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LEP 2.5.02 Polarimetry: Related Topics

1. The document describes an experiment to measure the specific rotation of sucrose and lactose solutions using a half-shade polarimeter. 2. It also aims to determine the reaction rate constant for the inversion of sucrose into invert sugar in the presence of hydrochloric acid. 3. Key steps involve preparing solutions of known concentrations, measuring their angle of rotation, and repeating for sucrose solutions after adding HCl to catalyze inversion over time. Results are used to calculate specific rotation values.

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0% found this document useful (0 votes)
52 views

LEP 2.5.02 Polarimetry: Related Topics

1. The document describes an experiment to measure the specific rotation of sucrose and lactose solutions using a half-shade polarimeter. 2. It also aims to determine the reaction rate constant for the inversion of sucrose into invert sugar in the presence of hydrochloric acid. 3. Key steps involve preparing solutions of known concentrations, measuring their angle of rotation, and repeating for sucrose solutions after adding HCl to catalyze inversion over time. Results are used to calculate specific rotation values.

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Netflix Tag
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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R

LEP
Polarimetry
2.5.02

Related topics Graduated cylinder, 100 ml, plastic 36629.01 2


Half-shade principle, optical rotatory power, optical activity, sac- Graduated vessel, 1 l, w. handle 36640.00 1
charimetry, specific rotation, reaction rate, Weber-Fechner Law. Funnel, plastic, dia 90 mm 36891.00 1
Spoon, w. spatula end, 18 cm, plastic 38833.00 1
Glass rod, boro 3.3, l = 300 mm, d = 8 mm 40485.06 1
Principle and task Pipette, with rubber bulb, long 64821.00 1
The rotation of the plane of polarisation through a sugar solu- D (+)-Sucrose 100 g 30210.10 1
tion measured with a half-shade penumbra polarimeter and the Hydrochloric acid 1.19 2500 ml 30214.79 1
reaction rate constant for the inversion of cane sugar deter- Water, distilled 5l 31246.81 1
mined. D(+)-Lactose, powder 100 g 31577.10 1
Balance LG 311, 4 beams 44007.31 1
Equipment
Half-shade polarimeter, 220 V AC 08628.93 1 Problems
Immersion thermostat A100 46994.93 1
1. To determine the specific rotation of cane sugar (sucrose)
Accessory set for A100 46994.02 1
and lactose by measuring the rotation of various solutions
Bath for thermostat, Makrolon 08487.02 1
of known concentration.
Stopwatch, digital, 1/100 sec. 03071.01 1
Crucible tongs, 200 mm, stainl.steel 33600.00 1 2. To determine the reaction rate constant when cane sugar is
Beaker, 250 ml, low form, plastic 36013.01 2 transformed into invert sugar.

Fig. 1: Experimental set-up for measuring the rotation of sugar solutions.

PHYWE series of publications • Laboratory Experiments • Physics • PHYWE SYSTEME GMBH • 37070 Göttingen, Germany 22502 1
R

LEP
Polarimetry
2.5.02

Set-up and procedure Theory and evaluation


To measure optical activity we use a polarimeter in which light Optical activity is the ability of many substances to rotate the
of wave-length 589 nm (sodium-D line) is first plane-polarised plane of vibration of a ray of plane-polarised light passing
by a polariser and then studied by a second polariser to find through them. It is caused by the two components of a plane-
its new plane of polarisation after passing through the sample polarised ray of light travelling at different speeds through the
substance. asymmetric medium and, in so doing, undergoing a phase
shift with respect to one another, this phase shift being indi-
In order to increase the accuracy of measurement, in one half cated as a rotation of the plane of polarisation.
of the field of view there is a Laurent’s quartz plate which
rotates the plane of polarisation through a further small angle. The specific rotation (rotatory power) of solutions of optically
The analyser is now set to equal brightness on the two sides active substances is defined as the angle through which the
of the field of view: this gives a sharp setting and is easy to plane of polarisation of a ray of sodium-D light (wave-length
reproduce (Weber-Fechner Law). l = 589 nm) would be rotated by a column of solution 100 mm
in length, containing 1 g of substance per cm3 at 20 °C. It is
1. First prepare a cane sugar solution of known concentration expressed by the symbol
c. For example, a solution of concentration c0 = 0.24 g/cm3
is made by dissolving 12 g of cane sugar and making up to [a] 20
D
°

a total volume of 50 cm3 with distilled water in the measur-


ing cylinder. If we assume that the rotation is proportional to the concen-
tration c, then the specific rotation can be determined from the
The rotation of this solution is determined in the half-shade rotation a at a known concentration:
polarimeter by adjusting the two halves of the field to iden-
a
tical brightness. In all, four concentrations [a] 20°
D = c
c0 c0 c0
c0; ; ; (related to a column length of 100 mm)
2 4 8
are made by making up the solution remaining in the meas- If the measurment temperature starts at 20 °C, the value
uring cylinder each time with exactly the same volume of obtained must be corrected in accordance with
distilled water (it may be necessary to pour some off first).
[a] 20 q
D = [a] D – 0.072 (20 ° – q)
°

The temperature of the solutions should be the same in all


cases. The containing vessels are tempered in the water for lactose, or
bath for approx. 5 minutes prior to each measurement.
[a]q
[a] 20°
D = 1 – 0.00037 (q – 20°)
The same procedure is used for measuring the rotation of
lactose (concentration c0 = 0.30 g/cm3, for example). for sucrose.

2. 12 g cane sugar are placed in the measuring cylinder and The mean value found for the specific rotation of the lactose
made up to 50 ml with distilled water (c0 = 0.24 g/cm3). solution was
[a] 20°
D = 53.0 °, with a standard
When the sugar has dissolved completely (stir it), the
deviation s [a] 20 °
D = 0.3 °
measuring vessel is filled and heated in the water bath for
approx. 5 minutes at test temperature T (approx. 30 °C).
The specific rotation of the cane sugar solution was
This temperature must be maintained throughout the
experiment. The measurement of the angle of rotation [a] 20°
D = 65.3 °, with a standard
gives a value a0. deviation s [a] 20 °
D = 1.3 °

The solution remaining in the measuring cylinder is now In the presence of H+ ions, which have a catalytic effect in this
made up to exactly double the volume with 2n HCl, stirred, case, an aqueous solution of cane sugar breaks down into
placed in the measuring vessel and brought to the test optically active glucose and fructose.
temperature in the water bath. The stop clock is started at
this time. The vessel is removed from the water bath after
approx. 5 minutes and the angle of rotation measured. The
series of measurements is dicontinued after 40 – 50 min-
utes and the final angle of rotation determined. For this
purpose, the solution is heated to 70 °C in the water bath
for approx. 5 minutes: this completes the inversion process H2O.H+
Cane sugar 33335 glucose + fructose
very quickly. The vessel is then brought back to the test
(sucrose) (d-gluose) (d-fructose)
temperature and the final angle of rotation b determined.
[a] D20 = 66.5 ° [a] D20 = 52 ° [a] D20 = - 92 °
6

invert sugar
[a] D20 = - 20 °

Fig. 2: Diagram of cane sugar inversion

2 22502 PHYWE series of publications • Laboratory Experiments • Physics • PHYWE SYSTEME GMBH • 37070 Göttingen, Germany
R

LEP
Polarimetry
2.5.02

This is a first order reaction, i. e. the reaction rate is proportion- Fig. 3: Semi-logarithmic plot of the measured values from
al to the concentration of the cane sugar. cane sugar inversion.

Since the reaction rate is defined as the decrease in concen-


tration per unit of time, the differential equation
dc
– =k·c
dt

can be used, from which

c0
ln =–kt (1)
c(t)

is obtained after integration, and where k is the reaction rate


constant, c0 the initial concentration at time t = 0 and c(t) the
concentration at time t.

If a(t) is the rotation at time t, a0 the rotation of the pure cane


sugar solution and b the rotation of the solution which has
been fully inverted, then
c0 a 1 |b|
= 0
c(t) a(t) 1 |b|

With (1) we obtain

1 a 1 |b|
k=– 1n 0
t a(t) 1 |b|

We can now calculate the reaction rate constant k for each


pair of values for t and a(t), and obtain the average value k, or
determine it using the expression

a0 1 |b|
t = A + B ln
a(t) 1 |b|

from the slope b of the regression line, applying the relation

1
k=
b

Evaluating the measured values shown in Fig. 3


(c0 = 0.24 g/cm3, q = 29.5 °C) gives

k = 23.7 ± 0.2 · 10-3 min-1

Note
The detailed instruction manual of the polarimeter gives exam-
ples for several other materials which can be analyzed and will
give reproducable results.

PHYWE series of publications • Laboratory Experiments • Physics • PHYWE SYSTEME GMBH • 37070 Göttingen, Germany 22502 3

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