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Improving Acid Wash Efficiency of Loaded Activated Carbon in a Gold

Desorption Circuit

Conference Paper · August 2018

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 Improving Acid Wash Efficiency of Loaded Activated Carbon in
a Gold Desorption Circuit

P. Forson1,2, A-S. Adam1,2 and G. Ofori-Sarpong1

1
Department of Minerals Engineering, University of Mines and Technology, P. O. Box 237, Tarkwa, Ghana.
2
Golden Star Resources Bogoso/Prestea Limited, Bogoso, Ghana

Forson, P., Adam, A-S. and Ofori-Sarpong, G., (2018), “Improving acid wash efficiency of loaded activated
carbon in a gold desorption circuit”, 5th UMaT Biennial International Mining and Mineral Conference, Tarkwa,
Ghana, pp. MR75-81.

Abstract
Acid wash is employed as a unit process in the Carbon-in-Leach (CIL)/Carbon-in-Pulp (CIP) process route chiefly for the
removal of calcium carbonate, magnesium and sodium salt from pregnant carbon surface. Conventionally, a 3% (w/v) HCl,
an hour soak and 1 bed volume of acid can typically give over 95% removal of calcium from carbon surface for calcium
loadings less than 2%, though lower acid wash efficiencies (<< 95%) have also been reported. In this study, parameters such
as acid concentration, contact time, bed volume and water source were varied to ascertain the best combination of these for
an improved efficiency. Causative factors as well as mitigation measures for the bad performance of the process were
investigated through method and sequence audit. A 5% (w/v) HCl with a 2 hour soak and 1 Bed volume of acid gave about
85% efficiency, and was considered the best condition, whereas a 3% (w/v) HCl with a 2 hour soak and 1 bed volume gave
77.90% efficiency. It was envisaged that the application of the best condition as a shock-treatment method for a relatively
short period of time and then reverting to a 3% HCl acid soak for 2 hours will remove substantial quantities of adsorbed
calcium from the carbon surface. This would translate into higher acid wash efficiencies at reduced cost, while minimising
damage to the reaction vessel.

Keywords: Acid Wash, Loaded Carbon, Bed Volume, Conditioning, Desorption

1 Introduction Gold processing companies over the years have

Leaching is the selective dissolution of a mineral of
interest from its ore/concentrate/calcine using a
suitable reagent so as to produce a concentrated
pregnant solution from which the metal of interest
can be recovered (Marsden and House, 2006;
Ofori-Sarpong, 2013).
Sodium cyanide has been the preferred reagent for
the dissolution of gold for more than 100 years
after its first successful use on the Witwatersrand
gold mine in 1890 (Davidson and sole, 2007). To
prevent the hydrolysis and volatilisation of cyanide
(a function of cyanide concentration and pH) as
seen in Equation 1, cyanide leaching systems
operate at pH that minimises cyanide loss, typically
at pH >10.5 (Marsden and House, 2006) and so this
calls for conditioning of slurry prior to cyanidation.
 
CN  H 2 O  HCN  OH (1)
resorted to using lime or slaked lime for raising
pulp pH because it is more economical, has the
ability to neutralise any acidic constituents present
in ore, aids in the decomposition of bicarbonates in
mill water as well as improves the settling rate in
thickeners (Marsden and House, 2006; Ramli and
Osman, 2015). However, calcium carbonate formed
from lime addition and some base metals found in
ores (inorganic foulants) have a detrimental effect
of fouling activated carbon used in the adsorption
of aurocyanide complex from the leach solution
(Stange, 1999; Rogans, 2012). This is because the
adsorption ability of activated carbon in such
systems is not selective to aurocyanide complex
alone but to both organic and inorganic foulants
resident in the slurry (McDougal et al, 1980).
The deposition of inorganic foulants on loaded
carbon surface is undesirable at the desorption step
in a gold process route because it causes a
reduction in the desorption kinetics leading to
higher residual gold on the barren carbon on most

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processing sites. Inorganic foulants may also
desorb and effect the eluate composition adversely
(Marsden and House, 2006).
Work done by researchers have proposed the use of
dilute mineral acids (HCl and HNO3) in dissolving
inorganic foulants prior to desorption (Beckmann
and Semple, 2002). The general equation for the
dissolution of a divalent metal carbonate in mineral
acid is given in Equation 2:
 2
MCO3  2 H M  CO 2  H 2 O (2)
The use of HCl in an acid wash cycle of loaded
carbon over the years has yielded good results and
has been adopted by most gold processing mining
companies as an integral process step of the
desorption circuit.
A typical acid wash cycle utilises 3% weight by
volume concentration of HCl syphoned into the
acid wash hopper or column to dissolve calcium
carbonate, fine ore minerals, magnesium and
sodium salt and fine iron particles from loaded
carbon surfaces. At the end of the acid soak period,
loaded carbon is rinsed with water at a total cycle
time of about 4.5 hours. Acid wash (AW)
efficiencies (Equation 3) between 80-95% is
achieved after the end of the cycle (Marsden and
House, 2006; Michaud, 2016). A higher efficiency
achieved maintains carbon’s ability to recover
additional gold, maximises surface exposure,
enhances carbon activity and minimises the
production of fines (Basi et al, 2016; Michaud,
2016; Beckmann and Semple, 2002).
Calcium( LC ),%  Calcium( AW ),%
AW Efficiency  * 100 %calcium analysis. The spent acid’s pH was checked
Calcium( LC ),%
(3)
Where LC and AW are loaded and Acid-washed
carbon respectively.
2 Materials and Methods Used
2.1 Materials and Equipment
Loaded carbon samples were obtained from the
desorption circuit of a gold mining company in
Ghana. Loaded carbon from four different elution
batches prior to acid wash was used for this study.
Batch numbers were noted for comparison with
routinely determined acid wash efficiency. Each
carbon batch was divided into two; one half was
washed thoroughly with raw water while the other
half was stored as-received. All experiments were
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carried out on the wet weight. Reagent grade
hydrochloric acid (37% w/v) was obtained from the
Mine’s metallurgical laboratory and acid strengths
of 3%, 5%, 7%. 10%, 12% and 15% (w/v) were
prepared.
5000 ppm potassium solution was prepared from
potassium nitrate salt and kept in a 2.5 litre flask
which was used as a matrix for calcium ions and
subsequent atomic adsorption spectrometer (AAS)
reading. This was done to prevent the ionisation of
calcium from solution due to the high temperatures
achieved using nitrous oxide and acetylene flame
for the AAS analysis. 0.1 M NaOH solution was
also prepared from caustic salt and used as titrant to
determine residual hydrochloric acid
concentrations.
2.2 Methods
2.2.1 Loaded Carbon Acid Soak at Different HCl
Concentration
Samples weighing 150 g each of the washed loaded
carbon from the five different carbon batches were
weighed into 250 ml beakers. The carbons in the
beakers were flooded with the different
concentrations of dilute acid prepared as one bed
volume and covered. After an hour soak, spent acid
was drained from the carbon into new beakers with
corresponding sample labels. The carbons were
washed thoroughly using raw water, after which it
was dried. Samples weighing 1 g each was picked
from each batch for calcium analysis. Samples of
raw water used for rinsing were picked together
with a head sample from each of the batch for
and a 5 ml sample picked and titrated against 0.1 M
NaOH to determine the residual acid strength.
2.2.2 Varying Contact Time for Pregnant Carbon
Acid Soak
The acid concentration which gave optimum acid-
wash efficiency was picked alongside 3% acid
concentration employed by the mine for further
optimisation. All washed samples at this point were
composited and 150 g lots weighed from the
composite for further test work. Using 3% acid
strength and the concentration which gave the
optimum AW efficiency, samples were contacted
for 1, 1.5, 2 and 2.5 hours. Solutions at the end of
the soak time, that is, spent acid was drained, its pH
read using a pH meter and the residual acid
concentration determined by titrating 5 ml of the
solution against 0.1 M NaOH solution.
Acid-soaked carbon were washed thoroughly using 3 Results and Discussion
raw water, dried together with a carbon head
sample and submitted for calcium analysis. Sample 3.1 Effect of Different Acid Concentrations
of the raw water used for rinsing was also on Acid Wash Efficiency
submitted to analytical laboratory to determine its
calcium concentration. The result of acid wash efficiency after contacting
pregnant carbon samples with 3, 5, 7, 10, 12 and
15% HCl concentrations for the four batches are
presented in Figure 1 It can be seen that, the
2.2.3 1 and 2 Bed Volume (BVs) of Acid for efficiency increased as the acid concentration
Pregnant Carbon Acid Soak increased. This is in line with the collision theory
proposed for reactions between calcium carbonate
The acid concentration and soak time which gave
and hydrochloric acid which says that as the
the optimum efficiency along with the 3% dilute
concentration of HCl in water increases, the
hydrochloric acid concentration were picked for
particles of HCl also increases with a greater
further optimisation. Using the optimum acid
tendency to collide with CaCO3 particles
concentration and soak time at this point, samples
precipitated on the carbon surface and pores in the
were soaked using 1 and 2 bed volumes; solution
form of scales (Beckmann and Semple, 2002). This
used in the soak, half way the optimum contact
will mean at higher HCl concentration, the acid
time were drained and replaced with the same acid
molecules will react with calcium carbonate more
concentration as a representation for a 2 bed
often than at a lower concentration (Walker, 2007).
volume soak. The same conditions were repeated
Above 5% HCl concentration, however, there was
using 3% acid strength. The concentration of
no substantial increase in efficiency.
residual acid for each spent solution was
determined by titration and the pH read using a pH Although 15% HCl gave the highest acid wash
meter. Samples were washed at the end of the soak efficiency, it was not selected as the concentration
time using raw water, dried together with a head for an improved recovery because the higher
sample and submitted for calcium analysis. concentration of acid will cause the stainless steel
columns used for the process to corrode faster and
2.2.4 Use of Process Water for Rinsing Pregnant
increase the concentration of residual chloride ions
Carbon after Acid Soak
on the pregnant carbon prior to elution. Higher than
The parameters which gave the best efficiency at desired residual chloride ions are known to increase
this point were used for the next run of experiment anode corrosion in electrowinning cells (Hu et al,
with a change in the water source to process water 2011; Chandler, 1998; Chambers, 2014).
to ascertain the effect of water quality (calcium-
laden water) on the acid wash efficiency. At the
end of the contact time, the spent solution was
drained, the concentration of acid after soak and pH
were checked and the acid-washed carbon rinsed
with process water. Samples of the process water
were picked for calcium analysis. The experiment
was done to determine the impact of use of process
water with high calcium content on the efficiency
of acid wash.

2.2.5 Test work on unwashed (As-Received)

sample

The experiment was aimed at determining the

effect of rinsing prior to acid soaking on the
efficiency of acid wash. Three batches of unwashed Figure 1 Acid wash efficiency for different
samples were picked and contacted with 3% dilute dilute HCl concentrations
acid for one hour. The concentration of acid and pH
were checked before and after the testwork.
Samples were washed at the end of the soaking
time using raw water, dried, and 1 g picked and
ashed, digested with aqua regia and diluted with
potassium solution. The resulting solution was then
sent for AAS analysis.

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3.2 Effect of Contact (Soak) Time on Acid
Wash Efficiency
Figure 2 shows 3% and 5% HCl acid wash and
their efficiencies. For 3% acid wash, the efficiency
increased as the contact time increased. The longer
the reaction period, the more likely the reaction
products will be formed so far as the reactants are
not totally consumed. However, the reaction rate of
HCl and CaCO3 are directly proportional to the
concentration of HCl, and hence, the reaction rate
decreases as HCl concentration decreases (Anon.,
2017). Residual HCl was reported in each case Figure 3 Acid wash efficiency and residual
suggesting that the acid was not totally consumed. acid concentration for 1 and 2 bed volume
The 5% acid wash showed a similar trend with no
soak
substantial increase in efficiency after the second
hour, which suggests the end of the reaction. Two
hours was picked as the optimum contact time for
an improved efficiency. 3.4 Effect of Water Quality on Efficiency
To determine the effect of water quality on
efficiency, process water was used for a 2 hour
soak and 1 bed volume for 3% and 5% acid wash,
and the results were compared with those of raw
water. The concentration of calcium in the process
water used was 454.83 ppm with a pH of 8.69.
There was a drastic drop in efficiency from 77.90%
to 50.68% when process water instead of raw water
was used for 3% acid concentration. For 5% there
was a drop in efficiency from 85.03% to 68.67% as
shown in Figure 4. The drop in efficiency could be
as a result of deposition of calcium from the
process water onto the activated carbon surface
Figure 2 Acid wash efficiency for 3% and which has regained, to some extent, its activity
5% HCl concentrations at different from chemical regeneration. It can be envisaged
contact times that as the rinsing time increases, the efficiency is
likely to drop further as more calcium would be
deposited on the carbon surface.

3.3 Effect of Bed Volume of Acid Used on

Efficiency
For 1 and 2 bed volumes of 3% and 5% acid wash
for a 2 hour contact time, acid wash efficiency
improved slightly from 75.95 to 79.57 and 85.03 to
87.78 respectively as shown in Figure 3. However,
the higher concentration of residual acid after the
second bed volume of acid was added in both cases
indicated that, there was little consumption of the
acid for the second bed volume of acid. This was
more pronounced in the 5% acid wash, which was
indicative of wastage of acid, should 2 bed volumes
be adopted. One bed volume of solution in each Figure 4 Acid wash efficiency for raw and
instance was thus selected to be the optimum.
process water rinse

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3.5 Effect of Rinsing Prior to Acid Wash on
Efficiency
To ascertain the effect of rinsing loaded carbon
with water prior to acid wash, conditions for acid
wash on the plant was replicated for the unwashed
samples; 3% HCl concentration, one hour soak and
one bed volume of HCl solution. The efficiency
reported was 33.39% with 0.53% of HCl left and a
pH of 2.6. The acid consumption and pH were
higher than all the other conditions used. This
could be as a result of titration of the acid with the
basic nature of entrained slurry on the carbon
surface from inefficient washing prior to the acid
wash.
Figure 5 Acid wash efficiency, acid
consumption and solution pH for
washed and unwashed samples
3.6 Effect of Flame Type on Quality of Assays
and Efficiency
Figure 6 shows comparison of efficiencies for
calcium analysis using air/acetylene flame and
nitrous oxide/acetylene flame type respectively.
The former was used as the flame type for routine
calcium concentration determination on the AAS.
For 3% HCl concentration, efficiency reported
from the experiment carried out was compared with
that of plant routine test work to determine
inconsistencies. From Figure 6, it can be seen that
plant-reported efficiencies were generally lower
than that from the experiment. Ca, Sr, Ba, Rb, Li,
Na, K, Cs and other metals which have 6.1 eV or
lower ionisation potential ionise at the air-acetylene
flame temperature and because atomic adsorption
measures quantity of free atoms, a decrease in
absorbance, that is a negative interference is
expected (Shimadzu, 2007). This was not the case
when nitrous oxide-acetylene flame type was used
with potassium solution as a matrix.
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Figure 6 Comparative analysis between
routinely determined acid wash
efficiencies and the experiment
From the above, it is clear that the use of
air/acetylene on the AAS for calcium analysis gives
erroneous and unreliable results. The use of nitrous
oxide/acetylene flame is therefore the most
optimum and recommended flame for Ca 2+
analysis.
4 Conclusions and Recommendations
The contribution of all parameters considered
towards improving acid wash efficiency were
determined. The best conditions for an improved
acid wash efficiency was realised as: 5% HCl
concentration, 2 hour soak time and 1 bed volume
of acid. However, it is expected, in the worst case
scenario, that residual chlorine ions and its impact
on downstream processing equipment coupled with
the extra cost of additional volumes of acid
required to raise the concentration of acid will
hinder the adaptation and continual usage of a 5%
HCl concentration. Improper washing of pregnant
carbon and the quality of water used for the acid
wash sequence were key players for lower acid
wash efficiencies reported. The use of
oxygen/acetylene flame was also a limiting factor
to the accuracy and consistency of acid wash
efficiencies reported.
It is thus recommended that,
 The parameters for an improved efficiency
in relation to the aforementioned
conditions can be used as a shock
treatment method over a relatively short
period of time with the aim of
substantially reducing the overall calcium
loading on the carbon. It is envisaged that
the use of a 3% HCl concentration for acid
wash thereafter will improve the acid
wash efficiency.
  Thorough washing of pregnant carbon
prior to acid soak should be ensured for an
efficient utilisation of acid used in the
sequence.
 The use of raw water only should be
encouraged during acid wash.
 Acetylene/nitrous oxide flame type with
potassium solution as a matrix should be
used for analysis of calcium loading on
pregnant carbon at all times.
Acknowledgement
The authors are grateful to the Golden Star
Metallurgical Department for granting them access
to their laboratories for the testworks to be carried
out.
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Authors
Philip Forson is currently a Graduate
Metallurgist at Golden Star Resources at
its Bogoso/Prestea operation. He holds a
Bachelor of Science Degree in Minerals
Engineering from the University of Mines
and Technology (UMaT), Tarkwa, Ghana.
His research interests include extractive
metallurgy, carbon fouling and mitigations,
physical chemistry and separation processes and
biohydrometallurgical processes. He is a member of the South
African Institute of Mining and Metallurgy (SAIMM), Society
for Petroleum Engineers (SPE) and Ghana Institute of Engineers
(GhIE).
Ahmed-Salim Adam is the Process
Manager for Golden Star’s Bogoso/Prestea
Mine. He received his BSc (Hons) Degree
in Mineral Engineering from the Western
University College of the KNUST and
MPhil Degree from the University of
Mines and Technology, Tarkwa. He holds
the Process/Metallurgical Managers
Certificate of Competency from the Inspectorate Division of the
Minerals Commission of Ghana with over 9 years of experience
in both Refractory and non-Refractory gold process operations,
Technical services, Project Management and waste water
detoxification. He is a Professional Member of the Australasian
Institute of Mining and Metallurgy (AusIMM).
 Grace Ofori-Sarpong is an Associate
Professor of Minerals Engineering at the
University of Mines and Technology,
Tarkwa. She holds a PhD in Energy and
Mineral Engineering from the
Pennsylvania State University, an MSc in
Environmental Resources Management
and BSc in Metallurgical Engineering,
both from the Kwame Nkrumah University of Science and
Technology, KNUST, Kumasi, Ghana. Her areas of research
interest include microbial-mineral interaction, water quality
monitoring, acid mine drainage issues, microwaves in extractive
metallurgy, bio-modification of recalcitrant organic matter and
small-scale gold mining. She is a member of the Society for
Mining, Metallurgy and Exploration Engineers (SME), Society
of Petroleum Engineers (SPE), Graduate Women in Science
(GWIS) and the West African Institute of Mining, Metallurgy
and Petroleum (WAIMM).

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