telescope[3]

The Abbe refractometer is very popular and owes its popularity to its convenience,
its wide range (n
D
= 1.3 to 1.7), and to the minimal sample is needed. The accuracy
of the instrument is about 0.0002.
A precision Abbe refractometer is also available; in which the improvement in
accuracy is obtained by replacing the compensator with a monochromatic source
and by using larger and more precise prism mounts. The former provides a much
sharper critical boundary, and the latter allows a more accurate determination of
the prism position.
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According to the law of refraction, n=sin(i)/sin(r), where i and r are the angles of
incident and refracted ray, n is a constant called the index of refraction. From this
equation, it is evident that when light is incident upon a transparent body, there
will be a definite angle of refraction corresponding to every angle of incidence. If
the refractive index of the body is greater than that of the medium outside, the
angles of refraction will be smaller than these corresponding angles of incidence.
But the upper limit of the angle of incidence is 90 degrees. There will be a
corresponding upper limit for the angle of refraction which determines the largest
angle, which any ray penetrating the body may make with the normal. This angle is
the critical angle of refraction r
c
. Its value is obtained from the basic equation by
substituting i=90 or sin(i)=1 where n=1/sin(r
c
.).Consequently a measurement of
the critical angle of refraction gives immediate information concerning the index of
refraction.

To an observer inside a medium of refractive index n, all rays incident upon the
surface from above are confined, upon refraction, within a cone corresponding to
the angles of refraction from zero up to the critical angle, as illustrated in fig. 2, no
illumination exists from any direction whose angle with the normal is greater than
this critical angle. Consequently the critical ray makes a boundary between a dark
and a light area. This is more clearly illustrated in fig. 3.





Fig:-3
Darkness obtained beyond critical angle



For monochromatic illumination this boundary will be a sharp line. For
measurements of the critical angle as commonly made in the laboratory, the circle
of fig:- 4, illustrates the appearance of the field of view of the observing telescope.
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Fig:-4
Field of view of the observing telescope

It is not possible as a rule, to make a direct measurement of r
c
. For the grazing
incident ray, i=90,we have 1=(n
g
/n
x
)sin(r) and for the ray emerging from the glass
into the air.
One can show that:-

where is the refracting angle of the prism.
For greater convenience of measurement the refractometer built on this principle
are equipped with a calibrated scale. The Abbe refractometer measures refractive
indices over the range of 1.3 to 1.7 and is provided with a practically linear scale
which can be read to 0.001 and is accurate to 0.0002. The essential feature of this
instrument lies in the use of a pair of so called Amici prism, two similar 45-degrees
prisms of high refractive index. A drop of the liquid whose index is desired is
placed upon the hypotenuse of one prism, and the hypotenuse of the other prism is
placed upon that of the first, so that the two together from a cubical block of glass.
A telescope focused for parallel light as shown in fig:- 5 will show the
characteristic divided field.
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Fig:-5
Characteristic divided field
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The index of the liquid is then read directly from the calibrated scale. The
calibration is made for sodium light, but the instrument can also be used with
daylight illumination. This is made possible by the introduction of a compensator
consisting of two direct vision prism. They can be rotated in opposite directions at
equal rates, and form together a system of variable dispersion. In this way, an
amount of dispersion can be introduced to counteract that of the specimen under
examination. The compensator carries a scale by means of which a measurement of
the dispersion of the material under examination may be obtained.
Amici Prism:-
An Amici prism, named for the astronomer Giovanni Amici, is a type of
compound dispersive prism used in spectrometers. The Amici prism consists of
two triangular prisms in contact, with the first typically being made from a
medium-dispersion crown glass, and the second a higher-dispersion flint glass.
Light entering the first prism is refracted at the first air-glass interface, refracted
again at the interface between the two prisms, and then exits the second prism at
near-normal incidence.

Fig:-6 An Amici prism [6]
The prism angles and materials are chosen such that one wavelength (colour) of
light, the centre wavelength, exits the prism parallel to (but offset from) the
entrance beam. The prism assembly is thus a direct-vision prism, and is commonly
used as such in hand-held spectroscopes. Other wavelengths are deflected at angles
depending on the glass dispersion of the materials. Looking at a light source
through the prism thus shows the optical spectrum of the source.

Fig:-7
A compact fluorescent lamp seen through an Amici prism[6]
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The dispersive Amici prism should not be confused with the non-dispersive Amici
roof prism.
An Amici roof prism, named for its inventor, the Italian astronomer Giovanni
Amici, is a type of reflecting prism used to deviate a beam of light by 90 while
simultaneously inverting the image. It is commonly used in the eyepieces
of telescopes as an image erecting system. It is sometimes called an Amici
prism or right angle roof prism. The non-dispersive Amici roof prism should not
be confused with the dispersive Amici prism.
The device is shaped like a standard right-angled prism with an additional "roof"
section (consisting of two faces meeting at a 90 angle) on the longest side. Total
internal reflection from the roof section flips the image laterally.
The handedness of the image is unchanged.
The roof faces of the prism are sometimes coated to provide mirror surfaces. This
allows the prism to be constructed with other beam deviate angles besides 90
without being limited by total internal reflection

Fig:-8
An Amici roof prism[7]
Now, in the measurements of the refractive index, light is directed into the prisms
along the axis of the telescope by means of a mirror attached to the instrument. The
eyepiece is focused simultaneously on the cross-hair and the scale by properly
turning the eyepiece. Using sodium light, the adjustment for an index of refraction
reading consists in turning the lower adjusting screw in such a way that a double
field half bright half dark with a sharp dividing edge passing through the center of
the cross-hair is seen.
Then the index of refraction is read off the scale to the third decimal and the fourth
decimal is conveniently estimated. When white light is used, the compensator must
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be adjusted before final adjustment of the prisms as described below in the
procedure.
If polychromatic radiation is used, no single sharp boundary such as that in fig:- 9
is observed. Instead, a diffuse chromatic region between the light and dark areas
develops; the precise establishment of the critical angle is thus impossible. This
difficulty is overcome in refractometers by the use of monochromatic radiation. As
a convenient alternative, many critical angle refractometers are equipped with a
compensator that allows the use of radiation from a tungsten source, but
compensates for the resulting dispersion in such a manner as to give a refractive
index in terms of the sodium D line. The compensator is made of Amici prisms, as
shown in Fig:- 10. The properties of this complex prism are such that the dispersed
radiation is converged to give a beam of light that travels in the path of yellow
sodium D line.

Fig:-9



Fig:-10
Amici prism for compensation of dispersion by sample. Note that yellow radiation (sodium D line)
suffers no net deviation from passage through the prism.[1]
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Temperature dependence of refractive index:-
The refractive index of a liquid varies with density, primarily because the density
of liquids varies with temperature. One can approximate the dependence with the
equation:-
) ( ) ( ) (
0 0
T T T n T n
T


where T
0
is some standard temperature where the index of refraction n(T
0
) is the
known index of refraction n at T
0
, and
T
is the temperature coefficient of the
index of refraction of the given liquid. Values of
T
vary, but they tend to be
0.0003 to 0.0004 for liquids with n < 1.63 (all of the liquids in this lab) and
approximately 0.0007 for liquids with n > 1.63. For simplicity, we take
T
to be
0.0004.

Wavelength dependence of refractive index:-
The refractive index of a material varies with wavelength, a phenomenon which is
called chromatic dispersion. In the visible spectrum, it can be represented to a good
approximation by Cauchys equation
2
) (

B
A n

Where A and B are constants that depend on the material, and is the vacuum
wavelength. For example, at 20 C, for water A = 1.324 and B = 0.00319 m
2
; and
for ethanol, A = 1.352 and B = 0.00318.

Procedure:-

General directions: The student is cautioned to handle the refractometer with
extreme care.
The prisms are made of flint glass; they are brittle and at the same time extremely
soft. Therefore they are easily broken and scratched. Be sure to keep the surfaces
of the prisms clean and to use only clean liquid on them.

1:-The scale and the cross-hair in the circle are focused by turning the eyepiece.
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2:-To lift the upper prism off for applying the sample to be tested, turn the small
knob attached to the prism into such a position, that the arrow mark at the side
points upward; if it points sideward, the prism is locked in position. With the
knob in the free position, swing the upper prism out into its rest position.
By means of a smooth glass rod apply a drop of the liquid to be tested of the
fixed prism and bring the upper prism back on top of the lower one.

4:-Start sodium light source and adjust its position, open the reflecting mirror of
the upper prism and if necessary, adjust it for good illumination of the circle
seen through the telescope; if necessary adjust the tube providing the
illumination of the scale.

5:-Adjust the positions of the prisms by turning the knob at the lower right until in
the middle of the bright circle a clear boundary line is observed between a dark
gray sector in the lower half and a bright sector in the upper half of the circle.
Make a fine adjustment of the prism position by turning the knob at the lower right
until the boundary line passes through the center of the cross-hair.

6:-Read off the index of refraction on the illuminated scale directly up to the third
decimal and estimate the value of fourth.

7:-Read and record the temperature of the thermometer attached to the instrument.

Repeat this procedure with other samples. Repeat one of the measurements using
white light. This requires the operation of the built-in compensator. The
compensator is adjusted by turning the knob at the middle of the instrument. Start
with the compensator at the zero mark. Adjust the prisms gradually until a bright
red-orange light appears across the middle of the circle. This will be the adjustment
close to the final position. For further refinement turn the compensator knob until
the color disappears and a sharp boundary line is obtained separation a gray sector
in the lower part and a bright sector in the upper part of the circle opening. Read
just the prisms until the boundary coincides with the center of the cross-hair. Read
the value of the index of refraction and the thermometer as before and compare
with the result of the previous measurement.

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Trouble-shooting [2]

a. The viewing area does not show a separation into a light and a dark field.
Check briefly if the range that you are in right now is anywhere +/- 0.05 units of
the expected refractive index (literature value) if not, make sure to get close to this
range by using the adjustment knob on the right side. Keep in mind that it is
relatively sensitive.

b. The viewing area shows fancy colors and not just a light and a dark field.
This is often observed if not enough material is applied to the prism and an uneven
film is coating the prisms. The same effect is observed if the hinged prism is not
pushed all the way down or the sample is inhomogeneous or strongly colored.
c. There is not light in the viewing area.
Is the instrument turned on? Is the lamp raised to its correct position?

Note:- Before every observation, clean the lower and
upper amici prism surface thoroughly.

Sources of Errors:-[5]
The secret to getting the most accurate possible refractometer readings is, in a
word, "temperature." Even if a refractometer is automatically temperature
compensated you will not get the most accurate results if you do not allow
temperatures to equilibrate (equalize).
Temperature is one of the single most important factors influencing accurate
refractometer readings and is one of the largest sources of error in measurement.
Refractive index is VERY dependent on temperature. The amount of error per
degree of temperature is different for every fluid and differs for different
concentrations of the same fluid. Although temperature compensation relieves the
user of the responsibility to measure temperature and apply a correction factor
when taking readings, it is not infallible.
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Whether you are using a traditional analog refractometer, a digital handheld
refractometer, or a desktop refractometer, you must allow time for the
refractometer temperature, the ambient temperature, and fluid temperature to come
to equilibrium .Since the volume of fluid is usually only a few drops, its thermal
mass compared to that of the refractometer is really rather small, allowing it to
come to the temperature of the refractometer relatively quickly, in most cases.
Thick viscous fluids, like maple syrup, typically take longer to come to equilibrium
than less viscous material such as water.
It will take a little time for a refractometer to adjust to changes in environmental
temperature. For instance, if you take a refractometer from a cool air-conditioned
laboratory out onto a shop floor on a hot summer day, it will take some time for the
refractometer to equalize with the temperature in the shop. Likewise, if in the
winter you are carrying a refractometer under a winter coat next to your body and
then pull the refractometer out to make a measurement, it will naturally take some
time for the refractometer to adjust to the change in ambient temperature.
Everyone asks, How much time? There is no magic answer to this since there are
too many variables. Each situation is different. But, providing the refractometer
and ambient temperature are in equilibrium, as a general rule of thumb, you should
wait about 10 seconds for every 5 F difference between refractometer temperature
and 68F, or about 30 seconds for each 10 C difference between the fluid
temperature and 20 C.
How do you know if the temperature is stable? For the Palm Abbe digital handheld
refractometer, if the rate of change of temperature exceeds a certain limit then the
refractometer will not allow you to take a reading. However, it is possible that
when putting a hot sample on a room-temperature refractometer the initial rate of
change will be very high for the first 10 to 20 seconds and then level off and drift
slowly towards equilibrium. If temperature is drifting relative to time you can
expect to see some drift in your reading as well. So, if your refractometer readings
are slowly drifting in one direction then there is a chance that the temperature is
not stable. The direction of the drift depends on the nature of the changing
temperature. Generally, if the temperature is stable and you take five
measurements in a row, the readings should not vary by more than the precision of
the scale.
Another issue of concern is evaporation. Evaporation is vaporization that takes
place at the surface of a liquid. The process of evaporation will increase the larger
the surface area, the higher the liquid's temperature, the higher flow rate of air past
the surface, and the lower its density. The Palm Abbe refractometer mitigates the
effects of evaporation by limiting the fluid volume/surface area and inhibiting air
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flow with its Evaporation Cover. If a sample is rapidly evaporating, you can expect
to see an upward drift in the refractometer reading over time.
For the most accurate possible refractometer readings, take your time and allow the
temperature of the refractometer, the ambient environment, and the fluid sample to
come to equilibrium. As a general rule of thumb, you should wait about 10 seconds
for every 5 F difference between refractometer temperature and 68F, or about 30
seconds for each 10 C difference between the fluid temperature and 20 C.
Sample Calculations:-
Least Count (L) =0.0005

S. No Name of Sample Main Scale
Reading(say u)
Small Division
(say w)
Refractive
Index
n=u+L*w
1 Water a 1.33 18 1.3390
b 1.33 17 1.3385
2 Propan-2-ol a 1.38 3 1.3815
b 1.38 1 1.3805
3 1-Bromonaphtalene

a 1.65 12 1.6560
b 1.65 10 1.6550
4 Benzene a 1.5 5 1.5025
b 1.5 3 1.5015
5 Non-Staining Oil a 1.46 7 1.4635
b 1.46 10 1.4650
6 Machine Oil a 1.46 1 1.4605
b 1.46 2 1.4610
Mean value of refractive index of Water=1.33875
Mean value of refractive index of Propan-2-ol =1.3810
Mean value of refractive index of 1-Bromonaphtalene =1.6555
Mean value of refractive index of Benzene =1.5020
Mean value of refractive index of Non-Staining Oil =1.46425
Mean value of refractive index of Machine Oil =1.46075
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References:-
[1]:- http://amrita.vlab.co.in/?sub=1&brch=195&sim=545&cnt=1
[2]:- http://www.chem.ucla.edu/~bacher/General/30BL/tips/refract.html
[3]:- http://www.refractometer.pl/Abbe-refractometer
[4]: http://www.mikroskop-online.de/Mikroskop%20BDA%20Gruppe%2032/32-
110f-2%20%20Abbe%20Refractometer.pdf
[5]:-http://www.misco.com/training/refractometer-general/47-the-secret-to-
accurate-refractometer-readings
[6]:- http://en.wikipedia.org/wiki/Amici_prism
[7]:- http://en.wikipedia.org/wiki/Amici_roof_prism

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