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Read the present manual carefully and follow the instructions herein ;
The present manual is an integral part of the machine, in case of loss or deterioration,
ask the manufacturer for another copy;
Do not remove or tamper with protective carters, protective covers or safety devices;
the present manual supplies all the necessary safety indications and instructions
according to the Safety Norms en force. This does not represent a substitution to the
common sense and experience of the operator.
6
The employer must analyse the various functions and characteristics of the machine,
the adopted safety precautions, any eventual personal protection devices, and any
remaining risks. Subsequent to this analysis, he must evaluate which personnel
should be authorised to operate the machine.
7
2.3 Rating plates
A
WARNING, ELECTRICAL POWER RISKS -ACCESS THE
ELECTRICAL EQUIPMENT ONLY AFTER HAVINGTURNED OFF THE
POWER SUPPLY AND WAITED FOR A MINIMUM OF 120 SECONDS
WARNING, RISKS DUE TO EXTREME TEMPERATURES
'A
WARNING, RISKS DUE TO FLAMMABLE GASES
PERSONS WITH PACEMAKERS OR OTHER ELECTRONIC DEVICES
ARE NOT ALLOWED TO APPROACH THE UNIT
()
FORBIDDEN TO USE WATER TO PUT OUT EVENTUAL FIRES
NON-AUTHORISED PERSONNEL ARE FORBIDDEN ACCESS TO THE
(%
\ \
U
i
OBLIGATIONTO WEAR HEAT PROTECTIVE GLOVES
8
3 LAYOUT
CD
LEGEND
A Frame B PPL hood
C 50 Lt reactor D 50 Lt (or 20 Lt) reactor
E n.2 Electric heaters for the reactors F PPL tray for the two acid storage tanks
G N2 100 Lt storage tanks for HCL and
HN03
H 10 Lt. graduated Pyrex container for HCL
1 10 Lt. graduated Pyrex container for
HN03
L Filter unit- also used to transfer solutions
using a compressed air pump
9
4 DESCRIPTION
The IA050-50 unit is used to refine gold alloys with minimumgold content of 250/1000 and a
maximumsilver content of 120/1000.
The cycle time of the aqua regia refining process is about 6 hours for 10 kg of gold. Using
two 50 It reactors, it is possible to carry out various steps of the process in parallel as well as
in a double cycle. This increases the refining capacity to about 40 kg of gold in 9-10 hours.
The first step of the refining process is to dissolve the alloy in the aqua regia solution: for the
maximum quantity of 10 kg, this will take about 3 hours. Subsequently, the solution is
transferred by vacuum from reactor n.1 to the filter. Further alloy can then be loaded into
reactor n.1 and the refining process can proceed in parallel.
A purity between 999/1000 and 999.5/1000 can be obtained.
Characteristics:
Pyrex glass is used as it is the only material that doesn't absorb precious metals. It
also facilitates the cleaning operations of the reactors and condensers.
For safety reasons, all parts in Pyrex (reactors and condensers) are positioned inside
a ppl hood fitted with a suction manifold that can be connected to a fume scrubber,
our model TLF/750. The hood has been designed to recover any acid or water
leakage.
The electric heaters for the reactors are fitted with power regulators to control the
dissolution process.
The units are supplied with two containers for HCL and HN03
positioned in a PPL
tray as requested by European laws. The acids are transferred from the storage
containers to 2 graduated Pyrex containers inside the hood by a vacuum system.
Fromthere, they are transferred to the reactors by gravity.
Filter unit on wheels with a compressed air diaphragm pump to transfer the solutions;
Cementation tank
Every unit is supplied with two storage containers on wheels for the king waters as
well as a control panel.
10
4.1 Set up
Refiningunit IAO50-50 + TLF750
The gold refining unit consists of :
Frame (A)
n.1 PPL hood (B) suction fan to be connected to a fume scrubber, type TLF/750 (M),
Designedto the recover any acid losses.
n.2 50 litre reactors (C + D) with relative 1m2 condensers (useful capacity: 45 It) flange O
185 mm.
n.2 Electric heaters (E) with power regulator (1500 W- 380 V) for the reactors
n.1 PPL tray (F) where the acid storage tanks are placed.
n.2 100 litre polyethylene acid storage containers (G) with cover and suction manifolds
n. 1Filter unit (L) used to transfer/wash/filter solutions using a compressed air pump. Also
used to wash the gold slime.
n.1 PPL 350 Lt cementation tank (N) - complete with stirrer, antiacid frame and service
stairs.
n.2 200 It polyethylene tanks, fitted onto a trolley to store king waters
All the personnel must be carefully trained by experts authorised by the user of the
plant. Courses to update them must be foreseen.
The personnel must have access to this manual and any other necessary information
at all times.
The personnel must be trained and must be sure, when entering the room, that it has
been sufficiently aired and does not contain toxic or asphyxiating gases. They should
also know how to work in confined spaces.
The personnel must wear the following protective devices : antiacid gloves, antiacid glasses.
14
6 INSTALLATION
The installation must be carried out by qualified personnel. The manufacturer declines all
responsibility for damage to things or persons derived by not observing this rule.
The environmental values (temperature, humidity etc) of the site must be in accordance with
the technical characteristics.
6.1 Working environment
The working environment must be well ventilated. The operators must wear the following
protective clothing and devices : antiacid gloves, antiacid apron, antiacid glasses, antiacid
boots.
6.2 Unpacking
Open the box and take out the components of the plant following the assembly sequence.
Refer to the room planimetry, to the enclosed drawing and to the legend.
Components have been marked with reference numbers corresponding to the ones used in
the enclosed drawings and in this manual. For electrical signs, refer to the electrical diagram.
The glassware (condensers, reactors etc.) are filled with salt to protect them during
transportation. When unpacking, it is necessary to put these parts into a tank filled with warm
water to dissolve the salt. Be very careful when handling all glassware as it is very fragile.
6.3 Connections
Followthe numbers on each items to connect the unit.
15
7 REFINING GOLDALLOYS USINGAQUA REGIA
7.1 Howto use the refining plant
The IA050-50 unit is used to refine gold alloys with minimumgold content of 250/1000 and a
maximumsilver content of 120/1000.
The aqua regia refining method is based on dissolving metallic gold in aqua regia. Aqua
regia is made up of nitric and hydrochloric acid. The proportions in volume are the following
(based on commercial concentrations) : 20% HN03 at 36 Be and 80% HCI at 21 Be.
For other concentrations, these percentages must be recalculated
WARNING
Its important for these acids to not contain hydrofluoric
acidwhich can quickly dissolve the glasswork
1-
2-
The first operation is to melt the alloy into fine grains,
(using our grain tank model RPG) in order to reduce
dissolution time.
Open the cooling water supply (1) (4-6 Lt/1') to the glass
condenser connected to reactor n.1. This must be done
gradually in order to avoid the water hammer effect. Turn
on the fume scrubber sprayer and subsequently the
fume scrubber suction fan. Rotate switches (3) and (2)
on the scrubber to do this.
16
3- Regulate the throttle valve (4) so that the suction force is strong enough to stop
fumes from exiting through the reactor inlet.
4- Put the grains into reactor n.1 using the appropriate PPLtube.
NOTE
It is recommended not to add powder alloys once the acids are inside the
reactors. If it is absolutely necessary to do so, the powder must be added a
little at a time as it causes a violent reaction as well as the production of
dangerous fumes.
5- The acids can now be vacuum transferred from the storage tanks (G) to the
graduated containers (H) and (F). From here the acids are loaded into the reactor by
gravity. This is done by manually opening the appropriate taps.
For each Kg of alloy to be dissolved, the quantity of HCI at 21 Be is 3.6 It and 0.9 It for
HN03 at 36 Be.
We recommend to load all the HCI acid first and subsequently the
HN03
acid in two
separate batches. To avoid loosing gold, the second batch of
HN03
should be loaded
once the initial chemical reaction settles.
Aqua regia =4 parts of HCI + 1 part of
HN03
Acid transfer sequence:
Filter suction
valve
17
Transferring
the acids from the
storage
tanks to the
graduated
containers:
a) Make sure the filter suction valve (7) is closed.
b) Open the main vacuum valve (8) on the fume scrubber.
c) Close the discharge valve (9) on the fume scrubber.
VACUUM
GUAGE
VALVE
d) Open the HCL suction valve (5)
e) Open the HN03 suction valve (6)
f) Wait until the graduated containers reachedthe desired level.
g) Once this level has been reached, open the discharge valve (9) to stop the flow of
the acids.
VACUUM
CONNECTION
(to be connected to
the vacuum inlet on
the IAO
unit)
18
Transferring
the acids from the
graduated
containers to the reactor:
h) Open the HCL inlet valve (10) and transfer the required amount of hydrochloric
acid into reactor n.1. The maximum quantity per operation is 10 It, which is the
maximum capacity of the graduated containers. Depending on the quantity of
alloy to be refined, it might be necessary to transfer acid from the storage tank to
the graduated container several times. It is advisable to transfer all of the HCL
acid first.
i) Open the
HN03
inlet valve (11) and transfer half the required amount of nitric acid
into reactor n.1. This acid must be added in two batches; wait until the reaction
settles before adding the second batch of acid.
6- A chemical reaction will occur after the first batch of
HN03
is added to the reactor
therefore make sure the reactor inlet is closed.
7- Wait until the reaction settles. Add the second half of the nitric acid at 36 Be. The
chemical reaction will resume and the temperature will increase to roughly 70C.
Wait for 1 hour and turn on the heater by rotating the two potentiometers (12) and
(13) setting them to "2-3" on the scale.
19
8- Wait for another 2 hours with the heater on, until the reaction finishes (the production
of yellow fumes will cease). It is not necessary to stir the grains during the dissolution
process.
9- Before turning the heater off, make sure there isn't a large quantity of undissolved
grains on the bottom on the reactor. Use the PPL stirrer to check this.
10- When the chemical reaction is finished, add a small
quantity of water to the solution in order to reduce the
cooling process time. Open valve (14) to do this.
11- Let the solution decant for a few minutes until it
becomes clear. During this length of time, the silver
chloride (AgCI) will separate from the gold slime and
deposit on the bottom of the reactor. This also stops
the silver chloride from clogging the filter paper in the
filter.
12- Fill the cooling tank (P) with water in roughly the same quantity as the refining
solution. Siphon off the entire solution from reactor n.1 into the cooling tank (P).
Position the cover on the tank and connect the flexible tube to the refining plant
suction connection. Open the suction connection valve.
20
Cooling tank (P)
13- The temperature of the solution will drop rapidly due to the presence of the water
inside the tank. This will also facilitate the decantation of the AgCI, improving the filter
process.
14- Remove the AgCI and the undissolved grains from the bottom of the reactor using
the PPI scoop. Place this material in a container for future use (cementation process).
15- Clean the sides and the bottom of reactor n.1 with hot water. Using cold water will
break the glassware due to the thermal shock. Transfer this rinsing water into the
cooling tank (P).
Pay attention before restart another refining cycle. Residual thermal capacity of
electrical heater could increase the temperature of empty reactor with the risk of a crack
during the refilling of the acids for thermal shock.
21
7.2 Filter process
A filter unit is supplied with this refining plant. It has two main uses :
a) to filter the solution inside reactor n.1 and to separate the silver chloride from the gold
in solution
b) to recover and rinse the precipitated gold and to transfer the king waters to the king
water storage tanks.
Connect the compressed air supply (5-6 bar) to the pressure regulator inlet (15) on
the filter unit.
Close valves (16) and (17) of the diaphragm pump positioned on the right side of the
filter (these will be necessary when the unit is usedto transfer various other solutions)
Connect the diaphragm pump inlet tube (18a) to the cementation tank (19) and the
vacuum tube (18b) to the filter vacuum inlet (7).
Cementation tank ICAU/D Filter unit
Open the filter unit cover. Position a 400 mm diameter filter paper onto the filter. Wet
the paper with water to make it adhere to the surface of the filter. Close the cover
and lock it into position.
Insert the flexible tube connected to the cover of the filter unit into the cooling tank (P)
and turn on the pump by opening the air valve (20).
The gold solution will be transferred from the cooling tank to the filter unit where it will
be filtered and subsequently transferred to the cementation tank (ICAU/D)
After the filter process is finished, open the cover of the filter unit and rinse with water
to eliminate any gold chloride residuals still present in silver chloride slime. This
rinsing water will also be transferred to the cementation tank (pump still on) - Put the
left-overs from the refining process (undissolved grains
-
see point 14 in the "How to
use the refining plant" section) into the filter unit and rinse as explained above to
eliminate any gold chloride from this material as well.
Close the air valve (20) and open the discharge valve (9) on the fume scrubber to
stop the vacuum.
Unlock and remove the top part of the filter unit and discharge the silver chloride
slime (and any traces of undissolved alloy) into a plastic container for future use.
23
7.3 Gold cementation process
The liquid in the cementation tank contains mainly gold chloride, copper chloride and other
precious metals (Pt, Pd Rd) present in the alloy.
S02
fumes develop during the cementation process. Make sure the cementation tank
is connected to the fume scrubber before proceeding.
Check for free nitric acid in this solution. Do this by preparing a solution of water and
urea (1 It of water + 200 gr of urea). Slowly pour this solution into the cementation
tank. No reaction means there is no nitric acid left in solution. If there is a reaction
(similar to "effervescence"), continue adding the water+urea solution until it stops.
As a second test, put 100 cc of the solution inside the cementation tank into one of
the glass beakers that come with the unit. Add about 10 gr of metabisulphite of soda
(Na2S2Os) to this. If gold doesn't precipitate, the cementation is over. Otherwise, add
more metabisulphite solution and continue with the process.
The solution inside the cementation tank will turn a dark green colour once the
reaction is finished.
Turn the stirrer off and leave the solution to rest for 15 minutes to complete the
precipitation process.
24
Plastic storage tank on wheels Cementation tank ICAU/D
Position the storage tank on wheels beneath valve (19) of the cementation tank.
Open valve (19) and discharge the king waters into the tank.
Position the filter unit beneath the large discharge valve of the cementation tank.
DISCHARGE
VAI \/F
Connect the pump outlet on the filter unit to the plastic storage tank. Turn the pump
on.
Open the valve (turn it anticlockwise) and discharge the gold slime into the filter.
Spray water into the cementation tank to wash it clean of any gold slime.
Remove the filter unit from beneath the cementation tank. Wash the gold slime
thoroughly with water at 50C. The pump on the filter unit will transfer this water to the
plastic storage tank.
The gold slime is ready for melting. No fluxes or solvents are necessary.
26
7.4 Howto treat the silver sludge
The silver sludge (AgCI) obtained during the initial filtration must be treated to obtain metallic
silver.
If traces of gold are still present in the sludge :
Physically separate these gold traces from the silver chloride using a sieve.
7.4.1 Howto transform silver sludge into silver metal
There are two methods :
7.4.1.1 Direct reduction method
Transfer the sludge to a plastic container and add sodium carbonate (Na2C03) in a
ratio of 1:1.
Mix well. Put this new sludge into melting furnace and proceed to melt. It is important
to heat the furnace slowly.
7.4.1.2 Chemical reduction method
Transfer the sludge into a glass container and add a small amount of zinc powder
which will reduce the silver into metallic form
Check that all the zinc has been dissolved by adding a few drops of hydrochloric acid,
then add hot water and filter by the usual method. The substance deposited on the
filter is metallic silver which, since it may contain traces of gold, should be treated
with nitric acid in a heated dish. In this additional treatment the silver passes into
solution inthe form of nitrate and it must be reduced again to metallic form by means
of zinc powder following the procedure described previously.
The gold obtained from the filtration must be returned to the reactor for the subsequent
refining cycle.
7.5 Treatment of waste waters after precipitation
The resulting waters after the precipitation process contain salts of all the metals except gold.
A special water treatment plant is needed to recover these metals (our model IN/A).
27
8 CYCLE TIMES
8.1 Single refining cycle using one reactor
A theoretical cycle time for 10 kg of grains using one 50 It reactor is roughly 6 working hours, not including the final melting stage.
- Foreseeen unit productivity = 80 - 90%
Single cycle for 10Kg. Au (one reactor) = 10Kg. time (rnin.) 1h. 2 h. 3 h. 4 Ik 5 h. 6 h. 7 h.
T me
1 Dissolution in aqua regia in Reactor 1 180'
2 Transfer the dissolved alloy from reactor 1to the coolingtank (P) 15'
3 Vacuumtransfer fromto filter unit/cementationtank 45'
4 Cementation 60'
5 Removal of gold slime fromthe precipitationtank 60'
Single cycle refiningtimefor 10 kgAu
_
36C(( h.
>
for 10 Eg. Au
28
8.2 Single refining cycle using two reactors
A theoretical cycle time for 10 kg + 10 kg of grains (total 20 kg) using two 50 It reactors is roughly 6 Vz working hours, not including the final
melting stage.
- Foreseeen unit productivity = 80
-
90%
Single cyclefor 10+10 Kg. Au (two reactors) = 20 Kg. fime (min.) 1h. 2 h. 3 h. 4h. 5 h. 6 h. 7 h.
J T me
_|
1 Dissolution in aqua regia inReactor 1 180'
2 Dissolution in aqua regia inReactor 2 180'
3 Transfer the dissolved alloy from reactor 1tothe coolingtank (P) 15'
4 Transfer the dissolved alloy from reactor 2 to the coolingtank (P) Iff
3 Vacuumtransfer fromto filter unit/cementationtank 45'
4 Cementation 60'
,
5 Removal of gold slime fromthe precipitationtank 60'
Single cycle refiningtimefor 10Kg. + 10 KgAu
29
8.3 Double refining cycle using two reactors
A theoretical double cycle time for (10 kg + 10 kg) plus (10 kg + 10 kg) of grains (total 40 kg) using two 50 It reactors is roughly 9 Vz working
hours, not including the final melting stage.
- Foreseeen unit productivity = 80 -
90%
Dissolutioninaqua regiainReactor 1 (1st cycle)
Transfer the dissolved alloy fromreactor 1to the coolingtank (P)
Dissolutioninaqua regia inReactor 1 (2ndcycle)
Transfer the dissolved alloy fromreactor t to the cooling tank (P)
Dissolution inaqua regia inReactor 2 (1st cycle)
Transfer the dissolved alloy fromreactor 2 to the cooling tank (P)
Dissolutioninaqua regia inReactor 2 (2ndcycle)
Transfer the dissolved alloy from reactor 2 to the cooling tank (P)
Vacuum transfer fromto filter unitfcementationtank (1st cycle)
Cementation(1st cycle)
Wash cementationtank
Vacuum transfer fromto filter unitfcementation tank ( ndcycle)
Cementation(2ndcycle)
Removal of goldslime fromthe precipitation tank (2ndcycle)
Double
cfcle
time for 10 >10 Kg. Au (two reactors) = 40 Kg.Au
30
9 MAINTENANCE
The frequency at which the operations listed below are carried out depends on the amount of
work the plant is required to do.
A. Periodically check the flexible hoses and replace them if there are any kinks.
B. Periodically check the waterworks connections and change any leaking parts.
9.1 Acid concentrations
To obtain 1 litre of acid starting with
HN03
at 42 Be, dilute with distilled water following the
table below :
Final conc.
hno3 h2o
22 Be
32 Be
36 Be
400 cc
690 cc
750 cc
600 cc
310 cc
250 cc
31
10 RESPONSABILITY
The manufacturer declines all responsibility in cases of :
o Incorrect use of the machine;
o Not foreseen or impropriate use of the machine;
o Modifications to the machine ;
o Removal or tampering with repair operations to the machines ;
o Use of the machine in impropriate environments ;
o Installation of the machines in an unsuitable environment ;
o Incorrect use of IPD's ;
o Use of machine by non-qualified personnel ;
32
11 SPARE PARTS
Consumables
Sodium metabisulphite
Na2S205
Recommendedspare parts
code description Qty
44000004242 50 It Pyrex condenser 1
33000007106 Lt. 10 Pyrex graduated container 1
44000004625 50 It Pyrex reactor 1
11230200003 PPI flexible tube for vacuum uses -to transfer acids 1
11230200004 PPI flexible tube for vacuum uses
-
for suction of acid fumes 1
33000001429 Pyrex condenser PTFEXPALL gasket (between reactor and
condenser)
1
33000006382 Aluminium valve D= 80 type CO ANTIACIDA for cementation tank 1
44000000803 1/2 " FF sphere valve 1
44000000804 PVC VEFV 1/2 " FF sphere valve 1
44000001797 1 " FF PPL sphere valve 1
44000002488 OR Code USA 2-124 Dint = 31,42 x 2,62 1
44000003886 OR Code USA 2-115 Dint = 17,13 x 2,62 1
44000003988 OR ORN00180 Dint = 78,74 x 5,34 VITON 1
44000004626 OR ORNA2371 Dint = 215,27 x 5,34 VITON 1
44000004063 OR ORNA2204 Dint = 9,11x 3,53 VITON 1
44000004064 OR ORNA2208 Dint = 15,47 x 3,53 VITON 1
44000004065 OR ORNA0129 Dint = 21,82 x 3,53 VITON 1
44000003864 PP sphere valve D=20 FF for acid inlet 1
44000004057 RTPR Vi' ATIL vacuum connection 1
44000004058 RTP 1" ATIL vacuum connection 1
44000003074 Manometer D=50 %" 0-10 ATM SMC for filter unit 1
44000003077 Filter EAW2000 ATT Vi" SMC for filter unit 1
44000004660 Diaphragm pump PP MINIBOXER-P for filter unit 1
44000005678 SP 820 PVC DN25 1" F-1" F-32F for TLF fume scrubber 1
44000005762 Vacuum regulation G Vi M04-02-10
Filter unit gasket 400 x 750
1
1
33
12 ENCLOSURES