Indian Institute of Technology

Department of Metallurgical and Materials Engineering

Final Exam: MM2080-Principles of Extractive Metallurgy

Total Marks: 90, Duration 3:00 Hrs

Date: January 2, 2021, 2:00 PM to 5:00 PM.

Instructions:

1. Attempt all the questions

2. All questions carry equal marks

3. The parameters may be assumed wherever you find necessary.

4. For calculations, Excel-Solver may be used.

5. Submit the answer sheet (Pdf and Excel Sheets) on Moodle by 5:15 PM. There will be penalty
for delayed submissions.

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1. The daily zinc production rate of a vertical retort was 8 tons. The charge consisted of
briquettes made from a mixture of roasted zinc concentrates (64% ZnO, 5% PbO, 2%CdO, 15%
Fe2O3 and 14% SiO2) and coke breeze (89% C, 7% SiO2 and 4% Al2O3). The retort was
operated at 1300 oC; all of the CdO and PbO and 98% of ZnO were reduced. In addition four-
fifth of the Fe2O3 was reduced to Fe and reminder to FeO. The CO/CO2 ratio of the retort gases
was 16. The gases also contained all of the Cd and 50% of the Pb in the charge. Nearly 2% of the
zinc in the gases was reoxidised during the condensation. The charge contained coke breeze 50%
in excess of the minimum required. Calculate the following:

(a) The daily consumption of roasted zinc concentrates and coke breeze

(b) The composition of the retort residue and its amount

(c) The composition of the retort gases.

2. Limestone was calcined in a rotary kiln fired with natural gas. The kiln was operated at steady
state, producing 280 tons of dead-burned lime per day. The stone fed to the kiln analyzed as 96
wt% CaCO3, 2 wt% SiO2, 1 wt% Fe2O3 and 1 wt% H2O. Calculate: (a) The feed rate of
limestone (b) The chemical analysis of lime made.
3. The melting point of CaTiSiO5 is 1673 oC, and the heat of fusion at normal melting point is
29.6 kcal/g.mole. Calculate the heat of fusion at 1073 oK. Given:

CP (solid) = 42.39 + (5.54 x 10-3. T) – (9.63 x 105. T-2) cal/g.mole. oK

Cp (liquid) = 66.8 cal/g.mole.oK

4. Aluminum is produced by electrolysis of alumina dissolved in molten cryolite. (a) In the Hall-
Heroult process, carbon electrodes are used to accomplish electrolysis. The oxygen liberated at
the anode electrochemically reacts with carbon to produce CO-CO2 mixture in the ratio of 4:1 at
1000 oC. Write the electrode reactions. Determine the minimum voltage required for electrolysis
if the anode gas pressure is 1 atm. Calculate the amount of carbon consumed per kilogram of
aluminum produced. Assume 100% current efficiency.

5. The equilibrium constant for the reaction Fe3O4(s) + CO(g) = 3 FeO(s) + CO2(g) is 1.177 at
1100 oK. If the mixture consisting initially of 1.6 g.moles of Fe3O4, 2.28 g.moles of CO, 0.64
g.moles of FeO and 0.96 g.moles of CO2 is heated to 1100 oK at a constant total pressure of 5.24
atm, what will be the amount of different substances present at equilibrium ? It is tacitly assumed
that no C(s) deposition occurs from the gas phase. Is this assumption valid ?

6. Please read the attached literature and answer the following questions:

1. Summary of the literature (within 500 words)

2. Explain mechanism and anode/cathode reactions.

3. What is the range of Al2O3 addition in cryolite so that melting point decreases ?

4. What are the factors for low current efficiency of the process and how they could be taken
care of ?
 Electrochemistry of the Hal-Heroult Process
for Aluminum Smelting
W. E. Haupin
Aluminum Corp. of America, P.0. Box 772, Freeport Road, New Kensington, PA 15068

Aluminum is the most abundant metallic element on the

surface of the earth, but it is never found free in nature. Its
many desirable physical, chemical, and metallurgical prop-
erties make it the most widely used nonferrous metal. The
aluminum industry, second only to steel in volume of metal
production, is the world’s largest electrochemical industry.
Bauxite, which contains 20-30% aluminum as hydrated oxide
and hydroxide, is the principal ore. It is chemically purified
See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.

by the Bayer process to 98+% pure aluminum oxide (alumina).

Downloaded via INDIAN INST OF TECH MADRAS on January 1, 2021 at 13:38:11 (UTC).

The Bayer process (1) makes a very interesting chemical en-

gineering study. The process employs the unit operations:
crushing and grinding, digestion, heat exchange, clarification,
filtration, precipitation, evaporation, and fluid bed calcina- 1. Aluminum electrolysis cell with prebaked anode.
tion. Figure

Electrolysis of Alumina
Nearly all aluminum is produced by the electrolysis of
alumina dissolved in a molten cryolite-based electrolyte, the
Hall-Heroult Process. A typical modern aluminum reduction
cell (2) consists of a rectangular steel shell, 9-12 m long by 3-4
m wide and 1-1.2 m high. The shell is lined with refractory
thermal insulation that surrounds an inner lining of carbon
to contain the highly corrosive fluoride electrolyte and molten
aluminum. The thermal insulation is adjusted to provide
sufficient heat loss to form a protective ledge of frozen elec-
trolyte on the inner walls but not on the bottom of the cell
cavity, which must remain bare to provide electrical contact
with the molten aluminum cathode. Electric current enters
the cell through prebaked carbon anodes (Fig. 1) or through
a continuous self-baking Soderberg anode (Fig. 2). A crust of
frozen electrolyte and alumina covers the top of the cell
around the anodes. The anode-to-cathode spacing ranges from
3-6 cm. Steel current collector bars keyed into the carbon
lining carry the electric current from the cell. Aluminum-
containing ions discharge into a molten aluminum pool resting Figure 2. Aluminum electrolysis cell with Soderberg anode.
on the carbon lining that also holds the melt. Simultaneously,
oxygen-containing ions discharge on and consume the cell’s
carbon anodes. Today’s cells have a current capacity in the orsloping steel pins or spikes. Periodically the lowest spikes
range of 50-250 X 103 amp. arereset to a higher level. The resistivity of Soderberg anodes
Prebaked anodes are molded from petroleum coke and coal is about 30% greater than prebaked anodes, while the current
tar pitch binder into blocks typically 70-cm wide by 125-cm density typically is lower, ranging from 0.6-0.9 A cm-2.
long and 50-cm high. These blocks are then baked to 1000- Alumina is added in appropriate increments, either man-
1200° C. Petroleum coke is used because of its high purity. ually or by automatic feeders. Molten aluminum is removed
Impurities such as iron andisilieon deposit on the aluminum, from the cells, generally daily, by siphoning into a crucible.
while less noble impurities such as calcium and magnesium
tend to accumulate as fluorides in the bath. Steel stubs keyed Electrolyte Chemistry
into the anodes, either with cast iron or with a carbonaceous The electrolyte is a solution of aluminum oxide in molten
ramming mix, both support and conduct electric current into cryolite containing an excess of aluminum fluoride over the
the anodes. The electrical resistivity of prebaked anodes 3NaF-AlF3 cryolite composition. The mole ratio NaF/AlF3 is
ranges from 0.005-0.006 ohm cm. Anode current density defined as the cryolite ratio while the mass ratio of NaF/AlFs
ranges from 0.6-1.3 A cm-2. Soderberg anodes are formed is called the bath ratio. Numerically, the bath ratio is half the
continuously from a paste of petroleum coke and coal tar cryolite ratio. Pure cryolite melts at 1012°C, but alumina and
pitch. This mixture is added to the top of a rectangular steel aluminum fluoride lower the melting point as shown in Figure
casing, typically 6-8 m long by 2 m wide and 1 m high. While 3. Owing to a small amount of calcium oxide impurity in the
passing down through the casing, the paste bakes forming alumina, calcium fluoride attains a steady state concentration
carbon to replace the carbon being consumed at the bottom. of 3-8% at which level calcium is codeposited in the aluminum
A baked portion extends past the casing into the molten and emitted in the off-gases at a rate equal to its introduction.
electrolyte. Electric current enters the anode through vertical Calcium fluoride lowers the liquidus temperature about 2.9°C

Volume 60 Number 4 April 1983 279

 however, using cyclic voltametry, stationary electrode polar-
ography, differential pulse polarography, and chronopoten-
tiometry found evidence only for three electron transfer
processes. He found no evidence for a chemical reaction fol-
lowing or preceding the electron transfer process. This ruled
out both discharge of Na+ at low activity followed by chemical
reaction to form aluminum and also dissociation to form Al3+
ions prior to discharge.
A1F03-
“
Al3+ + 6F- (6)

A1F- —• Al3+ + 4F“ (7)

Al3+ + 3e~ —
3A1 (8)

The latter mechanism is, however, supported by Rolin (9).

Bowman’s findings support the cathode reaction

Figure 3. The Na3AIF6-AIF3-AI303 system.

AIF63- + §r -
A1 + 6F- (9)

with the F~ ions neutralizing the charge of the current carrying

Na+ ions.
per weight percent calcium fluoride. Sometimes lithium flu- Anode
oride is added to increase the electrolyte conductivity and
further lower the liquidus temperature. The primary anode reaction may be represented simplis-
Molten cryolite ionizes tically by
Na3AlF6 -* 3Na+ + AlFfi3~ (1) C + 202_ -

4e~ —
C02 (10)

The hexafluoroaluminate ion undergoes further dissocia- Oxygen, however, is complexed in the electrolyte. The anode
tion reaction, therefore, must involve such complex ions as
AlFe3- —
A1F4- + 2F- (2) A1202F42- + 2A1Fh3_ + C 4AIF4- + C02 + 4e~ (11)

K =
(aAiT4-)(a2F-)/aA]Ffiax =
4arVf(i -

,_,•)( 1 + 2a)2] (3) 2A120F62- + 2A1F63- + C 6A1F4“ + C02 + 4e“ (12)

The mechanism and the degree of dissociation, a, of the
hexafluoroaluminate ions have been developed from cryos-
copy, density, viscosity, and Raman spectroscopy (8-5). The
degree of dissociation, a, of the hexafluoroaluminate ion at
the cryolite composition is about 0.3. Adding excess aluminum
fluoride to the melt decreases the A1FS3~ and F~ and increases
the A1F4- concentrations.
Dissolulion of Alumina
Virtually any addition to molten cryolite reduces alumina
solubility. Since rapid dissolution and a high activity of alu-
mina are desirable, additives usually are limited to less than
10 weight percent. When alumina dissolves, a strong chemical
interaction takes place between the solute and solvent causing
melt properties to change (5). The evidence suggests several
oxygen-containing anions. Complex, rather bulky oxyfluo-
roaluminate tons, Al203:Fy6_2x_T) are likely rather than the
simple aluminates such as A102~, A10+, A1204Z~, or AIO33-.
Probably a single oxygen atom is present per complex ion at
low concentrations of alumina and two at higher concentra-
tions. Gilbert et ah (6) found by Raman spectroscopy that all
oxygen species had bridging A1—0—A1 bonds. Reactions (4)
and (5) present dissolution mechanisms consistent with the
above.
4A1F63- + AI203 -a 3A130F62- + 6F~
2 A1F63- + 2 A1203 —
3A1202F42-
Thermodynamically, oxygen depositing onto carbon at the
cell operating temperature should form essentially all CO with
very little C02, However, net carbon consumption demon-
strates that the primary anode product is essentially all C02.
Reaction kinetics explain this surprising departure from
thermodynamic equilibrium. The desorption of CO from the
carbon surface must be kinetically hindered. Thonstad and
Hove (10) propose that the initial oxygen-containing ions are
transported through the double layer and discharged with
comparatively little overvoltage. This oxygen is chemisorbed
on the carbon surface as proposed by Blyholder and Eyring
(11) for ordinary combustion, forming C20 (Fig. 4a). This
breaks down slowly to CO gas. Accumulating C20 removes
sites for further oxygen discharge. As more sites become oc-
cupied, it takes more energy (overvoltage) to deposit oxygen.
Finally C302 forms, (Fig. 4b) which desorbs rapidly as C02
forming fresh carbon sites for oxygen deposition.
Anode Effect
The anode effect is a phenomenon common to many fused
salt electrolytic processes. Its physical manifestation is the
growth of larger and larger bubbles on the anode as the contact
angle of the bubble diminishes. Finally, a few large bubbles
coalesce, forming a single large bubble that covers most if not
the entire surface of the anode. With a constant potential
(4) source, the current falls to a low value. With a constant current
(5) source, as used industrially, the applied potential rises to

The solution mechanism of eqn. (4) would be favored by low

alumina (<1%) concentration and low bath ratio (<1.2) while 0 0
eqn. (5) would be favored at. higher alumina concentrations / \ / \
and higher bath ratios.
.c c —

c —
c —

c c —

Electrode Reactions
• o b
Cathode 0 „* 0

The fact that Na+ ion is the principal current carrier (7) and i \ / / \
• *
there is no Al3+ has lead some investigators to assume sodium —
c C c —
c —.c.
Vi
„
/ \ ^ ^
is the primary product discharged at the cathode and alumi-
num results from a secondary chemical reaction. Bowman (8) Figure 4. Formation of C02.

280 Journal of Chemical Education

about 30V and the current penetrates the gas film by a mul-
titude of small electric arcs.
In aluminum electrolysis, the anode gas composition
changes on anode effect from C02 to CO, with significant
quantities (3-25%) of CF4 and minor amounts of C2F0. It is
generally agreed (12) that a carbon-fluorine surface compound
is the triggering mechanism. As AI2O3 is depleted, overvoltage
increases. The increase in surface tension of the bath with
decreasing A1203 concentration coupled with the electroca-
pillary effect, resulting from the higher anode overvoltage,
reduces anode wetting and the bubble contact angle decreases.
At about 1.2 V anode overvoltage, sufficient fluorine activity
is generated to produce fluorine bonding to the carbon.
Fluorocarbon compounds have low surface energy and pro-
mote further dewetting and growth of the large bubbles that
coalesce, producing the anode effect. Restoring the AI2O3
concentration and breaking the gas film removes the effect.
Current Efficiency
According to Faraday’s law, 26.80 A hr should deposit one
gram equivalent of aluminum (8.994 g). In practice, only
85-95% of this amount is obtained. The loss results mainly
from recombination of anodic and cathodic products. Refer-
ring to Figure 5, reduced species go into solution at the alu-
minum-electrolyte interface, Zone A. Presumably the reduced
species are Na and A1F produced by the equilibria.
Al(l) + 3NaF(so1n) M 3Na(soln) + A#3{soIn)
2 A] (V.i +
—
3A!F(soln)
AlFa(s(oln)
Some evidence exists for dispersed (colloidal) aluminum (13).
The equilibrium or saturation concentration of reduced
species in the electrolyte is a function of electrolyte compo-
sition and temperature (14). The reduced species diffuses
through the boundary layer, Zone B, in Figure 5. Many in-
vestigators believe that this is the rate controlling step. Next,
electrolyte containing the reduced species is convectively
transported to the reaction Zone E. Here C02 goes into solu-
tion and most investigators believe it reacts instantaneously
with the dissolved reduced species, producing metal oxide and
CO. The reaction probably takes place within the boundary
layer of the C02 bubbles. A mathematical treatment of the
above has been made by Robl et al. (15) and Lillebuen et al.
(16).
Cell Voltage
The cell voltage is made up of a number of components:
Ecel! = E° + TJCA + TJSA + VCC + TJSC
~
HR A + Rr + Rc + Rx)
Figure 5. Mechanism of current efficiency loss.
E° is the thermodynamic equilibrium voltage; tjca is concen-
tration overpotential at the anode; and tjsa is surface over-
potential at the anode. The latter may be either activation or
reaction overpotential, tjcc is concentration overpotential at
the cathode; tjsc is surface overpotential at the cathode, gen-
erally negligible. Total cell current is represented by I. Ra is
the electrical resistance of the anode or combined anodes. Rb
is the effective resistance of the electrolyte (bath) allowing for
the fanning out of current as it flows from anode to cathode
and the increase in resistance caused by gas bubbles. Rc is the
cathode resistance, and Rx is resistance external to the cell
but must be included in calculating power consumption.
Formulae for calculating these variables is given in reference
' '
(2).
Specific power consumption in kWh kg of aluminum can
1
be calculated
kWh kg”1 =
298.06 Eceli/% CE (16)
where % CE is percent current efficiency. Cell voltages and
their heat equivalence are summarized in Figure 6.
Advanced Study
Graduate study could make significant contributions to the
preceding topics. Other areas for advanced study include the
fluid dynamics of the cell where the interaction of electric and
magnetic fields couple with gas bubble induced convection
to determine electrolyte flow and metal pad movement—
(13)
significant factors in cell life and current efficiency. Another
(14) area would be the study of combined heat flow, and electric
current flow, taking electrode overvoltages into consideration.
This could be extended to include ledging (the formation of
a protective layer of frozen electrolyte on the sides of the cell)
and crusting. Studies of environmental problems could be
helpful. The Light Metals series of books published by The
Metallurgical Society of AIME provide a wealth of both fun-
damental and practical information on these topics.
(15)
Figure 6. Energy Requirements of the Hall-Heroult cell. E1, decomposition of
alumina; E2, depolarization by carbon; E3, equilibrium potential; E4; anode re-
action overvoltage; E5, anode concentration overvoltage; Ee, cathode over-
voltage; E7, cemf of cell; E8, electrolyte voltage drop; E9, electrolyte bubble
induced voltage drop; £10, anode voltage drop; En, cathode voltage drop; E,2,
external voltage drop; enthalpy to produce aluminum + CO and C02; 02,
cell heat losses; and 03, bus heat loss.
Volume 60 Number 4 April 1983 281

Acknowledgment
The figures and much of the text were taken with permis-
sion from an article by W. E. Haupin and W. B. Frank,
Chapter 5 in “A Comprehensive Treatise of Electrochemis-
try,” Vol. 2, edited by Bockris, et al„ Plenum Publishing Co.,
New York, 1981; Figures 1 and 2 by permission of Kirk-Oth-
mer, “Encyclopedia of Chemical Technology,” J. Wiley, New
York, 1978.
Literature Cited
(1) “Extractive Metallurgy of Aluminum,” Vol I, Gerard, G. (Editor), Tnterscience Pub-
lishers, New York, 1963,
(2) Haupin, W. E,, and Frank, W. B., “Electrometallurgy of Aluminum,” in “Comprehensive
Treatise of Electrochemistry, Vol 2 Electrochemical Processing,” Plenum Publishing
Corp., New York, 1981, chapt. 5, pp. 301-325.
282 Journal of Chemical Education
(3) Paucirova, M., Malinovsky, M„ and Matiasovsky, K., Rev. Roum. de Chim., 17, 807
(1972).
(4) Sato, V., Kojima, A., and Ejima, T., J. Japan Inst. Metals, 41,1249 (1977).
(5) Grjotheim, K., Krohn, C., Malinovsky, M., Matiasovsky, K., and Thonslad, J., “Alu-
minum Electrolysis—The Chemistry of the Hall-Heroult Process ” Aluminum Verlag
GmbH, Dusseldorf, 1977.
(6) Gilbert, B., Mamantov, G., and Begun, G. M., Inorg. Nucl. Chem. Letters, 12, 415
(1976).
(7} Frank, W. B., and Foster, L. M., J. Phys. Chem., 61,1531 (1957).
(8) Bowman, K. A., Ph.D. Dissertation, Univ. of Tennessee, Knoxville, March, 1977.
(9) Del Campo, J. J., Millet, J. P., and Rolin, M., Electrochim. Acta, 26,59 (1981).
(10) Thonstad, J., and Hove, E., Canadian J. Chem., 42,1542 (1964).
(11) Blyholder, G., and Gyring, H,, J. Phys. Chem., 61, 682 (1957).
(12) Brunet, C., and Mergoult, P., “Electrode Effects in Cryolitic Baths,” in Extended
Abstracts of the 30th Meeting, International Society of Electrochemistry, Trond-
heim, Norway, 1979, p. 167.
(18) Gerlach, J., Schmidt, W., and Schmitt, H., Erzmetall, 20, 111 (1967).
(14) Yoshida, K., and Dewing, E. W., Met. Trans., 3,1817 (1972).
(15) Robl, R. F., Haupin, W. E„ Sharma, D., Light Metals, Vol 1, p. 185, Met. Soc. of AIME
publisher (1977).
(16) Lillebuen, R, Ytterdall, S. A., Huglen, R., and Paulsen, K. A.t Electrochim. Acta, 25,
131 (1980).
 END SEM MM 2080 -

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