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MINERAL PROCESSING COURSE

Sampling & Assaying

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Sampling

> Sampling is data collection

> Pierre Gy

> Purpose of sampling:-

― Qualitative sample for assaying

― Maintain process quality

― Improve process control

> Small proportion represents the bulk

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Sampling (cont.)

The best samples are taken at right angles to the free falling
stream, preventing:

― Particle size variation in belt loading

― Settling out of particles in the pulp due to velocity change

― Surges, etc.

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Sampling (cont.)

Continuous sampling:

― Performed at a uniform speed

― Produces increment samples

― Represents the entire stream at the time the sample was taken

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Sampling Methods

Two sampling methods:

> Manual

> Automatic or Mechanical

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Manual Sampling

Division sampling:

> Coning and quartering

> Riffling

> Pipe sampling

> Shovel sampling

> Grab sampling

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Manual Sampling (cont.)

Coning and Quartering:

> Relies on its radial symmetry to give four identical samples

> Two opposite corners are taken as the sample

> Other two corners are discarded

> Should not be used for accuracy sampling

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Manual Sampling (cont.)

Riffling:

> Splitting of sub-sample dry, free flowing material

> Sample is poured into the chute and split into equal

portions by the slots

> Accurate sampling

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Pipe Sampling

Pipe sampler:

> Is a piece of pipe

> Has one end with sharpened edge and the other fitted with a tee

and two short nipples to form a handle

> Is thrust vertically to the bottom of the heap at regular intervals

> Withdrawn and pounded with a hammer to release the sample

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Manual Sampling (cont.)

Shovel sampling:

> Involves taking a series of small scoops of sample and


placing them in a series of smaller piles

> The number of piles is determined by the sample size


requirement

> Individual scoops are placed on each pile in succession,


repeating until the original pile is completely distributed

> The number of scoops per pile range from 10 to 30 or more

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Manual Sampling (cont.)

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Manual Sampling (cont.)

Grab Sampling

> Taking a sample from the sample container by scoop

or spatula

> Grab sampling is not recommended as a sub-

sampling technique

> It fails to meet the Gy sampling criteria

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SAG Mill Sampling (Fimiston Circuit)

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Mechanical Sampling

> Mechanical Sampling provides:

― regular collection of unbiased samples


― deliver standards of operating reliability and sampling accuracy

> Automatic or mechanical samplers operate by moving a collecting


device through the material as it falls from a conveyor or a pipe

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Mechanical Sampling - Nine Rules

1. The cutter must fully traverse the stream with each cut

2. The cutter must have parallel edges and cut at 90 degrees to

the flow

3. The cutter opening must be at least 3 times larger than the

largest particle in the stream

4. The cutter velocity must be constant

5. The following stream must be in free fall

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Mechanical Sampling – Nine Rules (cont.)

5. The sample must pass quickly through the cutter to prevent

build-up or blockage

6. Sample must not spill from the cutter

7. The cutter should not degrade the sample

8. Changes in moisture content between stream and sample

should not occur

9. The minimum cutter aperture should be 30 mm

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Mechanical Sampler

Ratio between cutter width and the diameter of the largest


particle should be 20:1

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Modern Sampler

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Mechanical Sampling (cont.)

Most common samplers are:

> Linear cross-stream sampler

> Linear sampler in direction of flow

> Rotating arc path sampler

> Vezin Sample

> Poppet Sampler

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Mechanical Sampling (cont.)

> Vezin Sampler

― Consists of a revolving cutter in the shape


of a circular sector

― Various discharge angles up to 70° to


prevent material hang-up

― Adjustable sector cutter openings

― Inspection doors

― Small capacity fine size sampling

― Widely used for both slurry and solids


sampling

― Various models and linings to suit process


conditions
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Mechanical Sampling (cont.)

> Poppet Sampler

― Consist of a pneumatically
operated piston immersed
directly into the pipeline

― The cycle of opening and


closing is controlled by an
automatic timer, sample
level controller

― Pulp sampling

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Mechanical Sampling (cont.)

> Tilted Arc Sampler

― Sampling of high capacity solids


streams

― Coarse materials (up to 4 in. top


size)

― Rotating scoop

― Operation can be continuous, or


on single rotation cycles with a
timer

― Capability to handle more difficult


applications in moist, adhering
materials
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Mechanical Sampling (cont.)

> Rotating Splitter

― Cutter edges forming divider


segments

― Cutter edges subjected to


uniform wear

― Bias is avoided

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Mechanical Sampling (cont.)

> Linear Cross-Stream Sampler

– Properly sized cutter

– Travelling at the correct speed

– Produces a very accurate


sample of the stream

– Most economical sampler for


metallurgical assaying

– Applications at pipe,
conveyor, chute and launder

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Mechanical Sampling (cont.)

> Sliding Plate Sampler

― Used for primary or secondary


sampling of solids in vertical
chutes

― Accurate sampling of granular,


wet and sticky materials

― Sample prevented from process


air borne particles

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Mechanical Sampling (cont.)

> Linear Sampler in Direction of Flow

― The swing-arm sampler and


slotted belt sampler

― Sampling by linear traverse in


the direction of flow

― Cutters are integral to the


mechanisms

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Mechanical Sampling (cont.)

> Swing-Arm Sampler

― Consists of a bucket and drive


mechanism, preferably
hydraulic

― The bucket is driven on a path


to intersect the flow stream

― Cutter edges are positioned


perpendicular to the trajectory

― Loaded bucket is inverted for


discharge into a chute

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Mechanical Sampling (cont.)

> Conveyor Belt Sampler

― Accurate sampling of fines


to coarse material

― Typical used for sampling of


mill feed, concentrate, coal,
iron ore, sinter, pellets,
aggregates, limestone, etc.

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Mechanical Samplers

> Liquid Samplers

― Drip Samplers

― Placed within a pipe line,

― Are the most common and cheapest of samplers for liquids

― A valve, (gate, needle, K-type) is used to regulate the

sample flow

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Sampling

> Sampling Problems:


― The qualitative problem in broken ore sampling
― Particle intrusion, inter-granulation

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Plant Example

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Sample Preparation Area

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Sample Preparation Area (cont.)

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Sampling Errors

> Assay error (laboratory measurement error on small samples)

> Heterogeneity of material being sampled

> Fluctuations in mass or volume flow rate, causing error in the

sample

> Segregation and classification through cross section of

material on the belt

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Assaying

> Is the measurement of the amount of a substance in its


environment

― E.g. the determination of cyanide in CIP solutions or the


determination of gold in mine ore

> Assaying for gold is used to:

― Evaluate ore reserves

― Monitor mine feed to the processing plant

― Assay the bullion purity

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Atomic Absorption Spectrophotometry
(AAS)

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AAS (cont.)

> Sir Alan Walsh-CSIRO-Inventor


> AAS is an analytical tool
― It measures the amount of light absorbed by a metal
element
― For instance, gold has the wavelength of 242.8nm

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Assaying – Aqua Regia Method

> A known weight of ore is digested in hydrochloric and nitric acid

> A known volume of solution is contacted with DIBK

> Sprayed into the AAS to give a direct gold reading

> The Aqua Regia method is cheaper than fire assay but prone to under

assaying of sulphides and lateritic material

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Aqua Regia Assay

Au (s) + 3 NO3- (aq) + 6 H+ (aq) → Au3+ (aq) + 3 NO2 (g) + 3 H2O (l)

Au3+ (aq) + 4 Cl- (aq) → AuCl4- (aq)

The oxidation reaction can also be written with nitric oxide as the
product rather than nitrogen dioxide:

Au (s) + NO3- (aq) + 4 H+ (aq) → Au3+ (aq) + NO (g) + 2 H2O (l)

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Assaying (cont.)

> Fire Assay Method

― Accurate method of determining precious metals in ores

― Collection of the precious metals in a lead button

> Four dominant stages:

― Fusion

― Cupellation

― Acid Digest

― AAS

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Fire Assay

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Fusion and Cupellation

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Weighing or AAS Reading

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XRF Assay

> Pressed powders

> Glass beads

SIZE ASSAY DISTRIBUTION

WEIGHT %
50
IRON
45 PHOSPHOROUS

40 SILICA
ALUMINA
35

% DIST
30

25

20

15

10

0
38.00 25.00 15.00 10.00 6.30 4.00 3.35 1.18 -1.18

SIZE (mm)

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XRF Assay Facilities

XRF facilities at Cloudbreak

Robots processing XRF samples

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General Analytical Procedures CIP/CIL

> pH measurement

> Cyanide concentration

> Alkalinity

> Oxygen measurement

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General Analytical Procedures CIP/CIL
(cont.)

> pH measurement

― Used to maintain optimum leach conditions

for the cyanide

― Generally above 10.5

― In saline solutions sometimes down to 8.5

prevents precipitation of insoluble salts

> To measure pH, a pH meter and probe is used

― Calibration at pH 7.00 and pH 9.23 or 4.00

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General Analytical Procedures CIP/CIL
(cont.)
Cyanide concentration

> Cyanide analysis in the leach and tailings

> Titration with silver ions

2CN ( aq)  Ag ( aq)  Ag (CN ) 2 ( aq)


Ag (CN ) 2 ( aq)  Ag ( aq)  Ag[ Ag (CN ) 2 ]( ppt)

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General Analytical Procedures CIP/CIL
(cont.)

> Titration:

― 1ml or 1 drop (10%) of


potassium iodine added to 10
mL of cyanide solution

― Solution titrated with silver


nitrate until change in colour

― End solution is of milky


appearance

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General Analytical Procedures CIP/CIL
(cont.)

> E.g.
– 3.000 g of AgNO3 were dissolved in 1 litre of solution and
is thus 0.3% AgNO3

Mwt ( AgNO3 )  107.9 ( Ag )  14.01( N )  3  16.00 (O)


169.0 g

m 3.000
 moles ( AgNO3 )  
M 169.0
 0.01775 moles

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General Analytical Procedures CIP/CIL
(cont.)

> For every ml of AgNO3 there exists:

g / ml ( NaCN )  moles of AgNO3  moles per liter  moles of cyanide in the sample
0.01775 49
 1 
1000 20
5
 4.349 10 g NaCN / mL of solution
 4.349 10 5 kg NaCN / tonne of solution
 0.004349 % NaCN in solution

> If 15.25 moles of AgNO3 are used there is:

― 0.004327 x 15.25 = 0.066% NaCN in solution

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General Analytical Procedures CIP/CIL
(cont.)

> Alkalinity

― Protective alkali

― Stops decomposition of the cyanide in solution

― Analysis for calcine (CaO)

― Titration with oxalic acid

> Titration

― 10 ml of cyanide solution mixed with phenolphthalein

― Titrated with oxalic acid until colour change

― Endpoint color should be pinkish

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Marcy Scale-Density

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MLA

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General Analytical Procedures CIP/CIL
(cont.)

> Oxygen measurement

― Critical factor in controlling the leach

rate

― TPS type meter used for measurement

― Calibrated for 0 ppm in sodium

metabisulphite and in air for 7 ppm

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Instream Analysis

> AMDEL Probes

> Courier Systems

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IRONSCAN – Al, Si in Ore

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