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LEC 02
12150.00
12151.99
14602.00
12102.00
14503.61
11759.01
Calorimeter, transparent
04402.00
04450.00
13715.93
13500.93
07361.05
35720.93
35680.04
35680.03
02022.20
37697.00
Universal clamp
37715.00
48803.93
36294.00
39258.00
33006.00
Pasteur pipettes
36590.00
Rubber bulbs
39275.03
03071.01
33931.00
1,4-Dioxan, 1000 ml
31266.70
Water, distilled, 5 l
31246.81
P3020911
PHYWE Systeme GmbH & Co. KG D - 37070 Gttingen
LEC
02.09
Related concepts
Heat capacity, melting point, latent heat, calorimetry, Gibbs
phase rule, enthalpy of sublimation, enthalpy of vaporization.
Principle
When a solid melts, energy is required for the destruction of the
crystal lattice. A substance whose melting point lies slightly
below room temperature is first cooled until it solidifies and then
melted in a calorimeter. The melting enthalpy is calculated from
the decrease in temperature due to the melting process which is
measured in the calorimeter.
Tasks
1. Take a temperature-time-diagram for the melting process of
dioxan
2. Calculate the melting enthalpy and entropy of 1,4-dioxan.
Equipment
Cobra3 Basic-Unit
Power supply 12 V/2 A
Data cable, RS232
Temperature measuring module Pt 100
Software Cobra 3 Temperature
Temperature probe Pt 100
Calorimeter, transparent
Heating coil with sockets
Work and power meter
Universal power supply
Connection cable, l = 500 mm, black
12150.00
12151.99
14602.00
12102.00
14503.61
11759.01
04402.00
04450.00
13715.93
13500.93
07361.05
1
1
1
1
1
1
1
1
1
1
4
35720.93
35680.04
35680.03
02022.20
37697.00
37715.00
1
1
1
1
2
2
48803.93
36294.00
39258.00
33006.00
36590.00
39275.03
33931.00
31266.70
31246.81
1
2
2
1
1
1
1
1
1
PHYWE series of publications Laboratory Experiments Chemistry PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen
P3020911
LEC
02.09
Weigh out 44.05 g (0.5 mol) of 1,4-dioxan in a test tube (weighing accuracy 0.01 g) and close it with a stopper. Fill the Dewar
vessel with 300 g of ice and 100 ml of cold water. Place the test
tube in this water-ice mixture for about 1 hour until the dioxan is
frozen. In the meantime, fill the calorimeter with 850 g of distilled
water (weighing accuracy 0.1 g). Place it on the magnetic stirrer,
put in the oval magnetic stirrer bar and switch on the stirrer
(Caution: Do not switch on the heating unit by mistake!). Insert
the heating coil and the temperature probe into the lid of the
calorimeter and fix them in position.
When temperature equilibrium has been reached (after approximately 10 min) start the measurement by pushing <Start measurement>. Wait 3 to 4 minutes, then take the test tube out of
the Dewar vessel, quickly dry it, and insert it through the hole in
the lid into the water. The water level in the calorimeter should be
about 1 cm higher than the level of the dioxan in the test tube.
When the dioxan has completely melted and a thermal equilibrium has been established, continue to measure the temperature
for about another 5 minutes. Subsequently perform electrical
calibration to determine the total heat capacity of the calorimeter. Supply 10 V AC to the work and power meter for the electric
heating. Push the <Reset> button and then put the free ends of
the heating coil connection cables into the output jacks. The
system is now continuously heated and the supplied quantity of
energy is measured. As soon as the temperature in the calorimeter has reached the initial temperature, switch off the heating and
read the exact quantity of electrical energy supplied. After a further three minutes, stop recording the temperature.
Fig. 3 shows the graph as it is presented by the programme
when the measurement is stopped. If you use <survey> from the
toolbar you can read the temperature difference data.
Perform an analogous experiment with an empty test tube in
order to determine the heat capacity of the test tube.
Fig. 2:
(1)
Fh
n
(1a)
(2)
Measurement parameters
Fig. 2:
p = const.
P3020911
PHYWE series of publications Laboratory Experiments Chemistry PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen
LEC
02.09
(3)
Qexp = - CK . Texp
(8.1)
(8.2)
Qexp Wel
(4)
(8)
Texp
(8.3)
Tcal
where
Vs
Vl
For reversible processes, the phase transition entropy is calculated according to the second law of thermodynamics. The following relation results for the melting entropy FS:
FH
FS
TF
(5)
Texp
Tcal
CK
Wel
where
Texp, empty
Cp(s)
Cp(l)
TF
Tl
Th
n
(6)
Tcal, empty
Wel, empty
Q
Cp1s2 1TF Tl 2 Cp1l2 1Th TF 2
n
(7)
Q
n
Texp, empty
Tcal, empty
(9)
(7.1)
PHYWE series of publications Laboratory Experiments Chemistry PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen
P3020911
LEC
02.09
P3020911
PHYWE series of publications Laboratory Experiments Chemistry PHYWE SYSTEME GMBH & Co. KG D-37070 Gttingen