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The purpose of this procedure is to provide a formal documented approach the two hourly sampling and
the procedures used for free acid and copper titrations of different streams and samples at Boss Mining
New SX plant.

1. SCOPE
This procedure applies to SX-EW operators in charge of titrations in the plant and to the metallurgical
lab technicians.

2. DEFINITIONS
-End Point: The point at which enough titrant has been added to match the concentration of
the species being measured.

-Titrant: A chemical, which is accurately measured into a sample to determine the amount of a species
being measured.

-Tenor: Concentration of a species in a sample.

-Free Acid: Acid (usually sulphuric acid H2SO4) which is free in solution.

3. SAFETY AND RISK

4.1. PERSONAL PROTECTIVE EQUIPMENTS (PPE)
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4.2. HAZARDS/CONTROLS

Hazards Controls
Slips trips fall. Use caution in all areas, when going up stairs
and walk ways.
Sampler cutter fall. Ensure the cutter is long and cannot fall in the
tank when taking a stream sample.
Electrolyte solution contact with skin or eyes -MSDS must be read.
-Wear hard hats, safety glasses, rubber gloves,
safety boots, and long sleeve shirts & trousers.
Breakage of glassware. Wear hard hats, safety glasses, rubber gloves,
safety boots, and long sleeve shirts & trousers.

4. TOOLS AND REAGENTS

Burettes of 100 ml

Beakers of 250 ml
Conical flask of 250 ml
Potassium Iodide (K.I)
Starch
Sodium thiosulphate .01N

NaOH Sodium Hydroxide 0.204N

Pipettes of 10 ml
Methyl orange
Sample Cutter or scoop
Empty bottles of 500 ml

8. SAMPLES DENOMINATION AND SAMPLING POINTS

New SX Plant
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Area Streams Sampling points

Sampling point valve on PLS feed to E1 primary
PLS Mixer.
Raffinate E2 point valve before the raffinate tank
Strong Electrolyte S1 point valve before the strong transfer tank
E1 Raffinate to E2 E1 advance raffinate feed valve to E2 Primary
New SX Primary Mixer Mixer
Plant E1 Organic to Loaded
Organic Tank E1 organic launder
S1 Organic to E2
primary Mixer S1 Organic launder
S1 Advance electrolyte S1 Advance electrolyte feed valve to S2 primary
to S2 primary Mixer Mixer

9. PROCEDURES
9.1 Sampling
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Ensure that all the sample bottles are

1 clearly named and have lids (available -Clean properly the cutter / bottles before and after
and in good condition ) sampling to avoid contamination or dilution.
Select the empty sample bottles tagged -Do not confuse the tag or ID sample
2 for specific area in the cleaned bucket
Start taking sample every one hour
3 before reporting time
4 At the sampling point, wash the sample
-For ease and consistency, all samples must be
bottle at least three times with the

9.2 Free acid titration

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sample solution required before taking taken from the same sample points each time.
sample.

5 Take at least 350 ml of the required -Collect minimum 350 ml of sample for rechecking if
sample and ensure that the sample required and also for composite sample collection.
bottle is completely closed.
-The organic solution is a mixture of the extractant
16 Handle
Get the carefully
3 hourlythe samples
samples for todifferent
the lab and the diluent which is flammable and skin irritant.
for analysis
streams -The electrolyte is a mixture of copper sulphate and
For slurry sample let it settle to get clear sulphate acid which is corrosive,skin and eye irritant
2 solution to titrate
3 Clean the 10ml pipettes, 250ml beakers
4 Ensure the reagents are available and in
good condition
Take 10ml of the required sample
solution to titrate and put it in the 250ml
beaker.
5 For electrolyte solution dilute the 10 ml
of sample solution with water in to
100ml beaker before taking 10 ml for
titration.
Add 2ml of K.I in the beaker and agitate
6

Dilute with water (distilled or tap water if

7 distilled water is not available) the
mixture to get 100ml in the beaker
8 Fill the thiosulphate in the 100ml burette
Add drop by drop the thiosulphate in the
beaker solution until the solution colour
9 become white. Ensure that the beaker
solution is shake continuously until we
get the colour
After getting the white colour, add 3 or 4
10 drops of methyl orange in the beaker
solution and the solution become red.
Fill the second burette with NaOH,
11 ensure that the burette is fill at the
proper indicated level
Start free acid titration drop by drop and -Adjust the reagents speed from the burette to get
shaking the beaker solution until you get a correct end point.
12 yellow colour (end point) of solution in
the beaker -At the end point do not confuse the colour change
from red to yellow for Acid titration.
13 Stop titration and read correctly the
NaOH volume consumed
Multiply the volume read by the factor -Read well the volume of sodium hydroxide from
14 given. the burette.
Free Acid (g/l) = VNaOH used × Factor
For electrolyte solution: Free
Acid=VNaOH used x Factor x 10 -The factor will be given by Metallurgist

15 Record the number (result) in the log -Write legibly

sheet

16 Clean work area after use -Maintain a good house keeping

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9.3 Copper titration

1 Get the 3 hourly samples for

different streams.
2 For slurry sample let it settle to get
clear solution to titrate
3 Clean the 10ml pipettes, 250ml
beakers
4 Ensure the reagents are available
and in good condition
Take 10ml of the required sample
solution to titrate and put it in the
250ml beaker
5 For electrolyte solution dilute the 10
. ml of sample solution with water in
to 100ml beaker before taking 10 ml
for titration.
6 Add 2.5 ml of starch and agitate
7 Dilute with water(distilled or tap
water if distilled water is not
available) the mixture to get 100 ml
in the beaker
8 Fill the thiosulphate in the 100ml
burette
Add drop by drop the sodium -Adjust the reagents speed (drop by drop) from the
thiosulphate in the beaker solution burette to get a correct end point.
9 until the solution colour become
white. Ensure that the beaker -At the end point do not confuse the colour change
solution is shake continuously until from dark to white for Copper titration.
we get the white colour
When you get the white colour stop
10 titration and read the volume
consumed.
Multiply the volume read by the -Read well the volume of sodium thiosulphate from
factor given. the burette.
Cu (g/l) = V used × Factor
11 For electrolyte solution :
Cu (g/l) = V used × Factor x 10 -The factor will be given by Metallurgist

Record the number (result) in the log - Write legibly

12 sheet

13 Clean work area after use -Maintain a good house keeping