MERRILL CROWE MODULE

February 2005
Barrick Misquichilca Mining S.A.
High Chicama

MERRILL CROWE MODULE

INDEX

INTRODUCTION

CHAPTER 1.0 FUNDAMENTALS OF PRECIPITATION WITH Zn

1.1. Electrochemistry 3
1.2. Stability diagrams for the Merrill Crowe process 5
1.3. Free cyanide 7
1.4. Variables in precipitation with Zn 7

CHAPTER 2.0 DESCRIPTION OF THE PROCESS IN ALTO CHICAMA

2.1. Description of the process in the Merrill Crowe plant 12

2.2. Flowchart 13
2.3. Plant equipment 13

CHAPTER 3.0 STAGES OF THE MERRILL CROWE PROCESS

3.1. Clarification of the rich solution 19

3.2. Deoxygenation 23
3.3. Precipitation with zinc 24

CHAPTER 4.0 PROCESS CONTROL

4.1. Operating parameters 27

4.2. Plant calculations 29
4.3. Operating procedure with high solids 30
4.4. Analysis of solutions 30

ANNEXES

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MERRILL-CROWE MODULE

INTRODUCTION
Due to its simplicity and efficient operation, the Merrill-Crowe process has been used
around the world for the recovery of gold and silver from cyanide solutions. The
cementation or precipitation of gold using metallic zinc was applied in the plants
since 1890.
The method was characterized by:
Use pieces of zinc (shavings, plates, etc.)
Contact in trays or boxes.
High zinc consumption, 10 kg of zinc / 1 kg of Au.
Difficulty in harvesting and removing the gold adhered to the zinc.
Median yields.
Zinc passivation (Zn(OH)2, sales, etc.)

During the first three decades, three significant improvements were made to
improve the process:

The first improvement was the addition of soluble lead salts in controlled amounts.
to produce a lead-zinc alloy on the surface of the zinc particles
that inhibited the passivation of zinc surfaces and thus allowed for deposition
continue of gold.

The second improvement was the use of zinc powder instead of zinc shavings, which
provided a much larger surface area, and thus a kinetics of
very rapid precipitation.

The third improvement was the deaeration of the solutions to less than 1 ppm of oxygen.
which significantly reduced zinc consumption.

By 1916, the structure of the improved and known process was already established.
commonly known as Merrill Crowe.

In 1897, C.W. Merrill applied the use of filters in precipitation with zinc dust.
°1916 T.B. Crowe applies vacuum to deoxygenate the rich solutions and reduce the
zinc consumption.

The contribution of Merrill and Crowe gave rise to the current precipitation process with powder of
It is known as the Merrill-Crowe Process.

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CHAPTER 1.0

FUNDAMENTALS OF PRECIPITATION WITH Zn

1.1. Electrochemistry:
This process is based on the fact that the metal to be recovered (gold) from
The cyanide solution is more noble than the metal used for precipitation (Zinc).

This is how the normal oxidation potentials at 25 have been determined.°C. A

the following are detailed some:

Electrode (Half Cell) E° volts

Au = Au+ + e- 1.68

Ag = Ag+ + e- 0.799

2H+ + 2e- = H2 0.00

Fe = Fe+2+ 2e- -0.440

Zn = Zn2++ 2e- -0.763

Interpretation of the scale of normal electrode potentials:

A E° the larger (more positive) is a nobler metal, meaning it is more difficult to pass.
the ions to the solution (difficult corrosion). Oxidizing species.
A One° smaller (more negative) metal less noble, easier for ions to pass
to the solution (easy corrosion). Reducing species
It is basically an electrochemical process where zinc dissolves (anodic reaction) and
The donated electrons are used to reduce the aurocyanide complex to metallic gold.
(cathodic reaction).

The anodic dissolution of zinc is the result of two reactions.

Zn = Zn++ + 2 e-
Zn + 4CN- Zinc cyanide4 -2
++

Zn + 4 CN- = Zn(CN)4+ -22 e- General dissolution of zinc

The cathodic reaction of the auricyanide complex would be:

-
Au(CN)2+ e- = Au + 2CN- Cathodic Reaction (1)

It should be emphasized that both reactions occur simultaneously and that zinc
When it dissolves, it donates its electrons to the auricyanide complex to be reduced.
to metallic gold, the general equation is as follows:
-2
2Au(CN)2- + Zn = 2Au + Zn(CN)4Global Reaction (2)

The main reactions that directly intervene in the Merrill Crowe process are:
- -2
Zn° + 2 Au(CN)2 = Zn(CN)4+ 2 Auo

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Zn° + 2 Ag(CN)2 - = Zn(CN) -2 + 2 Ago

4 -2
Zn° + Hg(CN)4 -2 = Zn(CN)4+ Hgo

The addition of lead salts helps the spontaneity of the cementation; forming
cathodic areas; their addition must be controlled, as excess reduces efficiency.

Normal potentials Eoin the middle

alkaline (pH=14)

This graph presents the main normal potentials of the complexes that
they intervene in a precipitation.

From these, we can easily deduce that the greatest tendency to form pairs
-
Galvanic with Zn, commonly referred to as the pairs: Au(CN)2/Zn;
- -2
Ag(CN)2/Zn; Hg(CN)4As expected, these will depend on the complexes and
their respective concentrations in solution.

PRECIPITATIONMECHANISMOF
GOLDONZINC

Au(CN)-2
CN- CN-
Au(CN)-2
CN-

Golddeposits
e
CN-
e
CN-
CN-
CN-
Particle CN-
ofZinc Zn(CN)2- 4

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From the previous graph where the mechanism of zinc precipitation is shown, there
can extract the following:

i. The mass transport of the gold cyanide complex and free cyanide species
towards the surface of the zinc from the solution.
ii. Adsorption of the gold cyanide complex on the surface of zinc.
iii. Electron transfer between zinc and the gold cyanide complex, and dissociation
simultaneous formation of the gold cyanide complex and cyanide complex formation
zinc, reaction (1) and (2), from page 4.
iv. Desorption of the zinc cyanide complex from the surface of the zinc.
v. Transfer of the zinc cyanide complex to the solution.

1.2. Stability diagrams for the Merrill Crowe process

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Free Cyanide

The term free cyanide involves two species, the cyanide ion (CN-) and the acid
hydrocyanic acid (HCN). The relative proportion of these two forms depends on the pH of
system.
The reaction between the cyanide ion and water is expressed:
CN- + H2O = HCN + OH-

This dissociation is a function of the pH, for leaching the important factor is the CN.-

• At a pH = 8.4, more than 90% of cyanide exists as hydrocyanic acid (HCN).

• At a pH = 9.3, half of the total cyanide exists as hydrocyanic acid (HCN) and the
another half as free cyanide ions (CN-).
• At a pH = 10.2, more than 90% of the total cyanide is in the form of free cyanide ions (CN−).-).

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1.4. Variables in precipitation with Zn

The variables that have an important influence on the efficiency of the process of
precipitation with Zn, are the following:

Dissolved oxygen
Minimum concentration of cyanide
Suspended solids
Operational pH range
Interfering metallic ions

• Dissolved oxygen: Even small amounts of dissolved oxygen deteriorate.

considerably the precipitation, due to the passivation of the surface of Zn (oxidizes
the surface of Zn decreases the contact area, thus preventing all the Zn
reaction for precipitation); Additionally, the presence of oxygen can redissolve the
finely precipitated gold, whose velocity would be very fast.
• Minimum concentration of cyanide: For the precipitation reaction to proceed
until the end, the rich solution must contain a minimal concentration of cyanide;
below this concentration the precipitation rate is lower. Above this
cyanide concentration the precipitation rate is not affected, but a
high concentration of cyanide leads to excessive consumption of Zinc. Some
Experts say that this minimum concentration of cyanide is 0.002 M, others 0.035 M
sodium cyanide

• Suspended solids: Suspended solids can drastically reduce the

efficiency of the process, as they cause passivation of the zinc.

Zinc passivation

During passivation, the metal forms a compound (or product) that remains in the
metallic surface forming a barrier or resistance to the continuation of the
corrosion, for example ZnO, Zn(OH)2The passivation of the active anodic surface

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of zinc, causes a slower reaction rate and in the extreme case stops
totally the precipitation. Passivation occurs due to isolation of the
surface of the zinc as a consequence of the coating of:

Dense and compact layer of precipitated metals.

Zn(OH) layer2.
Coating with ZnS
Coatings with slats, gels, and hardness.

• pH of the rich solution: A variation in the pH value of the rich solution in the range
from pH 9 to 11.5 has no notable effects on the precipitation rate, but a pH
may cause the formation of Zn(OH)2this product tends to originate in the
surface of the Zn particles and can delay and even halt the precipitation
with zinc.

Zn(OH)2it is practically insoluble, therefore it inhibits the rate of precipitation.

The stability of zinc hydroxide depends on the concentration of cyanide, pH and
concentration of dissolved zinc. The formation of the passivating hydroxide is described by the
reaction:

Zn+2+ 2OH- Zinc hydroxide2

In higher concentrations of cyanide, the zinc ion is complexed to form complexes.

soluble, according to:

-n+2
Zn+2+ n CN- Zn(CN)n

Zinc hydroxide dissolves in the presence of cyanide as follows:

Zn(OH)2+ 4CN- = Zn (CN)4-2+ 2 OH-

• Interfering metal ions: Some metal ions have negative effects on the
precipitation with Zn. The most harmful ions are those of antimony and arsenic;
whose concentrations <1 ppm can reduce the precipitation rate by 20%
%.
The presence of copper in solutions generally causes high consumption of
cyanide and also decreases the precipitation efficiency due to the passivation of Zn.
• Influence of lead salts on precipitation: The presence of small
lead amounts in the solution have a positive effect on precipitation; Without
embargo if the lead concentrations are very high (> 20 ppm) the consumption of Zn
increase.
In minimal amounts, lead precipitates as a thin metallic film over
the zinc, thus creating an active galvanic pair, which makes the process faster and more complete.
gold precipitation, with lower zinc consumption.

Example 1

A zinc plate is submerged in an acidic solution with copper ions (acidic solution with
copper sulfate: CuSO. Determine
4 if zinc corrodes. The reactions that take place
son
Zn = Zn 2+ + 2e- ....................................... E°= -0.763 V.

Cu = Cu 2+ + 2e- ...................................... E°= 0.337 V.

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Of these two reactions, the one with a more positive potential is that of copper (Cu), for which
Thus, copper will be reduced and zinc will oxidize (corrode).

Anode Zn2+ + 2e- = Zn .............................. E°= -0.763 V.

Cathode Cu2+ + 2e- = Cu ........................... E°= 0.337 V.

[Link] Cu2+ + Zn = Cu + Zn
2+ ........................ Ecell = E°-CE°= 1.1
A V

Example 2

In the Merrill-Crowe precipitation process, the following reactions occur. Describe it.
global reaction and the spontaneity of the reaction.
-
Au(CN)2+ e- = Au + 2CN- .......................... E = -0.50

Zn + 4 CN- Zn(CN)4+ 2 e--2................. E = -1.22

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CHAPTER 2.0

DESCRIPTION OF THE MERRILL – CROWE PROCESS

2.1. Description of the Merrill–Crowe process in Alto Chicama

The rich solution from the leaching piles is filtered in the filters.
clarifiers until achieving a crystalline solution with less than 5 ppm of solids; The filtrate
it is essential to remove the fine solids that can quickly clog the line
from precipitation or passing through zinc. The filter is coated with a layer of diatomaceous earth.
before proceeding to the filtering. This allows the filter to remove particles smaller than a
micro in size and continue filtering a good amount before becoming saturated.

After the filtration, the rich solution is deoxygenated. The rich solution varies from 5 to
8 mg/l of oxygen, this must be reduced to 0.5-1.0 mg/l, for a production of a
good Barren and use reasonable amounts of zinc.

To achieve this, the filtered solution is circulated through a vacuum tower (or
Crowe) that contains plastic packaging (packing), these interrupt the flow of the
solution forming very thin layers.

The deoxygenated solution must be drained from the vacuum tower with a pump.
seal for fluids, in order to ensure that no air leaks occur
solution. Generally, precipitation problems can be reduced
considerably with a perfectly sealed vacuum pump.

Then, the zinc dust is added to a deoxygenated solution of cyanide gold,

zinc is dissolved and gold comes out of the solution as fine solid. These solids are filtered.
from the solution, generally through a plate filter, for the removal of gold.
The solids are periodically removed from the press, being melted down to recover.
the gold. The effluent from the filter press is regularly analyzed to determine the
gold present and to ensure that it is precipitating properly. This solution
The barren should normally be less than 0.01g/m3.

Zinc powder is added to a cone, which is designed in such a way that there is no
agitation or whirlpools on the surface that induce oxygen into the solution. The
the amount of zinc required depends on the rich solution.

The zinc dosing to the cone is carried out by screw feeders. For the purpose of
An appropriate addition of zinc requires a sufficient amount of cyanide.
free in the solution to dissolve the added zinc and also for all metals
heavy contaminants present in the solution remain in it.

Most of the problems in zinc precipitation can be due to 3 causes:

Too much oxygen in the solution (insufficient vacuum in the vacuum tower or cone)
of precipitation sucking air).
2. Zinc deficiency (the amount of gold in the solution has increased or the solution
is contaminated).
3. Insufficient free cyanide or lime in the solution. There may be too much
free cyanide in the solution, but this will result in excessive use of zinc.
At a neutral pH, the precipitation will be scarce; it is necessary to have the appropriate pH (9-
12)

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The fine material containing gold and silver is filtered from the solution using filters.
filter that has a layer of diatomaceous earth. This filtration medium does not allow for
the fine particles of gold and silver cover the fabric used for filtering, resulting in the
prolongation of the life of the filter press and the precipitate can be washed more easily
from the filtration fabric.

The filter presses continue to receive flow until the units reach capacity.
of precipitate storage or the fabrics become clogged.

When the pressure starts to reduce the flow, the filters are taken out of service to be able to
Wash each unit. Apply a layer of diatomaceous earth and return to service.

2.2. Flowchart
Merrill Crowe Process

Filtering

Filter 1

Filter 2 Tower of
Tk Clarified empty
Zinc
Tk Not Clarified

Filter 3 Nitrate of
lead

Cone of
zinc
Filter 4

The winds of the south

Tk Body Feed
Tk Precoat

Tk Sln
Barren

2.3. Plant equipment

Rich solution tank without clarification. - The rich solution is pumped by one of the
two vertical turbine pumps to the unclarified rich solution tank at the start of the
Merrill-Crowe circuit. This consists of a circular tank with a diameter of 8200 mm.
8200 mm high. The tank capacity is 406 m3 and a retention time of 15
my agreement with the total design flow. This tank feeds the pumps 0310 465
001A and B. has a level control system, if there is too much solution a valve
automatic throttling controls the flow in order to maintain stable levels in the plant. This
tank tends to fill up quickly, however the tank controller makes it
control valve in the discharge of the pumps that goes to the plate filters opens.
Rich solution without clarification is continuously pumped to two of the three leaf filters.
(a filter always on standby). Their function is to carry out the removal of
the solids that are still in suspension in the solution.

Pressure leaf clarifiers.- A plate clarifier consists of a shaft.

central where multiple fine meshes or plates are placed (the clarifiers of Pierina
consist of 51 plates each). The function of these meshes is to collect the

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fine particles present in the solution. The axis and the plates are placed in a
cylinder with appropriate pipe fittings for feeding, unloading the solution,
drained and the solution washed with jets. During the operation, the solution is introduced to
low pressure (inlet of the pipe to the clarifier. The solution passes through the plates
leaving the particles on the sides of the plates and discharging outside the clarifier by
the central axis.

PRESSURE LEAF FILTER

The plate clarifier operates with a washing sequence or process stage series.
The first step is to coat the meshes with diatomaceous earth material.
pre-coated) that applies a layer of this fine material on the surfaces of the plates
to assist in the filtration. The solution is then introduced; the fine solids are
retained on the pre-coated plates and the clean solution passes through the plates and exits from the
clarifier.

The end of the cycle consists of a washing of the plates (backwash). The poor solution is
introduced at high pressure by a manifold that distributes it through several injectors
that clean the particles from the plates. During a portion of this time, the shaft is
rotated by a chain-driven motor to help cut the weeds and the soil
diatomaceous earth of the plates. Access to the inside of the clarifier is through the door
posterior with automatic insurance.

Diatomaceous earth preparation tanks.-There are two preparation tanks for the
pre-coated: one is called the coating mix tank (precoat mix tank: 0310
482 009) and the other for filler feeding (body feed tank: 0310 482 010).

Both tanks are 96" in diameter and 120" high and each of them also has a
1 kW agitator. Each tank contains two pre-coated feed pumps.
(one in operation and the other on standby).

Additionally, they have a bag discharge hopper (0310 484 009A and 010A)
that operate powered by a 0.75 kW motor

Clarified rich solution tank.-The discharge from the clarifying leaf filters to
pressure is transferred to the clarified rich solution tank (0310 482 002) which has

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a size of 5500 mm in diameter by 5500 mm in height. This is a tank

of rich solution storage prior to entering the deoxygenation stage. The
solution levels are regulated by sensors, having a retention of 6 minutes.

TECHNICAL SPECIFICATIONS OF CLARIFYING FILTERS

U.S. FILTER
Characteristics Values
Filter type Double conical Auto-Jet
Filter model: 66AJ-1800F WCD
Type of door: 66" Auto-Lok
diameter
Frontal: 66"
Central: 74"
Back: 66"
Design pressure: 680 kPa (100 psig)
Design temperature: 66°C (150°F)
Container material Carbon steel
Interior material: Stainless steel 316
Coating: None
# of elements: 51 @ 3" spacing
Approximate flow rate: 429 m3/ h (1887 Gpm) @ 517 kPa (75 psig)
Approximate pre-cover ratio: 217 m3/ h (1000 Gpm) @ 207 kPa (30 psig)
Drain ratio: 125 m3/ h (552 Gpm) @ 379-414 kPa (55-60 psig)
Shaft RPM 3 (looking at the door in a clockwise direction)
Axis power 2.24 kW (3hp) @ 460 Volts/3 phases/60Hz
Central support: If(1)
Design and process information:
Total design flow of the team: 1200 m3
Nominal flow of the equipment: 1287 m3
Solid food content: 50 ppm at most
Auto-Jet filter capacity: 2.4 m3/ h/ m2
Contents of filter cake solids of the Auto-Jet filter: < 3 ppm
pH of the filtrate 10 to 11
Material of the precoat: Diatomaceous earth
Feeding body material: Diatomaceous earth
Temperature of the solution: 5°C to 25°C
Sodium cyanide (NaCN) concentration: 150 mg/L of total CN- approximately
Allowed corrosion: 3 mm (1/8")

Sludge tank.- It is the reception tank (0310 482 005) for the incoming sludge.
from the clarifying filters mainly, in addition to the sump in the area of the filters
clarifiers. The design of this tank with a diameter of 3000 mm and a height of 3000 mm is
composed of a stirrer and two mud pumps (0310 463 005A and 005B) that
the sludges are pumped to the leaching piles with an approximate flow of 45 m3/h y 20% of
solids.

Liquid ring vacuum pump. -This type of pump is ideal for the tower of
deaeration, because it can handle large amounts of liquid that is mixed with air in
the tower. This has a cylindrical electric rotor, so that the solution can pass through
outside the blades; the rotor spins freely in a cylindrical casing. The axial of
Encasement is a branch of the axial rotor.

The water partially fills the casing and acts as a piston. As the rotor spins
quickly inside the housing, the rotor blades cause the water to spin
around the cylinder in a whirlpool shape. The centrifugal force causes the water to form
a layer of uniform thickness inside the housing; this moves or pushes out
from the center of the rotor and returns again and again during each revolution. As the water
moves away from the center of the rotor (A) The rotor chambers are filled with liquid. This
the liquid spins with the rotor, but follows the contour of the casing due to the
centrifugal force. The water that completely fills the rotor chamber (the volume between
the blades), comes back from the center of the rotor when the engine moves forward, and pushes the air

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at the entry point to occupy the empty space. The rotor chamber is empty of
liquid and full of air. As the rotor continues to move in the direction of the clock hands.
From the clock, the water is forced into the rotor chamber until the chamber is full.
The air in the chamber is compressed by the liquid as the chamber advances.
and the air is forced to be evacuated through the discharge point. This cycle occurs once.
in every revolution.

Two vacuum pumps are available (0360 461 008 and 009), one in operation and one in reserve.
stand by.

Zinc feeder and the emulsifying cone. - Zinc powder is used for
precipitate the gold that is in the solution as a gold-cyanide complex. This powder is
fed to the emulsifier cone. The gold is precipitated almost immediately as gold
solid and zinc forms a complex with cyanide. By the time the solution arrives at
the vertical feed pump for filter presses 0310 463 006A the gold is
completely rushed.

The zinc powder slurry is prepared by manually adding the zinc powder to
tank over the zinc feeder (0310 442 003 and 004). The zinc feeder of
variable speed is adjusted to feed dry zinc powder into the cone
zinc emulsifier (0310 433 001) where it is mixed by agitation with water. The level
In the zinc emulsifier, it is kept constant by the interlocking of a sensor.
of level and a solenoid valve in the line that controls the entry of the Barren flow. The
zinc powder slurry flows out of the bottom of the emulsifier being injected or
sucked by the flow of deaerated solution flowing by gravity from the interior of the
tower deaereadora. The amount of zinc fed to the emulsifier is checked
manually by the operator. In a basic routine, the operator obtains a sample of
poor solution and is analyzed by atomic absorption. The amount of zinc to be dosed is
based on the law of gold and silver obtained in the solution and the treatment flow of
rich solution.

Vertical feeding pump to the press filter.- This pump (0310 463 006A of 330
Kw), immersed in a tank of water; the reason they are submerged is to avoid
so that air filters into the solution; thus if the seals of the pumps fail, it could not enter.
air to the bombs.

The precipitation of gold with silver, together with mercury, is instantaneous and the
the pump is an excellent mixer that carries out this process. All metals
precious metals must be precipitated at the moment the solution exits the pump.
solution that is downloading the feed pump to the filter presses, contains
small particles of gold, silver, and mercury with a little excess of zinc, which is
pumped to a bank of precipitation filters called filter presses (0320 413 009,
010, 011 and 012), three in operation one in reserve.

Press filters.-This type of filter is of the type used to separate solids from
the liquids. The individual filter plates are suspended in side bars of the
The filter frame, the filtration takes place between these plates.

A cylinder shaped like an arm at one end of the filter is where it is found.
housing a double-acting hydraulic cylinder. A stationary frame (head frame)
it is the opposite side of the filter which contains the two supply pipes and
download. The other head is placed on the side bars and connected to the arm
hydraulic; thus managing to move this head along the side rods and
compressing the intermediate plates to form the stack for the step of

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filtration. A manual hydraulic pump provides the necessary hydraulic power for
actuate the double-acting cylinder.

After the pressure filter is closed by the hydraulic cylinder, a slurry of

coating is pumped to the filter. This coating continues for the necessary time.
sufficient for the diatomaceous earth to be deposited in the cloths to achieve filtration
cleaner, without releasing the pressure to prevent the coating from coming off, the grout is
pumped into the filter, then the coating pump is stopped, initially the
food fills the chamber between the plates that are covered with a cloth of
filtration. Once the tank is full, filtration begins. As the slurry is
pumped at low pressure to the chamber, the liquid passes through the cloths leaving
the solids in them.

PRESS FILTER SPECIFICATIONS

DORR-OLIVER EIMCO FILTER
Characteristics Values
Filter model: EIMCO M1200-FB-60PP-RP-ALP-100-25MM
Cameras 64
Operating pressure 100 Psi(689 Kpa)
Operating temperature Environment
2 2
Filter area (square feet) 1521 feet (141.3 m )
3 3
Containment capacity (cubic feet) 73 ft (2.07 m )
Thickness of the cake: 1 1/4" (32 mm)
Construction of the filter plate: Poly - P
Filter screen:

The four corners of the plates have circular passages that close when the filter is closed.
Let the clear solution circulate, leaving the precipitate through the filter plates.

When all the plates are filled with precipitate, the inlet valve closes and to
In the press filter, air is injected for additional drying. The pressure in the unit.
hydraulic pressure is released and the plates are loosened. The lifting mechanism then,
automatically lifts each of the plates one by one by removing the movable head.

This mechanism removes the plates from the side of the movable head; this process continues
until all the plates have been removed.

Each of the cloths of the plates containing the precipitate is cleaned, using
some spatulas are placed in trays that are underneath the press filters;
once all the plates have been cleaned the filter is again suitable for
receive a new filtering cycle.

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CHAPTER 3.0

STAGES OF THE MERRILL CROWE PROCESS

3.1. Clarification of the rich solution

A clarification system using precoat is typically used when the

solutions contain less than 50ppm of suspended solids in order to obtain a
clear solution of <3ppm of solids. The filter aid used for the precoat is a
highly porous fine powder that cannot be compacted with normal pressures
of work.

The formed layer has an irregular shape with 80 to 90% vacuum which is capable of
to capture sub-micronic particles. Some propose it should be applied from a
pulp of 1 to 2% filtering aid and others propose that it can be >0.3%, defined in
function at a thickness of 1.6 to 2 mm of precast.

Another important factor is the dosage of body feed, which will have a huge influence.
in the duration of each filtering cycle. Currently, the times for each filtering cycle
they are very variable despite the turbidity level being approximately constant.

Elements of the filtration system

Filtering veil.
Filter tightness.
Feed pumps to the filters.
Clarifying filters.
The precoat tank.
The body feed tank.
Body feed dosing system.

Procedure

The pre-coating is done by recirculating a filter aid pulp until it becomes clear.
the liquid between the filter and the precoat tank. Given that most of the particles
The filtering aids are smaller than the openings of the fabric and must form bridges.
between these openings.

DIRECTION OF FLOW DURING COATING

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Problems in the formation of the precap

Presence of air bubbles.

Pressure variations.
Vibrations inside the filter
Erosion of the precap (very high speed).
Insufficient amount of diatomaceous earth.
Tightening of the fabrics.
Defective VTela (perforations, wrinkles, leaks).

Amount of precoat

The amount of precoat should be: 4.5 to 6.8 kg/9.29 m2

The pulp concentration must be >0.3% for good formation of the
bridges.
The thickness of the precap, 1.6 and 10 mm, must be determined by experience.
Concentrations lower than 0.3% hinder the formation of the aid 'bridges'
filtering by particle agglomeration.
Concentrations greater than 10%, tendency to accumulate in the vicinity of
filter entry: uneven pre-coating.

TABLE 1: DIATOMACEOUS EARTH CONCENTRATION AND PRECOAT THICKNESS

FOR USED DIATOMACEOUS EARTH BAGS
BAGS Diatom Thickness (mm)
(No) (%)
2 0.35
3 0.52
4 0.70 1.68
5 0.87 2.10
6 1.05 2.56
7 1.22 2.92
8 1.40 3.36
9 1.57 3.78
10 1.74 4.20

Speed of precap formation

The preparation speed of the precoat will depend on the viscosity of the liquid used,
so that it keeps the particles in suspension until the complete formation of the
precapa.

A general rule can be to form the precap at a speed that produces

a pressure drop in the filter between 1 and 2 psi. (Difference between the pressure gauge of
input and output.

Preparation method of the precoat

The solution containing the filtering aid must be clarified for 2 to 5 minutes. It is
necessary 5 to 10 more minutes to ensure that all the filtering help has been
located as precoat.

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The lack of clarity in the filtered solution may be due to:

Inadequate sale of the filter.

Blind spots or blocked areas in the fabrics.
Insufficient precoat on the top of the filter fabrics due to deficiencies.
recirculation.
Tears in the fabrics.
Damaged nets or separated wires in the sheets.
Deficient flow distribution due to failure in the solution inlet plate.
Wrinkles in the fabrics.

Commissioning of the filter

After the precoat solution is clarified, the filter is put into operation.
The change from the pre-layer solution to the rich solution to be filtered must be done in such a way
so that the flow is continuous and there are no sudden pressure variations.
For this purpose, the inlet valve of rich solution is first opened while
At the same time, the precoat tank is closed. Actions should be avoided.
quick and abrupt, as these "hits" break the bridges formed by the
diatomaceous earth, allowing the diatomaceous earth and impurities of the liquid to pass.

Body feed dosing

The proper dosing to MAINTAIN POROSITY, which translates to

long filtration cycles, delay the increase in pressure drop and clarity
appropriate filtering.

A very low dosage will produce

• A quick clogging of the cake and the reduction of the filtration cycle
• The diatom is quickly surrounded by solids and decreases the
permeability of the cake.
• The total flow is slowly decreasing.
• The diatom in small quantity only increases the thickness of the cake without adding
some porosity.

An excessive dosage will not increase the porosity of the cake but will shorten it.
cycle due to the reduction of the affected filtration area when contact occurs between
the cakes.

Filtration speed

For example, if the flow velocity is 0.244 m3/h.m2the filter operating for 480
minutes at a pressure of 30 Psi. At twice that speed, the cycle time will decrease.
approximately in 150 minutes.

The filtration speed must be adjusted in such a way that guarantees, at the end of the
filtration process a pressure drop to 50 Psi. very high filtration speeds
they will produce a deterioration of the quality of the filtering.

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Filtering
When the filter is put into service, the filtering clarity should be immediate. If it occurs
the opposite is possible that the following may occur:

Partially covered VTela.

Presence of air in the feed solution.
Loss of flow during the precoat operation, causing precoat rupture.
Inadequate precoat formation due to thin layer of precoat.

Short cycles can be caused by temporary or permanent obstruction of

addition of body feed, obstructed/covered cloth, changes in the characteristics of the liquid
to filter, air trapping in the filter that decreases the filtering area, and too much
filtration speed.

Pre-layer extraction: washing

At the end of the filtration cycle, the filter cake is removed by the following procedure:

Drainage of the liquid.

A combination of leaf drainage and irrigation.
Watering of the leaves with rotation of the support axis.

It is important that the cleaning is thorough as the fabrics can become clogged.
to start a next cycle and the result could be an inadequate service of the filter.

DIRECTION OF THE FLOW DURING CLEANING

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Technical data of diatomaceous earth

TYPICAL PROPERTIES OF DIATOMACEOUS EARTH

GRADE PERMEABILITY COLOR +150 pH HUMIDITY
(DARCY) TYLER (%) MAX
DIACTIV N°8 3.50 BLANCO 33 9.6 1,0
DIACTIV No. 9 3.00 WHITE 28 9.6 1.0
DIAOTV N°10 2.50 WHITE 26 9.6 1.0
DIACTIV No. 11 1.00 WHITE 70 9.6 1.0
DIACTIV N°12 0.80 BLANCO 4.3 9.6 1.0
DIACTIV No. 13 0.40 WHITE 2.2 9.6 1.0
OIACTIV No. 14 0.25 WHITE 1.0 9.6 1.0
DIACTIV No. 15 0.11 WHITE 1.0 9.6 1.0
DIACTIV No. 16 0.06 GRAY 1.0 8.5 2.0
DIACTIV N°17 0.02 GRAY 1.0 7.5 7.5
The indicated physical and chemical properties represent typical averages obtained according to tests and
Accepted methods are subject to normal variations associated with any industrial process.

3.2. Deoxygenation

The objective is to remove all the oxygen from the clarified rich solution. By removing the air
Oxygen is also removed from the solution. The solution coming from the tank of
Storage is pumped by a pump 0310 465 002A to the deoxygenation tower.
The deoxygenation line is completely sealed connected to a pipe that exits through the
top part of the tower connected to a vacuum pump 0360 461 008 or 009 (one in
stand by). This tower is kept completely sealed so that the pump maintains a
absolute vacuum, it is important to maintain it at an almost absolute value so that the
the solution has the least amount of oxygen.

Vacuum measurement.

The degree of evacuation or vacuum is measured by comparing the pressure of the space with the
atmospheric pressure. Atmospheric pressure is the pressure exerted on a body by the
weight of gases in the atmosphere.

• At sea level, the atmospheric pressure is approximately 101 kPa or

its equivalent to 10 meters of water at the same pressure it exerts a
mercury column of 736 mm (mercury is very heavy,
approximately 14 times denser than water.
• At the height of the Alto Chicama mine (around 4000 m.a.s.l.), the pressure
atmospheric is lower than sea level by 6.6 meters of water.
• A total or perfect vacuum at this point can be obtained with a pressure
485 mm of Hg, a pressure of 485 mm is usually considered a vacuum.
of Hg.
• A vacuum system is never perfect, and the vacuum of Alto Chicama will be
obtained with 100 to 150 mm of Hg less than the perfect system, it is
to say, at 365 or 385 mm of Hg. This is typical for a vacuum system
At this point, larger gaps require more equipment and costs.
additional. Any leakage at the joints or pipes means
reduction of vacuum so that operators must ensure that
is getting the largest possible void.

The clarified solutions are deaerated to achieve efficient precipitation.

Crowe method employs a vacuum, which is the most efficient for removing O.2dissolved to
less than 1 ppm.

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The following table shows the correction factor that can be used to compensate
the effects of the variation of atmospheric pressure with altitude

Pressure in mm kPa Altitude Correction

inches Hg Hg Feet Meters Factor
30.23 768 102.3 -276 -84 101
29.92 760 101.3 0 0 100
29.33 745 99.3 558 170 98
28.74 730 97.3 1126 343 96
28.11 714 95.2 1703 519 94
27.52 699 93.2 2290 698 92
26.93 684 91.2 2887 880 90
26.34 669 89.2 3496 1066 88
25.75 654 87.1 4115 1254 86
25.12 638 85.1 4747 1447 84
24.53 623 83.1 5391 1643 82
23.94 608 81.1 6047 1843 80
23.35 593 79.0 6717 2047 78
22.76 578 77.0 7401 2256 76
22.13 562 75.0 8100 2469 74
21.54 547 73.0 8815 2687 72
20.94 532 70.9 9545 2909 70
20.35 517 68.9 10293 3137 68
19.76 502 66.9 11058 3371 66

DEAREATION TOWER

CONNECTION TO VACUUM PUMP

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3.3. Precipitation with zinc

Zinc powder is added to a deep conical bottom tank; in the

that flows solution barren and other additives. This tank is designed in such a way that it does not
There is turbulence or eddies on the surface that induce oxygen into the solution.

This should ensure enough zinc for an initial precipitation, which could be
optimized from a ratio of 1. In some plants, the use of a solution of
soluble lead salt (lead nitrate is preferable) as a constant drip in the cone
of zinc.

Lead salt is usually added in a proportion that varies from 10% to 30%
from the weight of the zinc used. Lead creates a galvanic coupling in the zinc (it was mentioned in
the first chapter), producing a faster and more complete precipitation, generally
with less zinc consumption. For some silver solutions, lead salt should
to be added before clarification, because in most solutions
part of the lead is immediately precipitated as an insoluble basic salt, which
quickly obstructs the precipitation filters.

This solution after the precipitation should normally contain < 0.01ppm of
Some of the gold precipitations occur immediately after the addition of
zinc. A large part of the zinc, however, is captured together with the precipitated gold
in the filter press and the solution containing gold that passes through this thin
Zinc film, it precipitates the remaining soluble gold in the filter. According to what was stated.
by King..."approximately 50% of the gold in the solution is precipitated among the
zinc feeder and the press, and it sways in its swift step in the filter queue
"press." For this reason, a short period of detention of the zinc feeder, does not
it should have adverse effects.

For the purposes of a proper addition of zinc, it is necessary that there is a sufficient
amount of cyanide in the solution for:

Dissolve the added zinc,

To preserve in solution the compounds that are formed when the
zinc dissolves in alkaline cyanide solutions, and
To ensure that all the heavy metals present in the solution are
keep it in this.

With dissolved heavy metal solutions (copper, nickel, zinc), the increase of
cyanide may be necessary to ensure a good precipitation. It is suggested a
minimum requirement of cyanide and alkalinity of 0.11% NaCN and 0.010% CaO.
pH terms, this means a solution normally above 11.0 for a good
precipitation. Initially, a pH of about 9.9 was used without problems, but with
In practice, a better definition of this minimum can be found. Most of the
problems in zinc precipitation in plants may be due to four causes:

Too much oxygen in the solution (insufficient vacuum in the vacuum tower,
air leak at some point in the suction line, or cone of
precipitation sucking air
Zinc deficiency (the amount of gold in the solution has increased, or the
solution is more polluted.
Insufficient free cyanide or lime in the solution. It may be that there is
a lot of free cyanide in the solution, but this will result in
only an excessive use of zinc. At a neutral pH, the precipitation will be
scarce, and
Surprising advance of solids that interfere with precipitation.

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Key precipitation chemical reactions with Zn

Oxidation reactions Zn/Zn+2and reduction Me+/Me°

For the gold-cyanide complex Zn + 2Au(CN) -‰Zn(CN) +-2 2Au

2- 4-2
For the Cyanide-Platinum complex Zn + 2Ag(CN)2%Zn(CN) + 2Au
- 4-2
For the Mercuric Cyanide complex Zn + Hg(CN)2‰Zn(CN)4+ Hg

Reason Zn/(Au+Ag)

P.a. At 196.97
P.a. Ag 107.87
P.a. Zn 65.39

Stoichiometric ratio 0.21

Average reason in the field 1.00 ÏExceso (%) = 366

TECHNICAL DATA OF ZINC

Grade UP # 510 MERCHANT

Total zinc(%min) 99.00 99.00

Metallic zinc (% min) 96.00 ND

Iron(max) <0.002 <0.015

% max <0.002 <0.05

Copper(% max) <0.002 ND

Cadmium(%max) <0.001 <0.02

Insolubles(% max) <0.005 ND

Zinc Oxide Balance ND

Lime (CaO) 0 ND

Average particle size 4.00 to 5.00 4.00

100 mesh sieve (% min) 100.0 100.0

200 mesh pass (% min) 100.0 99.9

325 mesh (% min) 100.0 98.0

Less than 15 Micrones (% min) 99.5 ND

Less than 10 Micrones (% min) 97.0 ND

Specific gravity 7.00 7.10

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CHAPTER 4.0

PROCESS CONTROL

The Merrill Crowe process within its advantage includes the ease of operation and control.
both the process and the production. For many years and even in small plants,
The control practiced has been manual based on simple plant controls and support from
chemical analysis laboratory. In recent years, there has been a growing interest in
instrumentation and automation for process control. Undoubtedly given that
the cost of instrumentation is highly independent of the size of the process
control. Computers, coupled with 'on-line' samplers and analyzers, have
have been introduced for process control. Among the most commonly used instruments
they are counted:

Flow meters
Turbidimeters
pH meters
Analyzers by AA
Manometers (pressure, vacuum)
Selective electrode for cyanide ion.
Oximeters

4.1 Operational Parameters

Solution flow

The flow of the rich solution coming from the leaching pad and entering the plant
processing must be kept (constant) throughout the recovery process due to
Merrill-Crowe, so much so that the barren solution flow leaving the plant must be
similar to the flow of the rich solution that enters this plant.

DESIGN NOMINAL
Reason for the power supply flow 1287 m3/h(1eryear
rich solution
Solution flow rate 1200 m3/h
in the teams

Sampling of solutions.

Samples of solutions are taken to determine the concentration of the elements.

what is desired to be known. The rich solution is analyzed to determine the concentration of
Au and Ag mainly taking this measurement in the chemical laboratory; also
The concentration of free cyanide, the pH present in the solution, both are analyzed.
final parameters are determined in the metallurgical laboratory or in an environment
established within the plant.

The same parameters are analyzed in the barren solution in addition to the concentration.
from Zn, Hg, Cu, Pb, and As. The sampling of the solutions is done at the entrance of the
main line of the rich solution, from the filter presses, at the outlet of each filter press and
in the collection of all the outgoing solutions from the filter press (solution
barren). In addition to the barren solution and the enriched solution before its entry
to the leaching pile.

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Oxygen

Dissolved oxygen levels in the solution are measured in ppm, at the inlet and outlet.
from the aerator tower. The oxygen level entering that tower must be
reduced upon leaving this tower, in negligible amounts of oxygen.

Suspended solids

Suspended solids are measured at the entrance of the processing plant (rich solution)
that arrives from the leaching pad) and to the entrance of the clarified rich solution tank.

SOLUTION FILTER OF SOLUTION

RICA HOJA (salida) FILTRADA
Solids <5 ppm 3 ppm
contents in

Addition of Zinc Powder.

Zinc is added in powder form, into a small discharge hopper and from there to a
zinc feeder which discharges into the emulsifying cone.

Addition of anti-crusting agent.

The antifouling is presented in the form of an aqueous solution, which is added to

solution tank barren through a dosing pump. Likewise to the tank
of enrichment.

Diatomaceous earth

It is used as a pre-filter in clarifying filters and press filters in the form of

slurry, prepared in the body feed tanks and in the filling.

ADDITION OF REAGENTS
Zinc for a ratio Lead(II) nitrate3(Kg/hr) Flocculant (ppm)
1 4

Pressures

The working and hydraulic pressures in the clarifying filters and in the filters are measured.
pressure. The measurement is done in PSI.

PRESSURES
Clarifying Filters Filter Press
Drainage pipe (55 - 60 psi) Working pressure (90 psi max)
Working pressure (80 – 100 psi) Hydraulic pressure (4000 - 4500 psi)

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Cyanide

Once the sodium cyanide has dissolved in barren solution, measures are required.
security. Adequate containment systems and the minimum of connection pipes
they will reduce the risk of spills.

If the pH is not kept sufficiently high, dangerous amounts of HCN can be

generate and exit concentrated cyanide solutions. In the solutions exceeding
A minimum pH of 12 is necessary to keep the HCN at a low level, a measurement.
pH reliable is an important part of safe process control. When adding a
The caustic element added to the cyanide solution will raise the pH and minimize the formation of.
HCN.

4.2. Plant calculations

Example 1: Determine the Zn ratio, available cyanide, % recovery of gold and silver
according to the following operating data:

Flow: 1204 m3/h Weight of Zn: 162.2 g/min.

Sun Law. Rich Law Sun. Barren CN- free pH

To Ag To Ag Barren Barren
Rich Rich
ppm ppm ppm ppm make up make up

2.48 4.38 0.01 0.02 248.7 302.4 9.92 9.98

LeyRica− Mistress
%R= x 100
LeyRica
Weight of Zn x 60
Ratio of Zn
»Flow.x.(LawofGold+ LeydeAg)
ÿ
[Link]
CN disponible
1 + 10 (9.34− [Link])

Therefore:

2.48− 0.01
% R Au = x 100 = 99.60 %
2.48

4.38− 0.02
% R Ag = x 100 = 99.54 %
4.38

[Link]/ min.x.([Link]/hr )
Zn ratio = = 1.18
1204m 3.x.(2.48+
/hr
4.38)ppm

free CNRica= 248.7 ΩCN Disp = 239.4 ppm

CN freeMake Up302.4 ΩCN Disp

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4.3. Operating procedure in the presence of high solids

One of the conditions for a good recovery of Au from the rich solution,
So, it is the absence of suspended solids; but this is not the only reason.
through which the entry of solids into the circuit should be avoided. The details are as follows
some others:

First of all, once the solids pass through the Clarifying Filters,
the final destination of these are the Filter Presses (which eventually become
in a more efficient Clarifier), resulting in saturation
prematurely of these, increasing the pressure and presenting leaks to
through the plates. This means generating a sub-standard operation
of the Filters.

Secondly, the Filter Presses require a

greater amount of fluxing agents due to the excessive amount of
solids in the precipitate. Additionally, the operators report that the spills
these crops are more problematic, and the bars come out smaller
quality is affected by recovery.

Thirdly; the Clarifying Filters show a saturation

immediate and demands constant changes. Taking into account that the
Replacing one clarifier filter takes at least 20 minutes, this becomes
in a very slow response to the problem; being the consequence
immediate overflow of the unclarified tank, even if it is turned off
a bomb, reduce the flow and the filter change time is reduced to
minimum (approx. 10 min). Observe, in this case, that for the balance of
Production is taking a flow that monitors the flow arriving at the plant.
but does not reach the Press Filters. The presence of solids must be
controlled if we have a filter on standby in time.

4.4. Solution Analysis

Determination of free cyanide:

We titrate 10 ml of the sample with AgNO.3, using rodanine as an indicator.
The reaction that will be formed is the following:

Silver nitrate32 NaCN ---------- Na(CN)2Ag + NaNO3

Titrator of AgNO3

Concentration of AgNO3 Detection range (ppm)

2.17 g/l 250 - 2500

0.217 g/l 25 - 250
0.0217 g/l 2.5 - 25

If less than 5 ml of the titrant solution is used to identify the endpoint, then
re-do the volumetric analysis of the sample using the following concentration
lower title of [Link] more than 50 ml of titrant is required to identify
the final point, use the following highest concentration of titrant AgNO3.

NaCN(ppm) = VAgNO3spending (ml) x AgNO concentration3(g/lt) * 577

V sample (ml)

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CN- (ppm) = NaCN (ppm)

1.884

Example 2: Prepare 3.45 liters of a NaCN solution with a concentration of 500

ppm of CN-

Molecular weight of NaCN = 49

Molecular Weight of CN- = 26

500 ppm CN- (49/26) = 942.3 ppm of NaCN

0.942 g/lt x 3.45 lt = 3.25 g of NaCN

Example 3: Determine the ppm of anti-fouling agent that is being used in a

cyanide solution with a flow of 1200 m3when the addition of the anti-fouling is
40 ml/min.

Anti-fouling (ppm) = 40 ml/min x (60 min/h) = 2 ppm

1200 m3/h

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BALANCEDEUNFILTERPRESS

SOLUTIONRICH SOLUTIONBARRACK DRYPRECIPITATE TORTOFRISBEE

99854m3 99854m3 1272Kg 1077Kg
Content Content Content Content
ppm oz Kg ppm oz Kg Ozone conceo
n
a
rin
t Kg Concentration oz Kg
At 26.38450 26301. 32 1 590Toz/C8397 261715T
6oz/C84595. 264
Ag 64.920840 64802. 64 214850oz/TC20818 6481751T
5oz/C20794 647
Zn 84.52 8409059. 9495 09.4% 12 10.5% 11
Hg 2.53 25302. 32168.5% 21462%
. 23
Cu 40.72 406401. 4095 06.1% 8 07.1% 8
Iron 0.65 65603. 63 % 0 % 0

wetPESOPttd WH20+WHg+W(othermetals)
ZnConsumption 2086Kg
1083Kg
PESOPttdoSeco WHg+W (other metals)
1272Kg 39%H2O

PESOPttdoRetorteado PESOHg
1077Kg 195Kg

Pesosatomics Precipitation reactions

In 197
Ag 108 Zn + 2Au(CN)2- Zn(CN)4-2 + 2Au
Hg 201 Zn + 2Ag(CN)2- Zn(CN)4-2 + 2Ag
Zn 65 Zinc + Mercury cyanide4-2 Zn(CN)4-2 + Hg

Theoretical relation Zn/(Au+Ag) 0.21

Theoretical relationship Zn/(Au+Ag+Hg) 0.24

According to Reactions
ParaKgde Senecesitande ZincConsumption(Kg) 1083 100.0%
To 263 44KgZn Consumed by the RxQx 322 29.8%
Ag 648 196KgZn Deposited in Precipitate 12 1.1%
Hg 253 82KgZn ZnquevadirectoaS. Barren 749 69.1%
1164 322

Real relation Zn/(Au+Ag) 1.19

Real relationship Zn/(Au+Ag+Hg) 0.93

Necessary for precipitating Valuable Met. (AuyAg) 240KgZn

T.h.e.e.n
xc.e
1
s(0
si83
2-40) 843KgZn 351.n
zicexces

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