University of the West Indies

Mechanical Engineering

CHNG1003

Experiment E – Thermal Equilibrium Diagram

Date Conducted:

Date Submitted:

Name: DENZEL LERENZO BABOOLAL

Student ID: 807002654

Lab Group: K
 Table of contents

Abstract……………………………………………………………………………….

Introduction…………………………………………………………………………...

Apparatus ……………………………………………………………………………..

Procedure……………………………………………………………………………..

Results…………………………………………………………………………………

Discussion………………………………………………………………………………

Conclusion……………………………………………………………………………..

References……………………………………………………………………………..

Appendix……………………………………………………………………………….
 Abstract

The objectives of the thermal equilibrium experiment were to 1) plot the

cooling curve of the different alloy samples, 2) plot temperature curves for the binary
systems studied and compare them with the corresponding phase diagrams. The
experiment involved heating different alloys to their melting points and then cooling
them with respect to time. Different compositions of Lead – Antimony were used.
The results revealed the cooling curves where the plateau temperatures for 90%Pb –
10%Sb, 70%Pb – 30%Sb, and 30%Pb – 70%Sb were found to be 227.5 and 195oC,
280 and 200oC, and 235oC respectively. These were slightly off the universally
accepted values for these alloys.
 Introduction

The aim of this experiment was to investigate and comment on the thermal
properties of different alloy samples of Lead-Antimony, by the comparison of cooling
curves and their corresponding phase diagrams. The characteristics of a cooling curve
for any given alloy vary with the percentage composition of its constituents. For a
pure metal there is a clearly defined temperature on the graph where the sample
temporarily undergoes no further change while the latent heat of fusion is being
dissipated to form the solid phase from the liquid phase. This plateau in the graph
occurs at the melting point of the metal. Most alloys give two smaller plateaus where
firstly the latent heat of fusion of the higher melting point metal exists and secondly
where the eutectic point exists. This is because one of the constituents starts to form
solid crystals while the other(s) are still in the liquid phase. For a eutectic alloy there
is a single defined plateau again, but this time at the eutectic temperature.
The above is a Pb-Sb phase diagram which shows the regions ‘L’ where alloy is
liquid and the line ‘Pb Sb’ under which the alloys are solid.
 Apparatus

The apparatus used were:

1) 4 crucibles each holding one of the below alloy samples-
 100%Pb Boiling point- 327.3oC
 90%Pb – 10%Sb Boiling point- 254oC
 70%Pb – 30%Sb Boiling point- 400oC
 30%Pb – 70%Sb Boiling point- 560oC

2) 4 Bunsen burners with connecting hoses

3) 3 Thermocouples with connecting wires mounted on retort stands
4) 2 Stop-watches
5) 3 Tripods
 Procedure

The apparatus was set up so that the samples rest on the tripods with the Bunsen
burners beneath them for heating. The thermocouples were above and to the side of
the tripods and were set in place with copper wires in the samples.
The samples were heated gently until their respective boiling points and then
they were removed from the heat and cooled till 180oC with temperatures taken at 30
second intervals from the moment of removal from heat till the required temperature.
The results were taken in a table.
This was done for all four samples and the results plotted on their respective
graphs.
 Results

Temperature - Time values for 70%Pb - 195 1290

30%Sb 190 1320
190 1350
180 1380
TEMPERATURE/oC TIME/s
400 0
390 30
380 60
370 90
360 120
350 150
340 180
320 210
315 240
310 270
300 300
300 330
290 360
290 390
290 420
290 450
280 480
280 510
280 540
280 570
280 600
255 630
255 660
250 690
245 720
240 750
240 780
240 810
235 840
235 870
235 900
230 930
230 960
225 990
220 1020
220 1050
210 1080
205 1110
205 1140
200 1170
200 1200
200 1230
200 1260
Temperature - Time values for 90%Pb -
10%Sb

TEMPERATURE/oC TIME/s
254 0
250 30
250 60
245 90
235 120
230 150
230 180
225 210
225 240
220 270
215 300
215 330
210 360
200 390
195 420
195 450
195 480
190 510
180 540
Temperature - Time values for 30%Pb -
70%Sb

TEMPERATURE/oC TIME/s
560 0 200 1410
550 30 195 1440
530 60 190 1470
520 90 185 1500
505 120 180 1530
500 150
480 180
460 210
450 240
440 270
420 300
410 330
400 360
395 390
380 420
370 450
360 480
350 510
340 540
330 570
320 600
320 630
315 660
310 690
300 720
295 750
285 780
280 810
270 840
265 870
260 900
255 930
250 960
245 990
240 1020
235 1050
235 1080
235 1110
230 1140
230 1170
220 1200
220 1230
215 1260
210 1290
205 1320
200 1350
200 1380
 Discussion

Observing all three curves which can be seen in the appendix section of the
report we can see a trend, one that involves the decrease of temperature with the
passing of time, with one or two temperature plateaus along the curve.
The 90%Pb – 10%Sb alloy sample yielded results which show a general cooling
curve with temperature plateaus at 227.5oC and 195oC. this indicates the phase
change.
For the 70%Pb – 30%Sb alloy sample yielded results similar where there was a
normal curve interrupted by two plateaus, one at 280oC and the other at 200oC. this
was unlike the other samples as there seemed to be phase change occurring more
distinctly at 280oC. At this point the latent heat of fusion is dissipated from the liquid
form resulting in the sample remaining at a constant temperature until the alloy has
changed phase from a high energy liquid to a low energy solid. Atomically there is
realignment to conform to a crystalline structure.
For the 30%Pb – 70%Sb alloy sample there was the general curve again but this
time only one distinct plateau occurred, this was at 235oC indicating phase change.
Due to the fact there is one plateau an inference can be made as to this point being
very near the eutectic in composition.
In the case of the 100%Pb sample, the thermocouple was malfunctioning giving
unusually high readings at one instant and dropping to zero the next, as a result this
alloy test was not deemed valid.
In summary the eutectic temperatures of the 90% and 30% lead sample was
around 231oC but in the case of the 70% lead it seemed to be at 280oC.

The phase change temperatures observed in the experiment seem to somewhat

agree with the phase change diagram in the introduction. The inaccuracy can be
credited to the faulty thermocouples or contaminated samples or faulty crucibles.
There is also the issue of parallax which was minimised by placing a mirror at the
back of the scale of the thermocouple. There are also accuracy issues of the
thermocouple where the graduations on the scale of the device were
at increments of 20o
 The importance of the eutectic line is that it defines the conditions on a phase
equilibrium diagram where the phase change occurs.
Types of thermo couples:
There are three main types of thermocouples and these are:
i. Type K – Chromel(Nickel – Chromium Alloy) / Alumel
(Nickel – Aluminum Alloy)
ii. Type E – Chromel / Constantan ( Copper – Nickel Alloy)
iii. Type C – Tungsten 5% Rhenium / Tungsten 26% Rhenium

How it works:
A thermo couple works because there is a voltage drop across dissimilar metals
which are placed in contact with a substance. This voltage is a function of
temperature, where the relationship between temperature difference and the output
voltage of a thermocouple is nonlinear and is approximated by a polynomial
interpolation……………………..

The coefficients an are given for n from 0 to between 5 and 9.

The powdery substance on the alloy sample was carbon powder which was placed
there by lab techs for the experiment to minimise oxidation of the sample during
heating, allowing multiple uses of the sample with minimal contamination. If the
sample had been oxidised its composition would have changed and therefore the
cooling curve and eutectic temperatures found would have changed.
 Conclusion

In conclusion the experiment was a success in terms of understanding the

characteristics of the Lead-Antimony alloy and also yielded the euctectic temperatures
for the different mixtures. There were some problems with the accuracy and
efficiency of the thermocouples but the results show the eutectic points for 90% and
30% was 231oC, and the point for the 70% was 280oC.
 References

1. Brethaupt, J. “Understanding Physics for Advanced Level”.

2. http://www.soton.ac.uk/~pasr1/build.htm
3. http://en.wikipedia.org/wiki/Thermocouple#Principle_of_operation
4. http://en.wikipedia.org/wiki/Eutectic
5. University of the West Indies, ‘CHNG 1003 SCIENCE OF MATERIALS
LABORATORY MANUAL’ pgs 7 – 10.
Appendix