Abstract

The experiment examines the effect of cyanide on leaching of gold ore sample. The
gold leaching is based on Elsner’s equation which is will help in binding the gold ion and make
them soluble in water, thereby allowing them to separate from the rock. The test determines
the volume of gold that has been leached by the cyanide solution. To know the amount of gold
that has been leached, the gold-cyanide solution will be titrate with silver nitrate which is
known as cyanide analysis or Liebig method. After titrating standardize silver nitrate and
cyanide solution (after gold absorption) there will a development of turbidity due to the
formation of silver cyanide. The results of the experiment will be time dependant as the sample
is collected between interval of 30 minutes within 2 hours. The sample is then titrated with
standardize silver nitrate.
4Au + 8NaCN + O2 + 2H2O = 4NaAu (CN)2 + 4NaOH (Elsner’s equation)
Reaction: 𝑁𝑎𝐶𝑁 = 𝑁𝑎+ + 𝐶𝑁 −

Introduction
The purpose of this experiment was to observe the volume of gold that is leached by
the cyanide. These were determined indirectly using standardize silver nitrate. This experiment
also shows the optimum time of cyanide adsorption, as the sample will be collected at different
time with the same speed of stirrer.

Material and experimental procedure

Apparatus:
1 Beaker 100ml, 500ml and 1000ml

2 Volumetric flask 1000ml

3 Measuring cylinder 1000ml

4 Bulb pipette 5ml and 10 ml

5 Plastic bottles for keeping analytical 50/100ml

solution
6 Glass dropper and pipette

7 Filter papers

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Reagents and solutions:
 Sodium cyanide
 Silver nitrate
 Sodium chloride
 Sodium hydroxide (2M)
 Standard solution silver nitrate
 Indicator solution, Rhodanine
 Potassium chromate indicator

Experimental procedure
This experimental procedure has been divided to two procedure which is cyanide
leaching procedure and cyanide analysis procedure. For cyanide leaching procedure, the gold
sample were weight to 200g using pan weight and were put inside a large plastic beaker or
reaction flask. Then 1 litre of stock solution ~ 300ppm CN were prepared by weighing a
quantity of sodium cyanide equivalent to 300ppm CN. By using a measuring cylinder, 950ml
of the stock solution of ~300ppm CN is poured into the reaction flask where the leaching is
carried out. The remaining 50ml CN solution was keep in a dark brown bottle. Poured in 200g
weight of the roasted sample (gold sample) and mixed it thoroughly, if necessary rinsed the
sample beaker with CN solution. Next, CN leaching apparatus was set up inside the fume
cupboard and were fixed in the laboratory stirrer. When the stirrer was turn on (stirrer speed is
450rpm) the timer also started. The leaching is carried for 2 hours. Sample is collected at an
interval of time of 30 min. Aliquot sample with volume (2x10 ml) were taken out during CN
leaching at time interval of 30 min, 60min, 90min, and 120 min. The aliquot taken must be
filtered using the vacuum pump into a 100ml beaker and kept in a dark brown sample bottle
before CN analysis.
The cyanide analysis (refer to appendix A for cyanide analysis) on the 50ml remaining
CN stock solution is carried out while the leaching was running to determine the initial
concentration of cyanide concentration. 5ml of aliquot volume of the CN stock solution were
taken and transferred into an Erlenmeyer flask and were titrated with the standard solution of
silver nitrate solution (refer to appendix B for standardization silver nitrate solution). Triplicate
analysis was done, and the volume of silver nitrate solutions is recorded. The initial CN
concentration in ppm in the CN stock solution was obtained from the average volume of silver
nitrate solutions. Similar CN analysis was carried out on the aliquot sample solutions taken at
various time intervals.

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Appendix B
Before cyanide analysis is carried out, standardization of silver nitrate need to be done first.
Instead of appendix A, appendix B will be carry out first. To know the exact molar
concentration of the solution. Standardization of the silver nitrate solution was done with a
primary standard solution of 0.005M NaCl using potassium chromate as an indicator- The
Mohr method.
a) Preparation of standard stock solution of ~0.01925 M 𝐴𝑔𝑁𝑂3 solution.

Some finely powdered A.R. silver nitrate was dried at 120ºC for 2 hours
and allowed to cool in a covered vessel in a desiccator. A 3.27 g of the dried
AgNO3: salt was accurately weighed in a dried 100 ml beaker, about 50.0 ml
of deionized water was taken to dissolve the salt using a piece of glass rod and
then the solution was transferred quantitatively into a 1 litre volumetric flask
and was made up to volume to the mark with deionized water. The molar
concentration calculated from the weight of silver nitrate employed. This would
give about 0.01925 M solution of AgNO3.

b) Preparation of the primary stock standard solution of 0.1 M NaCl

A 0.1M bf NaCl solution was prepared by accurately weighing out

0.5844g of the pure dried A.R. salt. The salt was dissolved in deionized water
in a 100 ml volumetric flask and making up to volume to the mark. The
calculated molarity of NaCl solution would be 0.1M.

c) Standardization of ~ 0.001925 M AgNO3 with 0.005M of NaCl

A 0.005 M of NaCl solution was freshly prepared by transferring 5ml

aliquot from the primary stock standard solution of 0.1 M NaCl into a 100 ml
volumetric flask and the sample was diluted to the mark with deionized water.
The stock standard solution of AgNO3 (~ 0.01925 M) was also diluted by taking
an aliquot of 50.0 ml solution and diluted to the mark in a 500 ml volumetric
flask. This would give AgNO3 solution having a molarity of ~ 0.001925 M.
This solution was then transferred into a clean and dry burette for
standardization.

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Titration procedure.
Using a bulb pipette, 10.0 ml aliquot of 0.005 M NaCl was transferred into an
Erlenmeyer flask (resting upon a white tile) and after the addition of 3 drops potassium
chromate indicator, it was immediately titrated with the AgNO3 solution from the burette. The
silver nitrate solution was added slowly from a burette and the liquid was swirled constantly
until the red colour formed by the addition of each drop begins to disappear more slowly.
This gave an indication that most of the chloride has been precipitated. Continuous drop
wise addition of the titrant was done until a faint but distinct change in colour has occurred.
This faint reddish-brown colour should persist after brisk shaking. If the end point exceeds
(production of a deep reddish-brown colour), more of the chloride solution should be added
and titrated again.
All the titrations were repeated with two similar volumes of solution of 0.005M NaCl.
The various titrations should agree within 0.1 ml

Indicator Blank Correction

The indicator blank correction was determined by adding 1.0 ml of the indicator to a
volume of water equal to the final volume in the titration and then adding the silver nitrate
solution until the colour of the blank matches that of the solution titrated.

Appendix A
Titration procedure:
A sample of cyanide solution was taken using the appropriate sampling technique. The sample
size required depends on the approximate cyanide concentration in solution. About 5.0 to 10.0
ml aliquot of the sample solution was taken and transferred into a 50 ml Erlenmeyer flask.
About 2 drops of the rhodanine indicator was added slowly while swirling the flask steadily.
Once the sample cyanide solution is ready for titration, the silver nitrate solution is carefully
added from the burette into the cyanide solution flask with gently shaking of the flask until the
solution starts to turn to a pale-yellow colour. The flask should be agitated to ensure that the
end point has been reached but care must be taken not to add excess silver nitrate because the
end point of the titration is not always easy to detect. The final change from yellow to salmon
pink colour would give an indication of the detection of end point. The end point is sometimes
best seen against a black background. If the end point occurs on the first drop of the AgNO3
solution being added, there is no free cyanide in solution, usually due to the acidity of the
solution. The titration was carried out in duplicates and the results were recorded. The titration
values should agree within 0.1 ml.

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Results
CN analysis:
Time (min) Volume of 𝐴𝑔𝑁𝑂3
(ml)
I II Average
0 14.2 14.1 14.15
30 14.2 14.1 14.15
60 14.0 13.9 13.95
90 13.8 13.7 13.75
120 13.3 13.7 13.50
⅀=69.50

Standardization of silver nitrate:

Sample Volume of 𝐴𝑔𝑁𝑂3
(ml)
initial Final average

1 0 32.7 32.70

2 0 31.0 31.0

⅀=31.85

Indicator blank correction:

Blank sample Volume of 𝐴𝑔𝑁𝑂3
(ml)
initial final Average

1 0 2.5 2.50

2 2.5 5.1 2.60

⅀=2.55

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I. Percent pulp density of the feed sample used in the CN leaching process.

𝑠𝑜𝑙𝑖𝑑
% 𝑝𝑢𝑙𝑝 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 = × 100%
(𝑠𝑜𝑙𝑖𝑑 + 𝑙𝑖𝑞𝑢𝑖𝑑)
200
= (200+950) × 100%
= 17.39%

II. To calculate the exact molarity of AgNO3 after standardization

From the chemical reaction:
1 mole Ag+ ≡ 1 mole Cl-
Molarity of AgNO3 = 0.005𝑀 𝑋 10.0𝑚𝑙(𝐴−𝐵) 𝑚𝑙
where,
A = average volume of AgNO3 (ml) used in the titration
B = average volume of AgNO3 (ml) used in the blank determination

Molarity of AgNO3 = 0.005𝑀 𝑋 10.0𝑚𝑙 (31.85-2.55) 𝑚𝑙

= 0.001706 M

III. The strength of titrant

From the chemical reaction:
1 mole Ag+ ≡ 2 mole CN-
If the no. of moles of AgNO3 is 0.001835, then:
No. of moles of CN- = 2 x 0.001706
= 0.003421 moles
This would give an
Equivalent factor = 0.003421 x 26.01
= 0.08898 mg CN- per titre of AgNO3
1.0 ml of AgNO3 is equivalent to 0.08898 mg CN-

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IV. Cyanide content in the original samples:
The strength of titrant 1.0 ml of AgNO3 would contain 0.08898 mg CN-
If from a 1000 ml sample solution, 5.0 ml aliquot was taken and the volume of AgNO3
used in the titration was 14.15 ml.
1ml 𝐴𝑔𝑁𝑂3 = 0.08898 mg CN-
14.15 ml 𝐴𝑔𝑁𝑂3 = 14.15 × 0.08898
= 1.259067 mg CN-
1.259067 𝑚𝑔 𝐶𝑁 − = 5 𝑚𝑙 𝐶𝑁 −
1000
× 1.259067 = 1000 𝑚𝑙 𝐶𝑁 −
5

=251.81 ppm CN-

Thus, the concentration of free cyanide in 1L solution is 251.81 ppm/ 251.81g/ton
V. Cyanide content in 30 min sample.

If from a 950 ml sample solution, 5.0 ml aliquot was taken and the volume of AgNO3
used in the titration was 14.15 ml.

1ml 𝐴𝑔𝑁𝑂3 = 0.08898 mg CN-

14.15 ml 𝐴𝑔𝑁𝑂3 = 14.15 × 0.08898
= 1.259067 mg CN-

1.259067 𝑚𝑔 𝐶𝑁 − = 5 𝑚𝑙 𝐶𝑁 −
950
× 1.259067 = 950 𝑚𝑙 𝐶𝑁 −
5
=239.22 ppm CN-

Thus, the concentration of free cyanide in 950 ml solution is 239.22 ppm/239.22g/ton

VI. Cyanide content in 60 min sample.

If from a 930 ml sample solution, 5.0 ml aliquot was taken and the volume of AgNO3
used in the titration was 13.95 ml.

1ml 𝐴𝑔𝑁𝑂3 = 0.08898 mg CN-

13.95 ml 𝐴𝑔𝑁𝑂3 = 13.95 × 0.08898
= 1.241271 mg CN-

1.241271 𝑚𝑔 𝐶𝑁 − = 5 𝑚𝑙 𝐶𝑁 −
930
× 1.241271 = 930 𝑚𝑙 𝐶𝑁 −
5
=230.88 ppm CN-

Thus, the concentration of free cyanide in 930 ml solution is 230.88 ppm/230.88g/ton

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VII. Cyanide content in 90 min sample.

If from a 910 ml sample solution, 5.0 ml aliquot was taken and the volume of AgNO3
used in the titration was 13.75 ml.

1ml 𝐴𝑔𝑁𝑂3 = 0.08898 mg CN-

13.75 ml 𝐴𝑔𝑁𝑂3 = 13.75 × 0.08898
= 1.223475 mg CN-

1.223475 𝑚𝑔 𝐶𝑁 − = 5 𝑚𝑙 𝐶𝑁 −
910
× 1.223475 = 910 𝑚𝑙 𝐶𝑁 −
5
=222.67 ppm CN-

Thus, the concentration of free cyanide in 910 ml solution is 222.67 ppm/ 22.67g/ton

VIII. Cyanide content in 120 min sample.

If from an 890 ml sample solution, 5.0 ml aliquot was taken and the volume of AgNO3
used in the titration was 13.50 ml.

1ml 𝐴𝑔𝑁𝑂3 = 0.08898 mg CN-

13.50 ml 𝐴𝑔𝑁𝑂3 = 13.50 × 0.08898
= 1.20123 mg CN-

1.20123 𝑚𝑔 𝐶𝑁 − = 5 𝑚𝑙 𝐶𝑁 −
890
× 1.20123 = 890 𝑚𝑙 𝐶𝑁 −
5
=213.82 ppm CN-

Thus, the concentration of free cyanide in 890 ml solution is 213.82 ppm / 213.82 g/ton

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The effect of time on concentration of cyanide during
leaching
255
251.81
250
CN Concentration (ppm)

245
239.22
240
235 230.88
230
225 222.67

220
213.82
215
210
0 20 40 60 80 100 120 140
Time (min)

Figure 1

Discussion

From the graph obtained, it shows the concentration of cyanide is gradually decreasing
as time is increasing. This shows that the amount of cyanide binds with gold ion has increasing
along with the time. Meanwhile the concentration of free cyanide left in slurry is decreasing.
Time plays an important role to obtain optimum amount of gold leachant. Besides time, size of
the sample is also important as we need to achieve maximal recovery. Pulp density affects
viscosity considerably, which has an impact on gold leaching. It has been found that pulp
densities which are too high, as well as those which are too low can affect gold leaching
performance in a negative manner. Overly dense pulps hinder mass transfer whilst dilute pulps
result in a loss of ore leaching residence time as well as high reagent addition rates.

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Post-lab questions

1. Write the Elsner’s equation for cyanide leaching of gold

4Au + 8NaCN + O2 + 2H2O = 4NaAu (CN)2 + 4NaOH (Elsner’s equation)

2. The roasting of an ore concentrate in the laboratory is usually carried out by placing the
concentrate sample in a “fireclay” crucible and heat it in a muffle furnace to a
temperature between 550 – 700° C. Homogeneous mixing of the charge is carried out
at several time intervals until the process of roasting is complete in usually 5-7 hours.
If the gold in the ore exist in the form of sub-microscopic in the pyrite, why should the
ore undergo the process of roasting before cyanidation?

To obtain the valuable gold from the sample even though it is sub-microscopic in the
pyrite. It also helps in get rid of other minerals from react with cyanide such as arsenic
and others.

3. The correlation of the curve with the gold extraction methods with reference to the size
range and percent gold.

From the graph, we can see that different size of sample has different percent of gold.
Then we can conclude in gold extraction size distribution is important. But the size of
the gold should not be too fine or large. If it is too fine, we can see from the graph that
the percent of gold is decreasing. Same goes to the large size particle, the gold contain
in large particle size is also lower. Thus, it is important to know the optimum size for
the extraction of gold so the recovery will be high.

Conclusion
From this experiment we know that time is important for cyanide to binds with gold ion
and make it soluble. Optimum time is needed for cyanide to leach the gold. Pulp density also
important in gold leaching as it effect the grade of concentration and recovery of the gold. To
avoid the gold loss low pulp density is needed. Therefore, we need to know the optimum size
of gold sample and optimum time for leaching so that we can achieve maximum recovery of
gold.

References

S.Venkatachalam. (n.d.). Hydrometallurgy.

Stange, W. (n.d.). The process design of gold leaching and.

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