DETERMINATION OF THE LIME REQUIREMENT,

FREE CYANIDE AND PROTECTIVE ALKALINITY

IN GOLD PLACER ORE
Rosselle kim P. Castillano, Wilfredo T. Gatdula Jr., Gin derick L. Magno, Jhunalyn Parantar
METE 157N: HYDROMETALLURGY LABORATORY
ABSTRACT
The nature of many gold deposits (low grade-high tonnage) and the increasing sophistication of deposit
assessment procedures and exploration geochemistry demand better quality analytical data, particularly for the
lower range of gold values near and below cut-off grade. Modern geological models attribute formation of many
of these gold deposits to hydrothermal solutions that have added elements other gold or leached some elements
from the host rock, so that there is usually a multi-element from the host rock, so that there is usually a multielement metasomatic effect in and around a deposit. Analyzing gold by itself rarely will provide useful details
regarding geochemical halos, environmental baseline levels for potential problem elements and data on potential
metallurgical complication.in this activity, the pH, free cyanide and protective alkalinity are determined using
gold placer sample. Oxalic acid used as titrant during determining the lime requirements of the sample and also
for determining the protective alkalinity while for determining the free cyanide silver nitrate was used.
INTRODUCTION

SIGNIFICANCE OF THE STUDY

A cyanide bottle roll test is the industry standard

first step in assessing the gold recovery possible by
cyanide leaching. The first step in a heap leach
testing program is preliminary bottle roll tests at a
relatively coarse feed size to determine the ore's
leachability. Bottle roll tests provide initial
information about precious metal recovery,
recovery rate, and reagent requirements [1].

Using cyanide in gold leaching, the experiment

determines the various variables such as protective
alkalinity, lime requirement and free cyanide
content as a basis for industrial application in gold
leaching processes.

Cyanide leaching has been the industry standard for

gold processing for more than 100 years. During
the cyanide leach process, a cyanide solution, or
lixiviant, is percolated through ore contained in
vats, columns or heaps. Gold is dissolved by the
cyanide and then removed from the heap or
columns. It is then extracted from the pregnant
leach solution by adsorption on carbon or resins.
This cost-effective, proven method of ore
extraction provides maximum recovery for many
gold ores, including low grade and some refractory
ores [2].

A. For Preliminary Test (Lime Requirement)

OBJECTIVES OF THE STUDY

MATERIALS AND METHODS

The materials used were 1000 mL beaker, burette,

bottles and pipette.
4 trials containing 300 grams of sample each with
500 mL distilled water and 2.5 grams of cyanide
were prepared. Different weights of lime were
added on each trial measuring 4 grams, 4.5 grams,
5 grams and 5.5 grams each respectively. Bottle
roll was then done on the solutions prepared for 1
hour. Using oxalic acid solution, titration of the
trials was then conducted using phenolphthalein as
an indicator.

To be able to determine the lime requirement of the

ore by using Clennels method, titration using
silver nitrate to determine the free cyanide content
and the protective alkalinity of the cyanide leaching
solution.

Determination of the lime requirement, free cyanide and protective alkalinity in gold placer ore.
Submitted to Alma Mae Batucan, Instructor. Page 1 of 4

Sample preparation
Weighing of samples

Mixing of the sample

30 minutes agitation

obtained 25 mL aliquot
Titration of aliquot with
AgNO3
Agitate again the leached
solution with lime

Figure 1. Process flowsheet for Lime Requirement

Titration of 25 mL aliquot
with AgNO3 using KI

B. For Free Cyanide and Protective Alkalinity

Titration 25 mL aliquot
using standard oxalic acid
w/ phenolphthalein

Materials used are gold placer as the sample, 600

mL beaker, 100 mL graduated cylinder, AgNO3
solution, cyanide, CaO, KI, KCN, phenolphthalein
indicator, mechanical agitator, filter funnel, 250 mL
erlenmeyer flask, stirring rod and digital balance.
Weigh of 246.27 g (based from calculations) was
obtained it was then placed in a 600 mL beaker
with 500 mL distilled water. Cyanide of 2.5 g was
then added to the solution and was stirred until the
cyanide dissolves. It was then agitated for about 30
minutes. An aliquot of 25 mL was taken and
filtered for the titration with silver nitrate solution.
Then, 2.5 g of lime was added in the leached
solution and was agitated again for about an hour.
It was then titrated using silver nitrate and record
the readings. Then the sample was added by
phenolphthalein indicator and then it was titrated
by standard oxalic acid solution until pink color
disappeared.

Record data

Figure 2. Process flowsheet for Free Cyanide and

Protective Alkalinity
RESULTS AND DISCUSSION
A. Lime Requirement
Table 1. Data obtained for the lime requirement
Bottle
No.

CaO (g)

pH
(before
titration)

Oxalic
Acid (mL)

4.0

7.2

7.8

4.5

7.4

9.1

5.0

7.2

9.4

5.5

7.7

10.1

It was observe in table 1 that bottle 1 containing 4.0

g of Cao was titrated with 7.8 mL of Oxalic acid
and also for bottle 2,3 and 4 with 9.1, 9.4 and 10.1
respectively which are increasing.
Eqn. 1. Determination of the mass of the solution.
Mwater= DwaterVwater
= (1g/mL)(200mL)
= 200g H2O
Mtotal= Mwater + More
= 200 g + 50g

Determination of the lime requirement, free cyanide and protective alkalinity in gold placer ore.
Submitted to Alma Mae Batucan, Instructor. Page 2 of 4

= 250g
Equation 1 was used to determine the mass of the
water and the mass total.
Table 2. Calculated amount of remaining CaO per
bottle
CaO in kg/MT of the
Amount of CaO
solution
remained (% CaO)
4
4.5

0.078
0.091

5.0
5.5

0.094
0.101

Table 4. Data for free cyanide determination of ore

leached for 1 hour with lime.
No. of Amount
Drops
Vol
%
Trial of aliquot
of KI
AgNO3
NaCN
(mL)
used
(mL)

25

9.81

0.98%

Eqn 4. Determination of the %NaCN

Eqn.2 Determination of %CaO

100
Percent NaCN obtained for 30 minutes leaching
was 1.05 while for 1 hour was 0.98 and it was
calculated using equation 4.It was observed that the
longer the time it was leached the lower the %
NaCN.

%CaO

Table 2 consist of CaO in kg/MT of the solutions

data and amount of CaO per bottle in which
calculated using equation 2.
0.12
0.1
0.08
0.06
0.04
0.02
0
4

4.5

5.5

Table 5. Data protective alkalinity of ore leached

for 1 hour with lime.
No. of Amount
Drops of
Vol
pH
Trial of aliquot Phenolph
standard
(mL)
thalein
oxalic
used (mL)
1
25
5
1.8
11.81
2
25
5
1.2
11.63
The pH was calculated using the formula below.In
table 5 pH obtained are 11.81 and 11.63 for both
trial 1 and trial 2 with an average of 11.72.
Eqn 5. Determination of the [OH-] concentration

CaO (kg/MT)

Figure 1. line graph of CaO (kg/MT) vs. %CaO

In table 2 it was observed that with increasing
amount of CaO there was also increasing %CaO.

Eqn 6. Determination of Protective Alkalinity using

[OH-] concentration
[
]

B. Free Cyanide and Protective Alkalinity

Table 3. Data for free cyanide determination of ore
leached for 30 mins.
No.
Amount
Drops
Vol
%
of
of
of KI
AgNO3
NaCN
Trial
aliquot
used
(mL)
(mL)

25

10.6

1.05%

CONCLUSION AND RECOMMENDATION

The pH, alcalinity and the free cyanide was all
determined during the activity. It was all important
parameters in determining the 'leachability' not only
for gold but also for silver by leaching with
cyanide. Acid should be avoided, since if any acid
is used prior to the cyanide, and is still present on
the ore (as evidenced by a pH lower than 7 in
water) it will produce HCN, a very toxic gas. It is
good to take a sample of the ground ore and place it
in water and agitate it overnight to see if the pH

Determination of the lime requirement, free cyanide and protective alkalinity in gold placer ore.
Submitted to Alma Mae Batucan, Instructor. Page 3 of 4

changes. If it gets acidic, lime should be added to

neutralize the acid producing potential of the rock.
It is suggested that the activity must be done
properly with complete equipment during the
activity for better result. Also it must be done
carefully since we are using toxic chemicals such
as cyanide.

REFERENCES
http://www.sgs.com/en/mining/metallurgy-andprocess-design/cyanidation-technologies/cyanideleaching/cyanide-bottle-roll-test
http://www.sgs.com/en/mining/metallurgy-andprocess-design/cyanidation-technologies/cyanideleaching
http://www.infomine.com/library/publications/docs
/McClelland1988.pdf

Determination of the lime requirement, free cyanide and protective alkalinity in gold placer ore.
Submitted to Alma Mae Batucan, Instructor. Page 4 of 4