22/10/2019 Cyanide Bottle Roll Leach Test - Leaching Procedures

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Cyanide Bottle Roll Leach Test – Leaching Procedures

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List Equipment Required to Perform of a Standard Bottle Leach Test

Winchester bottles, with tops

Plastic tape to seal tops of bottles
Flexible air lines for possible aeration
requirements
Magnetic or mechanical stirrer for agitation
Timer, pH meter, thermometer and weighing
device
Leachants, i.e. acid, alkaline or neutral
solutions, or speci c solutions
Filter: vacuum or pressure
Titration systems

Procedures

Dry the ore and crush it to minus 2380 pm (or as speci ed, otherwise).
Prepare the solution of required concentration (e.g. 1M H2SO4 requires 52 ml of con.
H2SO4/litre of water).
Place 50 gm sample in the leach bottle and add 250 cc of prepared solution.

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22/10/2019 Cyanide Bottle Roll Leach Test - Leaching Procedures

Allow leaching to take place for 1 hour under stirred conditions, ensuring the right conditions
of pH, temperature, % solids, etc.
After leaching, discharge contents of leach
vessel into clean pressure or vacuum lter
without washing the vessel.
Filter pulp, and collect pregnant leach liquor
undiluted.
Wash ad dry the residue and record it weight.
Analyse residues and pregnant liquors for
relevant metal content.

Precautions

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When handling concentrated acid, always wear eye protection, and always add acid to water.
If water is added to concentrated sulphuric acid, the heat generated could vaporize the water
and cause an explosion; by adding the acid to water, the heat is generated more slowly and
is rapidly dissipated by the water.
Residues should be thoroughly washed of leaching reagents.
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CYANIDE LEACH TEST PROCEDURE

Bottle Leach Procedure for Cyanidation.

Be sure to use at least 500g, but 1000g per test is better. Be sure to use a big enough bottle.
You need to lay it on its side to use it on the roller while having a small hole in the lid to allow
air inside. Alternatively you can use an air bubbler during the leach. We normally run a kinetic
test where we take the bottle off the roller and sample the solution at 2, 4, 6, 24 hours and
each 24 hours afterwards until the leach is complete. During that time, after you take your
sample, you can sparge the sample with air or oxygen to simulate the air added during the
process. Measure the dissolved oxygen if you can. There really is no substitution for measuring
the DO, the redox or ORP can be informative but it is not equivalent. Even if you have suf cient
cyanide the leach can stop if there is not suf cient oxygen.

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22/10/2019 Cyanide Bottle Roll Leach Test - Leaching Procedures

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I suggest you conduct kinetic leaches. They are a little bit more tricky because you need to
replace the liquid you remove and then account for the gold removed in the balance. I have
attached a balance you can use. You should use at least 3 points for your kinetic curve. The time
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represented by the second cyanide addition point in your circuit at CIL tank 4, then the end of
the circuit, plus another lot of time that is convenient to the technician. You don’t want to die
wondering if the leach would have got a higher recovery if you just had more time, so add more
time. The balance provided has 8 points.

At the kinetic sampling points measure the cyanide. Your metallurgist and operators know the
cyanide titration procedure. Add enough cyanide to bring the concentrate back to the desired
point. The current circuit starts at 600-650 ppm then adds cyanide part way to 300-350 ppm.

Ok, that is the preamble. Prepare your sample. Homogenization is your friend. If you don’t split
your lab test samples representatively then you will have a mysterious time with your test
program. Sample from the existing circuit, the otation tail, and ensure your lab procedure
reproduces the actual results. Do a few repetitions, check the effect of the water you are using.
Perhaps lter off the existing water and add the water you intend to use during the lab testing.
Make sure you do enough tests where you have a good idea of what the results are supposed to
be for your circuit. Consider this a calibration. If you are not con dent of how your lab tests
reproduce your actual circuit performance then take care when reviewing your conclusions.
Make sure your heads match with each test. You should be able to reproduce a 95% match, you
can loosen to 92% knowing that you have coarse gold and it may be dif cult to reproduce the
head. Use duplicate tests to build your con dence.

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22/10/2019 Cyanide Bottle Roll Leach Test - Leaching Procedures

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A test program starts with using your current conditions on the new ore. If the recovery is good
then you are done, congrats. If not then you change one variable and do another test. I would
suggest running a sample you know along with your new sample, and a another new sample
with a higher cyanide concentration. Running 1 test a time is a bit slow because these can take
a week to get results. More than 6 at a time is dif cult for 1 technican. Although a good tech
can handle 20, they have to be really prepared.

Be aware of the First Aid Treatment for cyanide poisoning. Do not mix cyanides with acids:
deadly cyanide gas will result.

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22/10/2019 Cyanide Bottle Roll Leach Test - Leaching Procedures

Tare an empty clean glass leach bottle on an electronic scale. Record the bottle weight on
the Cyanidation Test Form.
Place the dry ground or pulverized test sample into the tarred bottle using a powder funnel.
Record the mass of the sample on the Cyanidation Test Form.
Calculate the amount of water required to achieve the target pulp density using the formula
given below:

Example:

% Solids = Dry Solids Weight * 100/ (Dry Solids Weight + Weight of Water)

OR

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Weight of Water = (Dry Solids Weight * 100 – Dry Solids Weight) /% Solids

Re-zero the scale with the bottle containing the test sample on the platform. Add the
calculated amount of water into the bottle containing the test sample. Record the volume of
water added and the percent solids.
Weigh the bottle containing the test sample and water on the scale. Record the total weight
of the bottle containing the sample and water.
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Agitate the slurry in the bottle. Measure and record the natural slurry pH.
Add lime (CaO or Ca(OH)2) to the slurry to achieve protective alkalinity (pH > 10). Record the
amount of lime added and the slurry pH.
Add sodium cyanide (NaCN) to the desired concentration (g/L) of solution. Record the amount
of sodium cyanide added.
Place the bottle on the bottle roller machine and start the roll. Record the cyanidation start
date and time.
Monitor and maintain pH levels.
At the end of the predetermined time intervals (ie: after 4, 8, 24, 48 and 72 hours), remove
the bottle from the bottle roller machine and set it on a table in the Assay Laboratory.
An Assay Technician will pipette a sample of the cyanide leach solution from the settled
slurry and lter it. The ltrate sample is analyzed for residual lime and cyanide and assayed
for elements of interest by atomic absorption spectroscopy.
When the Assay Technician has completed sampling and analysis, add lime and cyanide to
the slurry, equivalent to amount consumed during the time interval. Measure slurry pH and
record. Record weight of the fresh lime and sodium cyanide added to the test.
Zero the scale and weigh bottle containing the slurry. Add water to the slurry (if required) to
reach the original (time zero) total weight of the bottle containing sample and water.
Place the bottle test on bottle roller machine and start the rolls. If more than one cyanide
leach test is in progress, add a sleeve onto the neck of each bottle, then lower each bottle to
allow air into the bottle when it touches the bottom of the top bottle on the rolls.
At the end of each timed interval, repeat steps 11 through 15.
At the end of the test, vacuum lter the nal cyanide leach slurry through a Buchner funnel
containing lter paper into a lter ask.
Wash the nal lter cake a minimum of three times with three 1000 ml volumes of hot water
to wash the soluble metals from the cyanidation tailing solids. Depending on the client’s
request, the nal ltrate wash solution is either retained or discarded.
Label and dry the cyanidation tails for sample preparation and assay.
Fill out an Assay Request/Report Form and submit it to the Sample Preparation department.

Laboratory leaching procedures

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22/10/2019 Cyanide Bottle Roll Leach Test - Leaching Procedures

Laboratory leaching procedures include studies of dissolving metal ions with an acid, a base or
cyanide. Although not so common today, gold amalgamation may also fall in this category. The
testing may involve eld tests on ore in place, broken ore in stopes, ore and waste in dumps or
crushed ore in vats and laboratory tests of ground ore, concentrates or calcines in agitators. The
technique may be used to effect the selective solubilization of a desirable component such as
copper, uranium or gold or the puri cation of a product to remove impurities such as MgO from
zinc concentrates, copper from molybdenum concentrates or iron from silica sands.

Very little laboratory testing can be done on ore in place so that the research team will have to
depend on descriptions of the deposit from the geologist, mineralogist and miner, tests on
coarse rock samples and knowledge of the characteristics of the ores of the region involved.
Leaching tests on rock samples of any size from 20 cms to 1 cm can.be simulated in columns of
adequate diameter and height.

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The metallurgist should choose a large enough diameter that there is no adverse “wall effect”.
Non-corrosive materials of construction such as asbestos or plastic pipe should be utilized for
the columns so that maintenance in the lab will not be high and undesirable constituents of the
pipe will not enter the leachant.

The bottom of .the column should be tted with a suitable lter media. A positive circulating,
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corrosion-proof pump and reservoir system should be employed – usually using plastic tubing
for solution transfer. The most important variables to monitor when leaching ores are time,
temperature, feed size, additive requirements, density and leachant concentration and
consumption vs. extraction of desirable and undesirable components.

Agitation leaching of ore, concentrates or calcines may be easier to test than static leaching but
liquid-solid separation of the residues may be a problem and should be included in the testing.
Consumptions of reagents may be higher than in static column tests so that the extra operating
costs would have to be justi ed by higher recoveries. One is not liable to discover that elevated
temperatures and/or pressures would be economic today with high energy costs in treating low
grade ores by leaching’ but this statement may not be • true with some high grade ores or
when treating, high value metals such as uranium or higher grade materials such as
concentrates or calcines.

Certain additives such as lime during precious metal cyanidation and oxidants during uranium
leaching will be important reagents to monitor.

“Old” Gold Leaching Method

Experiments with small quantities of material in the laboratory will usually determine the
maximum extraction that can be looked for. The weight of ore taken may be from 100 to 200
grammes. It is placed in a funnel or lamp glass, tted with a perforated cork and lter bed, and
washed with water, or, perhaps better still, shaken with distilled water in stoppered bottles and
ltered. The ltrate may contain soluble salts of iron, copper, and tests are applied for these and
also for acidity, and for soluble sulphates and chlorides. The water ltrate may also be mixed
with cyanide solution to determine how much cyanide, if any, is decomposed by it. In this way
the value of the water wash on the particular ore is determined.

Preliminary tests as to the amount of alkali which it is necessary to add, and the amount of
cyanide decomposed are made as follows:

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22/10/2019 Cyanide Bottle Roll Leach Test - Leaching Procedures

(a) Alkali.—200 grammes of washed ore are made into a paste with water in a porcelain
basin, and tested with litmus paper. If an acid reaction is observed, a titrated solution of
caustic soda is run in, little by little, until the mixture is neutral. It is convenient to make
the alkaline solution of such a strength that each c.c. corresponds to one pound of caustic
soda per ton of the ore which is being tested,

(b) Decomposition of Cyanide.—100 grammes of the ore are shaken in an 8-oz. stoppered
bottle with 50 to 100 c.c. of a solution of KCy for fteen minutes, then left undisturbed for
twelve hours, and nally shaken again for ve minutes. The available cyanide in the
separated solution is then estimated and compared with that in the original solution. By
merely shaking for a few minutes, most of the decomposition of cyanide is made to take
place, but not the whole.

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Cyanide solution of 0.1 or 0.2 per cent, is then passed slowly through the ore drop by drop, or
shaken and left in contact with it for some time, and then drawn off and the ltrate tested for
soluble sulphides, ferrocyanides, sulphocyanides, copper, zinc, and for its reducing power. The
tests recommended are:

1. Add hydrochloric acid. A white turbidity may indicate the presence of soluble sulphides or of
zinc.
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2. After adding the acid in slight excess, add a few drops of K4FeCy6. A brown coloured
precipitate indicates copper, a white occulent precipitate may indicate zinc.
3. Add lead tartrate dissolved in excess of NaOH; a brown or black colour indicates soluble
sulphides.
4. Acidulate with H2SO4 and add dilute K2Mn2O8 drop by drop. If it is decolorised, reducing
power of the solution is indicated, and aeration may be necessary.

The percentage of extraction by cyanide may then be tried by passing solutions through the ore,
washing thoroughly by ltration, and assaying the residues to nd what quantities of the
precious metals have been removed, checking the results by recovering the gold from the
ltrate.

The consumption of cyanide may be determined by titrating the solution before and after use.
In this way, the maximum extraction of gold and silver from an ore which has been crushed to
different degrees of neness, with solutions at different strengths, acting at various
temperatures and for different lengths of time, may be determined. The best proportions of
solution to ore may also be determined. Such data will be of great value in determining the
degree of suitability of the process to any given ore, but the results obtained cannot usually be
repeated on the large scale. Mechanical dif culties preclude ne crushing beyond a certain
point; the relative amount of solution used in practice must be less than the large quantities
giving the best results on a small scale. Moreover, the washing and ltering is more perfectly
performed in the laboratory than in the mill, but, on the other hand, the consumption of
cyanide may be less in the latter case than in the former.

We recommend tests on ore crushed to 10, 20, 30, 40, and 60-mesh size, with solutions of 0.01,
0.05, 0.1, 0.2, and 0.5 per cent, of KCy, amounting to 1, 1¼, 1½, 2, 3, and 4 A.T. of solution per
A.T. of ore in successive washes, remaining in contact with the ore for 1, 2, 3, 4, 7, and 14 days.

By David Michaud | June 24th, 2015 | Categories: Concentrator Manuals/Procedures, Cyanide Leaching, Laboratory Procedures,
Reagents and Chemicals | Tags: Cyanide Leaching | Comments Off
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