Met - Test - Methods - Ausimm
Met - Test - Methods - Ausimm
Met - Test - Methods - Ausimm
METHODS
(RENISON, TASMANIA
3 Laboratory sizing...................................................................................................... 14
3.1 Introduction .................................................................................................................. 14
3.1.1 The ASTM Sizing Scale..................................................................................... 14
3.1.2 The Ro-Tap Testing Sieve Shaker .................................................................... 15
3.1.3 Preliminary Comments on Sieving Procedure................................................... 15
3.2 Dry Screening .............................................................................................................. 15
3.2.1 Purpose ...................................................................................................... 15
3.2.2 Technique ...................................................................................................... 15
3.2.3 Equipment Required .......................................................................................... 15
3.2.4 Sample Preparation ........................................................................................... 16
3.2.5 Procedure ...................................................................................................... 16
3.2.6 Calculations ...................................................................................................... 17
3.2.7 Weighing of Residue.......................................................................................... 18
3.3 The Cyclosizer ............................................................................................................. 18
3.3.1 Purpose ...................................................................................................... 18
3.3.2 Principles ...................................................................................................... 18
3.3.3 Equipment ...................................................................................................... 19
3.3.4 Procedures ...................................................................................................... 19
3.4 Additional References.................................................................................................. 20
5 FILTRATION ............................................................................................................ 25
5.1 Introduction .................................................................................................................. 25
5.2 Leaf Filter Testing ........................................................................................................ 25
5.3 Test Data Format ......................................................................................................... 26
5.4 Preliminary Information ................................................................................................ 26
5.5 Laboratory Pressure Filtration...................................................................................... 27
5.6 Steps for Leaf Testing.................................................................................................. 27
5.7 Factors Affecting Filtration Rates and Cake Moistures ............................................... 28
6 AGGLOMERATION ................................................................................................. 31
6.1 Introduction .................................................................................................................. 31
6.2 Procedure..................................................................................................................... 31
8 Magnetic separation................................................................................................. 42
8.1 Introduction .................................................................................................................. 42
8.2 Laboratory Magnetic Separator ................................................................................... 43
8.3 Procedure for Using the Laboratory Separator............................................................ 43
9 introduction .............................................................................................................. 44
9.1 Electrostatic Separation ............................................................................................... 44
11 LEACHING............................................................................................................... 49
11.1 Theoretcial Overview ................................................................................................... 49
11.1.1 Leaching of Minerals.......................................................................................... 49
11.1.2 Leaching of Metals............................................................................................. 50
11.1.3 Leaching of Oxides ............................................................................................ 51
11.1.4 Leaching of Sulphides ....................................................................................... 52
11.2 Leaching Procedures ................................................................................................... 54
11.2.1 Performance of a Standard Bottle Leach Test .................................................. 54
11.2.2 Bottle Leach Procedure for Cyanidation............................................................ 55
11.2.3 Column Leaching Procedure ............................................................................. 56
11.2.4 Free Cyande Determination .............................................................................. 57
12 flotation .................................................................................................................... 58
12.1 Theoretical Overview ................................................................................................... 58
12.2 Laboratory Flotation Testing ........................................................................................ 58
12.2.1 Pre-Flotation Procedures................................................................................... 58
12.3 Oxide Flotation ............................................................................................................. 59
12.3.1 Flotation of Cassiterite Ores .............................................................................. 59
Collector Type .............................................................................................................. 60
12.3.2 Flotation of Tungsten Ores ................................................................................ 62
12.4 Sulphide Flotation ........................................................................................................ 63
12.4.1 Flotation Agents................................................................................................. 63
12.4.2 Types of Sulphide Occurrences ........................................................................ 65
12.5 Standard Flotation Test Procedure.............................................................................. 69
12.5.1 Treatment of Products ....................................................................................... 70
12.5.2 Record of Information ........................................................................................ 70
12.5.3 Additional Notes................................................................................................. 70
List of Appendices
Appendix 1
1 INTRODUCTION
This laboratory manual attempts to collate operating and test procedures at the CMS
laboratory with the following objectives in view:
To enable easier comparison and acceptability of CMS laboratory data with those from
outside laboratories, reference is made to relevant Australian and International standards.
The wide diversity of testing procedures utilised at the laboratory necessitate the highest
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various portions of the manual and it is recommended that they be strictly adhered to.
Ore characterisation studies the mineralogical relationships within a potential ore and the
detailed responses of that ore to specific physical and chemical upgrading procedures. It
forms the basis of metallurgical process design or process modifications.
x crushing, grinding and screening tests with associated assaying and mineralogy to
determine breakage (work index) and liberation modes;
x physical beneficiation steps like heavy liquid separation, flowing film tests, magnetic and
electrostatic separation;
x physico-chemical concentration processes, e.g. flotation; and
x chemical concentration procedures like leaching.
Table 1.1 (Missing) illustrates the information obtainable from these tests, by applying
experience, and good mineralogical backup, it should be possible to make reasonably
accurate estimates of recovery.
It is recognised that the validity of sophisticated test work hinges on correct sampling and
preparation techniques. Specific procedures are outlined. With large numbers of samples it
is important that, apart from normal precautions to prevent cross-contamination, sample
comminution preparation procedures at CMS, i.e. techniques of jaw and rolls crushing and
pulverisation, should take into account liberation characteristics of the ore-body evident from
preliminary size analysis data, rather than achieve a blanket size reduction to a specific fine
size for all ores.
Heavy liquid analysis, derived from washability tests in the coal industry, constitute an initial
assessment of any specific ore body. These tests yield qualitative data on liberation, and the
amenability to gravity separation, preconcentration techniques and flotation.
Subsequent release analysis, flotation, magnetic separation and leaching tests provide
specific metallurgical data of particular relevance to recovery and grade.
x Suitability of the ore for heavy liquid testing is assessed by the requirement that
combined CO2 + Fe + S is < 50% and SiO2 is > 30%.
B B B B
Laboratory heavy liquid testing will be recommended for samples < 4kg. Larger bulk
samples with a topsize up to 40mm may be tested with an Erickson cone.
Independent of the above steps, ore characterisation studies should desirably envisage:
The ultimate aim of all ore characterisation exercises should be the determination of detailed
and optimum metallurgical response to specific unit concentration steps, specifically grades
(enrichment ratios) and recoveries realistically attainable, to enable onward plant design. It
is likely that in most cases, full scale-up to mill operating tonnages may be difficult without
intermediate scale pilot-plant testing.
2.1 Introduction
This section of the laboratory manual discusses aspects of sample preparation as well as
operating details of individual crushing, grinding and classification equipment. The individual
steps outlined are recommended for guidance purposes. A suggested time frame, where
applicable, is indicated for some unit operations (sequence of steps) to help with planning
specific test programmes.
x If samples are bulky and require size reduction, reduce to a workable size as per Gy’s
sampling equation (Appendix 1).
x Pack samples into plastic bags each with detailed identification labels.
x If samples are not to be worked on straight away, store them in the sample storage area.
The method which is used for sampling large quantities of material say 20kg, consists of
pouring or forming the material into a conical heap upon a solid surface (e.g. a steel plate)
and relying on radial symmetry to give four quarters when the heap is divided by a cross.
Two opposite corners are taken as the sample the other two set aside. The portions chosen
may be further reduced by a repetition of the process, until the required size of sample is
obtained.
This sample splitter is an open V-shaped container under which a series of chutes are at
right angles to the long axis, giving a series of rectangular slots of equal area. These
alternatively feed two collection trays. The sample whose particular size allows free
movement through the slots (the largest particle being one-third the riffle opening) is poured
into the feeder and becomes split into equal portions. After repeated cycles the desired
sample size is obtained.
1. Set up sample and riffle, ensuring that the riffle is initially clean.
2. Riffle once.
3. Repeat riffling, discarding every alternate sample.
4. Bag sample and label – store excess sample.
5. Clean riffle.
The sample of core may be delivered a whole or split core, usually in lengths not exceeding
150mm. Each core sample should be weighed so that any future compositing may be done
on a weight basis if needed. Prior to any crushing, a portion of each core is retained in its
original condition for mineralogical examination, and depending on a visual assessment, a
slice may be cut along or across the axis of one or more pieces of each core.
2.5 Crushing
This is the first stage performed in the size reduction of a sample leading to some liberation
of minerals from gangue and is a dry operation involving use of a jaw crusher, followed by
screening and rolls-crushing.
The laboratory sample preparation room is equipped with a 200 x 130mm jaw crusher and a
200 x 150mm rolls-crusher, both manufactured by Altec WA.
Materials fed to these crushers must be limited to a certain top-size and feed rate as
prescribed in the maker’s instruction manuals. Lubrication requirements and the procedure
for the alteration of settings are set out clearly in these manuals, which are kept near the
machines.
SAFETY GLASSES AND EAR MUFFS ARE PROVIDED AND MUST BE USED
When changing the gap between the rolls, adjust both nuts equally so that the rolls remain
parallel to each other. Gap openings can be set with standard lead cylinders, the diameter of
the latter being equivalent to the jaw opening. Apply lock cut procedure.
Steps:
1. Jaw and rolls crush if required – Riffle out head sample.
2. Wet screen at 38 microns; dry the products and record their weights.
3. Riffle out 200 gram of the oversize and screen at the desired sizes.
4. Weigh each fraction including the –38 micron fraction and record.
5. If required, cyclosize the –38 micron fraction as per procedure.
6. Weigh each fraction from the cyclosizer and record.
7. All samples being sent for metallurgical analysis should be pulverised and neatly
bagged and labelled.
8. Ensure that each work area inclusive of screens, buckets, beakers, pulverisers etc.
are thoroughly cleaned after use.
9. Calculate and tabulate distributions from returned assays.
2.6 Pulverising
This operation prepares the sample for metallurgical analysis by reducing to a particle size,
usually –10µm, so that the mineral is exposed to dissolution by the normal assay solvents or
meets the requirements of x-ray fluorescence determination.
Pulverising grinders used in the sample preparation room are of two types:
x the disc pulveriser, generally for sample >1kg, where the material is fed through a hopper
and enters a space between the discs, one of which is revolving, the other stationary.
Fineness of product is determined by a screw adjustment;
To ensure that in every case, sufficient pulverising is achieved minimal pulverising time
should be ~2½ minutes. Further, it is recommended that one in every two hundred
samples is tested for consistency in liberation. Difficulties in attaining metallurgical
balances often can be traced back to insufficient pulverising.
* If sample appears to be damp, submit it to drying under the lights before pulverising.
2.7.1 Purpose
2.7.2 Principles
Grindability of a material depends upon its hardness, structure, the manner in which it is
fractured, water of combination, hygroscopicity, tendency of flocculate and agglomerate,
combustibility and sensitivity to changes in temperature. The grindability is useful in
evaluating power requirements for grinding. To design a particle breakage system it is
important to know the energy required to achieve a given size reduction. The most
commonly used energy-size relationship is Bond’s third law equation.
W
Wi = 10 - 10 ..................................... 1 (a)
¥P ¥F
10 Wi¥F 2
P= W¥F + 10Wi ..................................... 1 (b)
For the ball mill grindability test, the work index is calculated from the following revised
equation:
Wi = 44.5
(P ) 0.23
i
B B
x
(Gpb)
0.82 x 10 - 10 .................................... 2
¥P ¥F
where:
3.68 43 7880
2.97 67 7847
2.54 10 511
1.90 71 2143
1.55 94 1744
20.125kg
- Agitator rolls.
- Measuring cylinder, 700ml volume.
- Set of screens, including the following sizes:
850µm, 600µm, 425µm, 300µm, 210µm, 150µm
- Ro-tap machine, with timer.
- Drying facilities.
- Pressure filter.
2.7.4 Procedures
1. Carry out wet and dry sizing on the split sample. The percentage of undersize from the
screen which is the required size (297µm in this case) is the percentage of finished
material in the feed.
2. Fill the 700ml test can with ore and compact by shaking. Add more ore as necessary
until further compaction ceases.
3. Weight and transfer ore to the ball mill.
4. Grind dry for 100 revolutions.
5. Empty the ball charge and ore through a coarse screen to separate the balls from the
ore.
Calculations:
Number of revolutions required to produce 250% circulating load can be calculated using
following formula:
W (Y) (P) R
X= 3.5 100 U ....................................... 3
where:
X = number of revolutions required.
W = weight of original feed.
Y = corrected weight undersize previous cycle.
P = percent undersize in original feed.
R = revolutions previous cycle.
U = actual undersize produced previous cycle.
d80 = X + Y (Z - X) ....................................... 4
where:
d80 = 80% passing size.
X = micron size of screen through which nearest percentage below
80% passes.
Z = micron size of screen through which nearest percentage above
80% passes.
Y = ratio of the difference between 80% and the nearest cumulative
percent below 80% AND the difference between the nearest
cumulative percent above 8p% and the nearest cumulative percent
below 80%.
841 98.35
495 92.71
420 84.32
297 78.65
210 65.30
149 52.18
d80 = X + Y(Z - X)
Ball Mill Grindability (Gpb) = (gm/rev) average of last three grinding cycles to give 250%
circulating load.
There should be consistency in compaction of ores in the 700ml test can. This is
normally done by shaking.
2.8.1 Purpose
The test is designed to give a reasonable indication of the grinding work index of an ore
material relative to one or more known standards. It is not applicable to mill tailings material.
CMS ball mill No.1 with approximately 10kg of ball charge distributed as follows:
Ball Diameter %
1½“ 20
1“ 50
¾“ 30
100
Procedure
1. Crush the known and test samples to -3350 micron using either the jaw or rolls
crusher.
2. Riffle split the crushed sample. Weight out approximately 300 grams for feed sizing
and exactly 1000 grams for grinding.
Wash the pulp thoroughly from the mill and the charge, wet screen the pulp @ 75 microns
and dry product.
Dry screen the oversize (+75µm) product on 1680, 850, 600, 425, 210, 106, 75µm.
Plot feed and product sizings on a log-normal graph sheet as cumulative weight % passing
versus particle size. Each particle size is determined by calculating the geometric mean size
(GMS) of two successive screens used. For example, GMS of –3350 + 2440µm size range
equals to:
¥ 3350 x 2440µm
= 2830µm
Read off F80(µm) and P80(µm) from the plots and calculate the comparative grinding work
B B B B
Calculation
U
1 1 1 1
CWi x = RWi x
¥ P80 ¥ F80 c ¥ P80 ¥ F80 R
where R refers to the reference standard sample of known Wi and C refers to the unknown
sample.
Caution
U
For the comparison to be valid, the following rules of thumb should be noted:
- Feed size distributions of the reference sample and unknown should ideally be similar.
- Grinding conditions must be identical.
3 LABORATORY SIZING
3.1 Introduction
Since the effectiveness of practically all mineral processing operations is a function of the
size of the particles treated, a thorough knowledge of the size characteristics of the materials
handled is of the greatest importance. Hence, the significance of consistent and reliable
laboratory sizing techniques. The two most important sizing methods are:
1. Screening
2. Classification (Elutriation)
The ASTM scale is based on a geometric progression, i.e. ore in which successive grades
are in constant ratio, e.g. ¥ 2 . For practical manufacturing reasons, the reference screen
opening is that of the so-called 200 mesh screen. This standard screen is a woven screen
having 200 wires per linear inch, and likewise 200 openings per linear inch, in which the
opening is a square having an edge of 74 microns or 0.074mm. Graphical Representation of
Sizing Analyses
x Cumulative plot where the ordinate is the percentage of the total weight coarser than a
given size, the abscissa, the particle or screen opening (mm or microns).
x Plot of percentage of the total weight included within consecutive divisional sizes (i.e. the
amount retained by each screen and passing the screen immediately larger) (ordinate)
versus actual screen opening in mm or micron. This type of plot could be misleading in
that uneven emphasis is placed on the various size ranges. Difficulties could also be
experienced in dealing with the material finer than the finest screen to which the sizing
operation is conducted. Useful data can often be obtained by using a log scale for
particle size (abscissa) versus cumulative percentage retained (ordinate) or direct
percentage retained by individual size.
This machine causes a circular motion of the material on the screen; the frame in which the
screens are placed is provided with a translatory motion at one end and a circular motion at
the other so that there is eventual movement of the material on the screen. Besides, a blow
is delivered to the nest of sieves, once for each revolution of the frame. A nest of sieves,
consisting generally up to six screens, and occasionally 12, is shaken in the machine for from
5 – 20 minutes depending upon the extent to which it is desired to approach the end point of
the screening operation.
If proper care is taken not to overload the screens, and the material is deslimed (i.e. rejection
of –38 micron fraction) and dried, machine screening gives excellent results. Most
satisfactory results are obtained when the amount of material on each screen, at the end of
the screening operation, does not exceed that required to form a layer one particle deep.
However, a bed of particles of extremely fine particles to coarser particles or to each other
through electrostatic action or the presence of minute amounts of moisture can be overcome
by a combination of wet and dry screening.
3.2.1 Purpose
Dry screening is used to determine the size distribution of particles coarser than 38 micron.
For an accurate determination, it is necessary to deslime at 38 micron before
commencement of dry screening.
3.2.2 Technique
1. Set of standard screens, including bottom pan and lid. The usual range of sizes includes
4760 micron, 2380 micron, 1190 micron, 841 micron, 595 micron, 297 micron, 210
micron, 149 micron, 105 micron, 74 micron, 53 micron, 44 micron, although not all of
these sizes will necessarily be used in a given test.
5. Weighing pan.
2. Split material to get the approximate sample size required, as per schedule below:
3.2.5 Procedure
1. Starting with the finest screen, stack the screens on the bottom pan in order of increasing
micron size. The top screen will be the coarsest one in the nest.
3. Place the sample on the top screen, and secure the lid in place.
6. Starting with top screen (coarsest one), transfer the screen fraction to the weighing pan
and accurately record and weight. Use a brush to remove wedged particles from the
screens.
7. Always brush up and down a screen, never brush with a circular motion.
9. All data and calculations are to be recorded on the standard screen Analysis Data sheet.
10. Plot weight per cent of each screen fraction, and the cumulative per cent undersize.
Size Distribution
wt% of a screen fraction = Weight of Screen Fraction x 100
Total Sample Weight
Also, cum.% passing = 100 - (Total per cent of fractions not passing the screen)
d80 = X + Y (Z – X)
where d80 = 80% passing size
X = micron size of screen through which nearest percentage below
80% pass.
Z = micron size of screen through which nearest percentage above
80% passes.
Y = ratio of the difference 80% and the nearest cumulative per cent
below 80% AND the difference between the nearest cumulative
per cent above 80% and nearest cumulative per cent below 80%.
Sizes Cum. %
Microns Passing
841 98.35
595 92.71
420 84.32
297 78.65
210 65.30
149 52.18
d80 = X + Y (Z - X)
x Accurate weightings compatible with an overall accuracy of ± 0.2% are mandatory for all
screen products.
x For screen undersize from rinsing operations, do not remove undersize from filter paper
U U
before weighing.
- Tare a clean filter paper of same size and type as that used as undersize.
- Weigh undersize plus filter paper.
- Weight shown on tared balance will be the weight undersize.
By following this procedure, no material is lost with the filter paper or with a transfer
operation.
NOTE: Always be sure that the balance is properly zeroed before commencing a
weighing.
3.3.1 Purpose
3.3.2 Principles
One of the most widely used methods of sub-sieve sizing in modern mineral-processing
laboratories is the Warman Cyclosizer which is extensively used for routine testing and plant
control in the size range 8 – 38 micron for minerals of specific gravity similar to quartz (s.g.
2.7) and down to 4 micron for particles of high specific gravity, such as galena (s.g. 7.5).
1
TP PT Adapted from “Mineral Processing Technology – B. A. Wills”; Pergamon Press, 2nd Edition.
P P
The tangential entry into the cyclones induces the liquid to spin, resulting in a portion of the
liquid, together with the faster-settling particles, reporting to the apex chamber, while the
remainder of the liquid, together with the slower settling particles is discharged through the
vortex outlet, and into the next cyclone in the series. There is a successive decrease in the
inlet area and vortex outlet diameter of each cyclone in the direction of the flow, resulting in a
corresponding increase in inlet velocity and an increase in the centrifugal forces within the
cyclone, resulting in a successive decrease in the limiting particle-separation size of the
cyclones.
3.3.3 Equipment
x Warman Cyclosizer
x -38 micron sized material
x Beakers
3.3.4 Procedures
1. Switch on both power points at wall and check hot and cold water main valves open.
Also check hot water control valve open. Also check that automatic water temperature
(23° ± 2°C) is correctly set and operational.
2. Plug in sample chamber.
3. Switch on pump.
4. Open rotameter valve.
5. Close pot discharge valves (after removing air).
6. Check the room temperature.
7. Set timer to five minutes (Feed Cycle) and open sample chamber slowly to feed particles
within five minutes.
8. After feed time (five minutes) buzzer sounds. Set timer to separation time (20 minutes)
and adjust rotameter flow down to 185 (as for 5).
9. After separation time (20 minutes) buzzer sounds; adjust rotameter flow up to 200.
10. Discharge CS5 pot product in to 1 litre beaker and return plastic hose to drain.
11. Repeat discharge of CS4, CS3, CS2 and CS1 in that order as for (10)
12. Shut off rotameter valve.
13. Open all valves.
14. Switch off pump.
15. Switch off power points at wall.
16. Dry, weigh and pack each fraction.
N.B. If separation time, water temperature, flow rate or s.g. of solids (2.7) are different to
above, correction factors will be required for cyclone cut sizes.
CS 1 2 3 4 5
Micron 45 34 24 16 11.5
Precaution
Read the Warman instruction manual carefully and inspect the cyclosizer, noting all the
component parts and how to operate them. Do not operate the machine until you are
sure of the procedure.
4.1 Flocculation
Flocculants are added to suspensions of solids in water to cause the individual particles to
collect in the form of flocs. The formation of flocs aids in improved settling rates, better
overhead clarity and/or faster filtration rates. There are three main methods for achieving
aggregation of very small or colloidal particles in suspension:
There are basically three types of organic polymers (or flocculants) that can be used,
nonionics, anionics or cationics. The nonionics which are a neutral polymer molecule, have
a wide application and can be used as flocculants for most solids in acid, basic or neutral
conditions. In some systems where flocculation is dependent upon the “ionic” charge of the
particles a polymer with either a positive or negative charge will aid in the attachment to the
solid particles and hence improve efficiency of flocculation. The charge of the particles is
dependent on a number of factors and is usually pH dependent. If the charge on the particle
is overall positive, then an anionic polymer will be most suitable and vice versa.
The solubility of polymers varies considerably, but in general is very low and therefore they
should be prepared as a very dilute solution, usually less than 1% by weight. Addition of the
polymer aqueous solution should be very slow, with slow agitation.
The method of application is also important. With most flocculants adsorption is rapid and
irreversible, so thorough and complete dispersion of the flocculant throughout the slurry is a
necessity. The recommended techniques of application for maximum efficiency are as
follows:
Consumption of flocculants usually range from 0.005 to 0.2 kg/tonne of dry solids.
4.2.1 Introduction
The choice of test method depends to some extent upon the temperature of the pulp, its
flocculating characteristics, the required supernatant clarity, and the equipment available.
4.2.2 Methods
The Long Tube Method may be used for all materials which settle without a clearly defind
interface. However, where the feed in question is well flocculated, either naturally or
artificially, a simplified test method as indicated below may be used to obtain significant data.
1. Place pulp in a measuring cylinder and make up to say 1000 ml mark with water. Shake
thoroughly after addition of flocculant.
2. Allow to settle quiescently and note interface depth as a function of time (seconds).
4. A log-log plot of this data usually will give a straight line of slope m.
5. The static detention time calculated for the desired overflow clarity, and the observed bulk
settling rate may be used, with proper scale-up factors that determine sedimentation area
and depth requirements.
1 _ _1
Unit area m2 / tpd = 0.0415
CG CF
R
4.3.1 General
Beaker decantation is a technique used to separate a mineral sample into two size fractions
according to the differences in settling velocities of the particles. It is a technique which can
be used to accurately split a sample at a pre-determined cut size but has some
disadvantages in that it is a time consuming method especially when splitting at fine sizes.
Also a dilute solids content is required to stop natural coagulation from occurring. A
spherical shape is assumed for the calculations.
The procedure is based on Stokes Law which relates the settling velocity of a particle to its
size and specific gravity through the equation.
P
VT =g( P P PB B – PF) (DST)2
P PB B P P
18VF
V
where P
T PB B = terminal settling velocity of particle
D
P
ST PB B = equivalent Stokes diameter of particle
g = acceleration due to gravity
VF = fluid viscosity
By calculating the settling velocity of a particle of the required cut size and specific gravity,
the time for the particle to fall a certain distance unhindered through the liquid, can be
calculated.
4.3.2 Procedure
Preliminary
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x A settling vessel is required, the size of which depends on the amount of sample and the
cut size chosen. The vessel should be large enough to avoid any form of coagulation
which would interfere with the unhindered settling of the particles. The higher the settling
height the longer the settling time – sometimes several hours.
x A syphon to remove the fluid containing the unsettled particles and decantation
equipment, usually consisting of a plate with a tube attached with facilities to set at a
predetermined depth. Decant fluid can then pass over the plate and up the tube.
x Enclose entire system in a water bath to maintain constant temperature and viscosity
and reduce disturbances to the sedimentation process, if complete accuracy is
required.
4.3.3.1 Procedure
Place the sample in the sedimentation vessel and fill with water up to the required level. If
the sample was previously dry, complete rewetting of the sample must be performed.
Ultrasonics may help in the wetting process. To ensure sample does not naturally coagulate,
dispersants should be used, but only if no further processing of products is to be performed.
If natural coagulation does occur, more dilution may be required.
Check that all the decanting equipment is ready with the tube set at the correct height, but do
not leave the tube in the liquid during the settling period.
Measure water temperature (to calculate viscosity of fluid) and maintain as constant as
possible.
Position the decantation tube delicately into position prior to completion of settling.
Remove the supernatant dispersion as quickly as possible. Do not disturb the settled
particles.
Repeat the above procedure several times until clear supernatant is obtained. The
separation efficiency is determined by the number of decantation steps.
Collect all the supernatant, flocculate, dry and weigh to obtain a weight balance.
5 FILTRATION
5.1 Introduction
Filtration is defined as the separation of insoluble solids from a liquid by forcing a portion of
the liquid through a porous medium by a pressure differential, while the solids are trapped on
the surface or in the depth of medium. The two main methods that exist to create the
required pressure differential are:
The “leaf test” represents a small section of a continuous filter incorporating typical fliter
medium support and filtrate drainage. When used with techniques properly simulating the
continuous filter, it can give results adequate for sizing production filters and predicting
performance or determining the need for pilot testing.
The test data format (missing) calls for the minimum of essential data and calculated rates.
The feed % solids analysis on the bulk sample being tested is the “feed basis”. By dividing
the cake dry weight by the sum of cake wet weight (vol x specific gravity), the “product basis”
feed % solids is determined. A significant difference between the two is evidence that the
system is not at equilibrium due to filter thickening, inadequate or excessive agitation, or
excessive loss of solids to the filtrate.
The actual vacuum throughout a test should be controlled and observed since this is a major
factor in performance and sizing.
Further slurry information desirable is: its physical nature; plant upstream process and
possible variations to meet filtration objectives; the solids settling tendency and hence gravity
thickening possibilities; whether solids are naturally flocculated or amenable to flocculation;
temperature variations; flexibility for pH adjustment; aging effect inherent in the process,
particle shape and variations with size; variations of the kind solids with size (eg. % ash may
be higher in fine particles); porosity of individual particles; solubility of filter cake; inherent
water of hydration; impurities; temperature of permitted oven drying. Other useful liquor
information is: soluble solids content and their relation to saturation; viscosity; surface
tension, vapour pressure variation with temperature; compatibility with flocculants.
Measure and record the filtrate volume. When the cake has a mushroom shape requiring
exclusion of the trim weight, the same proportion of filtrate must also be deducted. Comment
on the quality of the filtrate, testing for solids content when pertinent. Measure and record
the specific gravity and pH of filtrate.
The laboratory batch pressure filters installed at CMS serve the primary purpose of
dewatering solid-fluid suspensions and have not been designed for the performance of
specific pressure filter tests. However, by maintaining operating parameters constant e.g.
slurry % solids, overall pressure applied and overall filtration time, it is possible to obtain
comparative filterability data.
Stir the slurry with a spoon or spatula or an agitator to obtain a uniform suspension of the
solids.
Turn on the vacuum source and adjust the test vacuum while pinching off the hose to the test
leaf.
Submerge the leaf in the slurry, open the hose and simultaneously start the timer. Stir the
slurry as needed during form time.
At the end of planned formtime rotate the leaf up and out of the slurry just as a filter section
and dry. During the dry time slowly rotate the leaf, tilting it from it horizontal plane to half
drain the leaf. Dry for the planned time. Note the time of any cake cracking.
Turn off the vacuum, quickly remove the tubing from the flask to break the vacuum on the
leaf. Elevate the leaf and drain remaining filtrate to the flask. If necessary to facilitate
draining, lift a portion of the cake off the cloth.
Explore the best method of cake discharge as detailed under 11 below. If cake is
mushroom-shaped, extending beyond the 0.1 ft2 cloth area, trim off and separately weigh
the trim. Note: this correction is approximate.
Transfer the 0.1 ft2 cake to a tared dish. Again allow leaf to drain residual filtrate to the flask.
Set the leaf aside.
Weigh the dish and contents. Record the gross wet weight. Put the dish in an oven at 1050C
or lower temperature if necessary. Dry overnight, then record the gross dry weight.
Alternatively, use drying lights until a constant dry weight of the filter cake is obtained.
Generally the large the particle size, the higher the filtration rate in Kg/m2/h and the lower
P P
the cake moisture. However, the validity of the last statement depends on other factors,
e.g. distribution specific gravity of solids, absence of slimes and feed concentrates. For
instance, a small average particle size, but with a narrow distribution range and no
slurries, will have a high rate.
The slimes or extreme fines in a filter feed slurry affect filtration rates to a vastly greater
extent than their percentage. The residual cake moisture is similarly seriously affected.
A particularly difficult slurry is one that contains relatively coarse particles and a number
of very fine or slimy particles with little or no intermediate size.
Filter aids like diatomaceous earth, perlite, powdered coal, fly-ash or paper pulp may be
added to the flurry to increase its filtration rate and cake porosity.
In general, the greater the percentage of suspended solids in a given slurry, the higher
the cake filter rate in Kg/m2/h and the lower the filter rate in m3/m2/h. Where maximum
P P P P P P
x Filter Thickening
Filter thickening normally occurs in a continuous filter rotating in a tank containing slurry
wherein the solids in the filter tank increase in concentration and shift to a coarser size
distribution. While an equilibrium concentration and size distribution is usually obtained,
it may sometimes be necessary to dilute the pulp.
x Slurry pH
Since slurry pH and particle dispersion are closely related, changes in pH could be one of
the most effective methods to achieve flocculation and improved filterability, if the
process can tolerate it.
Flocculation is generally desirable for slurries of fine solids which are in a dispersed state
and generally filter poorly. The wide variety of polyelectrolyte flocculants provides room
for a substantial improvement in filtration rates. Effective use of flocculants, especially
polyelectrolytes, on moderately high concentration filter feeds requires strong agitation to
get good solids-flocculant contact. A minimum of further agitation and minimum aging
are important.
Some slurries may be so viscous as to create filtering problems and a dispersant may be
a better way to gain fluidity than dilution.
x Slurry Age
Sometimes processes involve detention times whether international or not, which provide
a conditioning effect, modifying filter performance. Samples shipped for testing involve a
risk that excessive aging may have some effect on filterability.
This is one of the most significant variables both in filtration rate and rate of dewatering to
a minimum moisture. Viscosity is closely related to temperature. As temperature is
increased, viscosity is decreased resulting in a higher filter capacity and lower cake
moisture.
As the same time, increased vapour pressure will help reduce moisture.
x Agitation Speed
Some slurries, particularly with a wide particle size range, tend to classify in the test
slurry container or the filter tube. Increasing the agitation speed (or stirring) to a point
that the coarse and fine particles are always thoroughly mixed may be desirable although
too high a speed could limit cake thickness, prevent coarser particles from forming in the
cake or cause delicate flocs to break down.
Filtering characteristics of fabrics depend mostly on the type of yarn and weave. Yarns
can be momo-filament, multi-filament, spun from staple fibre, or a combination of the
latter two. A high twist can make a multi-filament perform more like a mono-filament.
Permeability and porosity are prime qualities in cloth selection. The Frazier permeability
rating, expressed as cfm/sq ft, is a measure of air flow at one-half inch water pressure
through a dry cloth, and is comparable to per cent open area.
Cloth conditioning refers to the reduction of pore size or open area due to entrapment of
fine solids in the interstices.
x Applied vacuum
The applied vacuum creates the pressure differential which is the driving force for
filtration and dewatering. High vacuums give somewhat higher rates and lower moistures
in all cases except for unusually incompressible cakes or where the filter medium
becomes more conditioned. With coarse particles and porous caked lower vacuums (e.g.
5”-10” Hg) may be adequate. With such porous cakes, the vacuum capacity (m3 / m2 )P P P P
x Cycle Time
Cycle time of leaf tests is analogous to the filter drum speed, generally expressed in
seconds or minutes per revolution. Generally the faster the drum speed, the higher the
output. However, under these conditions, the cake is thinner and sometimes wetter, so
discharge may deteriorate. At all times, a dischargeable cake must be produced. Any
final selection of cycle or drum speed is a compromise of these conditions.
x Surface Tension
x Cake Compression
Cake compression is normally achieved as an adjunct to the filtration step to reduce cake
moistures of compressible cakes.
6.1 Introduction
Agglomeration is the formation of aggregate by the sticking together of feed and/or recycle
materials, and it includes the formation of agglomerate nuclei. The main objective in
agglomerating fines being the conversion of ores, minerals and chemicals of undesirable
fineness into agglomerates characterised by a size consistency desirable for subsequent use
or processing. In metallurgical applications, the unit process of balling aims at achieving
highly permeable large aggregates with a built-in ability to withstand large crushing forces.
The latter can be achieved by resorting to particular binder additions which confer structural
integrity to the ball or pellet after a specified curing period. The ability to form strong pellets
then enables metallurgical recovery of finely disseminated metallurgical values by
subsequent hydro or pyrometallurgical techniques.
6.2 Procedure
Homogenise the sample, and determine and record its chemistry, size analysis and (when
necessary and possible) the specific surface area.
Where applicable add necessary quantity of binder e.g. Portland cement, lime or bentonite.
For a standard column leaching charge of 25kg, weigh out separately 3 kg for seed ball
preparation. Normally, you would require around 10% of overall charge.
Clean inner surface of balling drum and moisten very lightly. It may be desirable to precoat
inner surface of drum with a thin layer of material being agglomerated.
Start rotation of drum and add small quantities of ore in 50 gram amounts to the drum. With
a water spray bottle, ensure a fine adequate wetting of the ore surface. The precise amount
of water addition will be arrived at after some practice.
When sufficient seed balls have formed empty them onto a nest of sieves such that seed-
balls only in the range 0.45 to 0.55 mm are accumulated. The minus 0.45 mm balls will be
re-fed into the drum, along with fresh fine ore. The object of restricting seed-ball size range
is to ensure a small size spectrum with regard to finished green balls.
Maximise build-up of seed-balls in the above size range. Divide the rest of the charge to be
agglomerated into say 3 batches and equivalently the number of seed-balls.
Introduce seed-balls into the balling drum and allow to cascade in drum. Wet surface lightly
with spray.
Complete ball growth utilising all of the available fines which have occurred by now.
Allow rotation of green balls for a further 90 secs and then spread out prepared balls onto a
plastic sheet for drying.
Set aside samples of green balls for moisture, green compression and dry compression
testing.
7.1 Introduction
In principle it is the simplest of all gravity processes and is a standard laboratory method for
separating minerals of different specific gravity. Fluids of suitable density are used so that
the minerals lighter than the fluid float and those denser sink (as shown in Figure 7a.)
Heavy liquids are used in laboratories on small samples (50g to 10 kg) at specific gravities
ranging from 0.80 to 4.00.
The low S.G. range of liquids are used for coal/ash samples, while most mineral samples are
separated in the range 2.50 to 4.0.
[Suspensions of ground material (known as media – usually magnetite, S.G. 5.1, and/or
ferrosilicon, S.G. 6.8) are used on larger scale laboratory samples and in industrial
applications.]
Sample Preparation
Closely sized samples are required for optimum separation. The ore sample to be tested is
crushed to the required topsize and screened at at appropriate sizes (we and dry screening
is carried out at 38-75 microns if these sizes are to be examined). A typical C.M.S. size
distribution on crushed drill core would be 2440, 850, 300, 106 and 38 microns from a
topsize of 3350 microns.
Warning
The general procedure is as follows. The sample is placed in the liquid of lowest specific
gravity and is split into two fractions. The float fraction is set aside to be weighed and
assayed. The sinks fraction is washed in a suitable solvent, dried and placed in the liquid of
+HDG6DPSOH
ZHLJKHG
6* 6LQN
)ORDWQ
7.3 Results
After assaying the fractions for metal(s) content, the distribution of material and metal in the
density fractions of the sample can be tabulated. Table 1. shows such a tabulation:
As may be seen from the table, a separation at S.G. 2.75 would result in a float product of
68.48% of the weight contain 3.81% of the tin of that size fraction. Laboratory separations in
heavy liquids are “ideal” – all the sinks should report to the sinks and all the floats to the
floats. In industrial applications heavy media is used (rather than the organic heavy liquids)
and inefficiencies in the separation are seen (i.e. sinks misreporting into floats and vice
versa). This is because particles with the same or near S.G. as that of the media have an
equal chance of reporting to either fraction. The efficiency of separation depends on the
ability to separate material of s.G. close to that of the medium. This can be represented by a
Tromp or Partition curve, which relates to the partition coefficient (i.e. the percentage of feed
material of a particular S.G. which reports to the sinks (or floats) product plotted against
S.G.). An example is shown in Figure 7b.
,GHDO
3$57,7,21&2()),&,(17
5($/
% $
6*
Ep = A-B
2
As can be seen the lower the Ep the more idealised is the separation. An ideal separation
has an Ep of 0.0, while most practical Ep’s are in the range 0.02-0.08. (Full details of the
construction of Tromp curves are given in Wills (1) pgs 267-274).
Heavy liquid data can also be interpreted by washability curves. To plot these curves, the
axes shown on Fig. 7c are used.
Figure 7c
% Assay
0 100
Cum.% Cum.%
Wt. To Wt. To
Floats Sinks
100 S.G. 0
SG
If the material consists of two minerals completely liberated from each other, the curve will be
a stepped line. The width of the step indicates the S.G. difference between the minerals and
Figure 7d
Figure 7d(i) shows the curves obtained for completely liberated (solid line) and almost
liberated (broken line) material.
Figure 7d(ii) shows the curves obtained for completely unliberated (solid line) and very poorly
liberated (broken line) material.
S.G. values lower and higher than the theoretical minimum and maximum will often be
otained due to the presence of closed pores and the inclusion of heavier minerals in the
material.
The S.G. curve should not be used alone to indicate the ease or difficulty of separation
because the width of the step depends on both the liberation of and the S.G. difference
between the minerals. The curve is also difficult to interpret when a mineral with two S.G.
phases is present.
The cumulative % assay of the floats or sinks is plotted against the cumulative % weight of
the floats or sinks.
Figure 7e
These curves indicate cumulative assay that the cumulative floats or sinks will have at a
particular S.G. of separation. They are used in conjunction with the S.G. curve and can thus
predict the weights and assays of the two products of separation at any S.G. Conversely the
S.G. of separation can be found for a desired of concentrate or tails.
At an S.G. lower than that of the lightest mineral, all the material sinks. Therefore at 100%
inks, the cumulative % assay of the sinks will equal the head assay. As the cumulative
weight of sinks tends to zero, their assay will tend to that of the richest particle which, if any
of the particles are completely liberated, will equal the assay of the heavy mineral.
At an S.G. greater than that of the densest component, the assay of the cumulative floats will
equal the head assay. As the weight of the floats tends to zero, the cumulative assay will
tend to the lowest possible assay unless the valuable component is present in both low and
The incremental assays obtained for each S.G. are plotted against the average cumulative %
weight of sinks and floats.
Figure 7f
This curve shows the assay of the richest particles in a float or sink. If it is used in
conjunction with the cumulative assay of floats or sinks curve, it indicates the spread of
assay values obtained in a given product.
A material that contains equal amounts of all possible grades of particle will be shown by a
straight line joining the maximum assay at zero sinks to the minimum assay at zero floats.
If the feed material is completely homogeneous, that is with no mineral liberation at all, the
minimum and maximum assays will tend to the head assay and the characteristic Assay
curve will be a vertical line at the head assay.
- Clear inflexion points with a wide flat mid-section indicates the absence of middlings
with the possibility of easy clean separation.
The three types of curve described so far completely define the behaviour of the material in a
heavy liquid under ideal sink-float conditions.
In practice, we wish to use the data to predict the performance of a commercial process such
as D.M.S., Jigs, Tables, etc. In these processes, the S.G. of separation will vary between
certain limits about a mean S.G. due to fluctuations in operation conditions.
The accuracy of the split , in terms of the mean and characteristic assays of the products, will
depend on the weight of material sinking or floating when the separating S.G. is varied about
its mean value during separation.
To enable this to be read off the curves directly, it is usual to plot the S.G. Distribution curve.
This is related to the slope of the S.G. curve and is calculated simply by finding the difference
in the cumulative % weight floating or sinking between the stated tolerance limits for each
mean separating S.G. These differences are plotted on the cumulative % weight of sinks or
float ordinates against mean S.G.
For coal, a table has been built up by experience to give the ease of separation for given
weight percentages or material sinking within ± 0.10 of the mean S.G. of separation.
Figure 7g
± 0.1
Tolerance
Curve
Cum % Cum %
Wt Floats Wt Floats
S.G.
S.G.
Where large samples (both in topsize and weight) have to be examined it is not practical to
use heavy liquids (being both expensive and time consuming). A laboratory heavy media
separator may be used which simulates the action of a heavy liquid bath. Figure 7h
schematically shows an Ericsson cone separator. Sized fractions of particles in the range of
6-50 mm.
Figure 7h
The media passes up through cone A and overflows into cone B. Baskets are filled into the
cylindrical sections of the cones and the feed put into cone A. The floats are carried up and
over into the basket in cone B while the sinks remain in the basket in cone A. A similar
analysis to the laboratory heavy liquid analysis is performed, at several media S.G.’s and
particle size ranges.
8.1 Introduction
Magnetic separation is a process used to separate materials from those that are less or non-
magnetic. All materials have a response when placed in a magnetic field, although with
most, the effect is too slight to be detected. The few materials that are strongly affected
(magnetised) by magnetic fields are known as “Ferromagnetics”, those lesser (though
noticeably) affected are known as “Paramagnetics”.
Ferromagnetics require relatively weak magnetic fields to be attracted and devices to sperate
these materials usually have magnets that are permanently magnetised (“Permanent”
magnets do not require electricity to maintain their magnetic fields). Paramagnetics require
stronger magnetic fields and these can only be achieved and maintained by “electro”
magnets (large wire coils around an iron frame – current is continuously passed through the
coils creating the magnetic field within the iron. The field is concentrated across an air gap in
the circuit).
Both ferromagnetic (low intensity) and paramagnetic (high intensity) separation devices may
be operated with dry solids or with solids in pulp form. (A complete classification of magnetic
separating devices is given in Wills “Mineral Processing Technology”, pp. 338-356).
a) The removal of tramp iron (which would deleteriously affect subsequent processes) from
an ore stream. This is usually achieved by a low intensity magnet suspended above, or
at the head of, a conveyor.
b) Separation of magnetic minerals from less magnetic minerals Table 8.1 shows the more
common magnetic minerals and the range of field intensities that may be required to
separate them.
The extremes of field strength used are based on experience from a magnetic separation
testing laboratory over many years.
As can be seen from the table, minerals from different deposits may have varying magnetic
properties.
The laboratory separator is a high intensity dry device which uses a rotating iron disc to
concentrate the magnetic field and remove the magnetic particles from the non-magnetic.
The separator is shown in Figure 8a. It essentially consists of an electromagnet (the applied
current is controlled by a rheostat) which produces a magnetic field across the airgap and a
belt which passes through the air gap. Mineral particles are fed from a vibrating feed onto
the belt and through the magnetic field. The magnetic particles are attracted to the disc
above the belt and from there are removed from the field by the disc above the belt and from
there are removed from the field by the disc’s rotation – they fall from the disc and are
collected at the side of the belt. The non-magnetic particles are collected at the end of the
belt.
a) The machine should be thoroughly cleaned with compressed air, and the product
collection trays placed in position.
b) The sample to be tested should be closely sized (e.g. 425-300 microns, 75-45 microns)
and Ferromagnetic particles removed prior to separation (a hand magnet inside a plastic
bag may be used for this).
d) The air gap between the disc and the belt should be set to approximately treble that of
the largest particle in the sample (NOTE: The air gap cannot be adjusted when the
current is on).
e) Press the mains “START” button and turn on the three switches (feeder, magnet and
belt disc drive).
g) Slowly start the vibrating feeder and adjust such that a single layer of particles is
distributed over the belt (periodic adjustment may be necessary).
h) Once optimum separation is achieved, switch off the feeder, recombine the products in
the feed hopper and commence separation.
i) When the sample has run through, collect, weigh, label and bag the products.
k) Reduce current to zero, turn off all switches, clean the machine thoroughly
9 INTRODUCTION
Separation of minerals utilizing differences in their electrical properties may be carried out
using an electrostatic separator. It will separate electrical conductors (minerals such as
cassiterite and rutile) from those that are electrical non-conductors (minerals such as zircon
and siderite). The principle of separation is that as the particles to be treated are passed
through an intense electric field each particle acquires a charge. The conductors pass on
their charge when emerging from the field while the non-conductors retain theirs
momentarily.
Separation is effected by passing the particles on to a rotating metal cylinder (the roll);
without any external forces all the particles will follow a ballistics trajectory when leaving the
roll surface, as shown in figure 9a.
Laboratory machine
Procedure
x Sample Preparation
Particles to be closely sized as in magnetic separation.
x Safety
The normal operating voltage of the machine is 30,000 volts (D.C.); consequently strict
adherence to the safety procedure as indicated below is imperative.
a) vibrating feeder
b) high tension volts (gradually reduce to zero)
c) high tension switch (light off)
d) filament (use key)
e) infra-red lamp
f) rotor
g) power supply
n.b. clean machine thoroughly
Additional Bibliography
1. Readings 270 mm High Tention Separator Manual
2. Wills, B.A. “Mineral Processing Technology”, 1979 (and late editions)
3. MacDonald, E.A. “Manual of Beach Mining Practice”, 1973
4. http://www.carpco.com
PART 1 SUPERPANNER
10.1 Purpose
10.2 Principle
To simulate gravity performance of a given sample. Recovery and grade achieved are
normally higher than in plant operation, but analyses of grade/recovery curves permits
relative assessment of performance.
10.3 Equipment
The superpanner itself is a completely integrated machine which only needs suction lines to
draw off concentrate tailings. The superpanner can simulate the hard knocking action of a
shaking table or the gentle washing of a panner.
Micron
- 600 +212
-212 +106
-106 +75
-75 +38
-38 +12
10.5 Procedure
A 50 gram maximum of sample is recommended for the U-shaped deck of the superpanner.
The superpanner itself has the ability to rock sideways and tilt in the horizontal. The knock
that is applied to the end of the deck is like all other motions in that the degree of motion
needed can be varied. The speed of the motion sideways and the interval of the knock can
also be controlled. It is very important that water additions throughout the separation are
such that the solids are kept in solution and that dry beds do not appear, thus hindering
separation. Normally the deck starts in the horizontal with a hard fast knock and no side
motion. It is hoped by this arrangement that the heavy mineral will fall through the sample
onto the bottom of the deck (much like a jig).
After a period of time the knock is taken off and the deck angled towards the tail pipe and a
gentle sideways motion is applied to remove the gangue from the top of the heavy mineral.
Once the heavy mineral is separated from the remainder of the sample it can collected into
the concentrate holding bottle by means of the vacuum system. Tailing are normally taken
off throughout the separation and re-superpanned several times. This enables production of
a rougher concentrate with the final tail free of liberated cassiterite. The rougher concentrate
can then be put back on the deck and a super concentrate of the highest possible grade
removed (minimum weight – approxiametly 0.2g). Subsequently the remaining rougher
concentrate may be re-superpanned and spread out along the deck of the superpanner
where it can be split into three separate concentrates depending on S.G. (that is the
proximity to the concentrate end of the deck). In the finer fractions it should be possible to
attain the liberation size of the heavy mineral and recovery should hence be high. In the
coarser fractions, however, high recovery is not always obtained because of unliberated
cassiterite.
Note: High recovery and grade can only be achieved if the heavy mineral is liberated. The
ability to quickly visually identify the heavy mineral and considerable operator patience are
important attributes for high recovery.
The separator enables release analysis of mineral grains of close specific gravity in the size
range below 2 mm and can give additional data to heavy liquid results in the higher S.G.
ranges.
It consists of a V profile stainless steel tray with a 1o to 3o slope, which can be made to
oscillate with a horizontal amplitude of adjustable from 2 to 4 inces and a longitudinal
amplitude of ¼ “. An adjustable end knock action ;is also provided.
An irrigation pipe is attached to the tray’s perimeter and a concentrate wash water pipe is
situated centrally at the feed end of the tray.
Adjustments are provided for leveling, slope setting and a control panel houses a switch
timer, water valves and rotameter.
The separator also has an interchangeable stainless steel tray which is flat and which can be
used to predict slime table performance on ultra-fine materials.
After the wetted sample has been added to the tray the cyclic motion stabilizes the mineral
particles and stratification takes place. Heavy (usually valuable) mineral sinks to the tray
surface and is moved “upstream” by the end knock action, “whereas the lighter (gangue) is
carried downstream by the flow of the irrigation water to discharge via a tailings launder.
Once established, test run parameters should not be varied for reproductibility to allow
comparisons to be made between samples.
11 LEACHING
x Diffusion of solvent through the pores in the solid particles, and of the
dissolved substance outwards after solution.
x Chemical solution at the reaction site in the particle.
x Transport of the dissolved substance in the solvent away from the particle
surface.
Factors controlling the rates of the above steps are temperature, agitation, concentration of
leachant, particle size, leaching time and pH.
1) Naturally occurring metals in the native state, e.g. Au, Ag, Platinum metals, Cu.
2) Produced as a by-product of a metallurgical process, e.g. Au, Ag, Pt, Se.
3) Produced by metal oxide reduction, e.g. Cu and Ni.
For Gold and Silver, the most common leachants used are Na or K cyanides in the presence
of oxygen, Thiourea (NH2. CS.NH2), also in the presence of oxygen, or Ammonium
B B B B
levels in solution.
b) Formation of complex cyanides, eg. Cu, Zn and iron minerals may dissolve
preferentially in cyanide solution, thereby depleting the solution of its
cyanide content.
c) Formation of thiocyanate: the sulphide ion liberated when the sulphide
mineral reacts with cyanide and oxygen forms a thiocyanate which has no
action on Au.
d) Adsorption on gangue mineral: Gold ores containing aluminosilicates or
other silicates when finely divided in an aqueous alkaline medium often
form colloidal Silica and Alumina to which ferric hydroxides with a strong
adsorptive capacity for sodium cyanide get attached.
e) Film formation on the surface of the metal
x As a consequence of build-up of a thin layer of sulphide ions
x Formation of a layer of calcium peroxide at pH > 11.5 or
x Films of insoluble cyanide, e.g. Pb(CN)2 or of flotation reagent like
B B
The effects of retardants can be ameliorated somewhat by addition of Lead salts like lead
oxide, nitrate or acetate which, as insoluble lead salts, eliminate the sulphide ions as soon as
they are formed. Additions of small amounts of Potassium permanganate also help eliminate
difficulties due to sulphides by apparently oxidizing the sulphide ion to sulphate. Additionally,
agitating the ore pulp in an alkaline medium helps decompose sulphide minerals, after which
the solution is discarded. The sulphide-free pulp is then subjected to cyanidation.
Native Copper and Nickel containing ores are generally leached in aqueous ammonia
solutions, important parameters being ammonium ion concentration and Oxygen partial
pressure.
a) Cassiterite
a) Acid leaching:
Dilute acids dissolve some metal sulphides with liberation of H2S, e.g. B B
b) Alkaili hydroxides:
NaOH may be used to leach PbS and ZnS forming soluble plumbite
(Na2Pb02) and zincate solutions respectively (Na2Pb02) respectively.
B B B B B B B B
c) Alkali sulphides:
Sodium sulphide solution reacts with sulphides of arsenic, antimony, tin and
mercury to form soluble thiosalts, additions of NaOH helping prevent
hydrolysis of Na2S. B B
d) Alkali cyanides
Sodium cyanide has a solvent action on sulphides.
e) Double decomposition
Copper sulphate can be used to separate Copper from Nickel in a sulphide
ore or Copper from Fe in Cu –Fe sulphide ore. CuSO4 solution can also be B B
used for removing Pb, Zn, and Fe from copper sulphide ores.
a) Ferric ion:
Ferric sulphate or chloride react with metal sulphides liberating elemental
sulphur, e.g.
Zns + 2Fe3+ ĺ Zn2 + 2Fe2+ + S P P P P P P
During leaching with Ferric ion a critical balance between Fe2+ and Fe3+ ions P P P P
The technique can be used for Lead (PbS), copper (Cu2S and CuS), Iron B B
The oxidizing action of nitric acid and nitrates can be utilized to leach
sulphides, but this is seldom adopted because of costs.
Most sulphides are oxidized to sulphate. From the sulphated ore, all of the
zince, copper and iron can be leached with water while lead, silver, gold
and antimony will remain in the insoluble residue.
11.2.1.2. Procedures
1) Dry the ore and crush it to minus 2380 pm (or as specified, otherwise).
2) Prepare the solution of required concentration (e.g. 1M H2SO4 requires 52 ml of
B B B B
3) Place 50 gm sample in the leach bottle and add 250 cc of prepared solution.
4) Allow leaching to take place for 1 hour under stirred conditions, ensuring the
right conditions of pH, temperature, % solids, etc.
11.2.1.3 Precautions
1) 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.
2) Residues should be thoroughly washed of leaching reagents.
11.2.1.4 Calculations
x100
B
2) Grind to pass 200 microns ( Ҕ13-15 minutes for hard rock ores; Ҕ 10 minutes for oxidized
ore) grind at 35% solids.
3) Wet screen. Retain and dry fractions. Settling overnight of – 45µ will be required.
Decant and dry. Perform cyclosiing on – 45µ fraction. Ensure to include – 45µ material
dry screened from remaining size fractions. (20 minutes on Ro-tap screen shaker).
4) Reconstitute sample – add to bottle along with same weight of 0.1% (1 gram/litre)
NaCN solution, to give 50% solids. Adjust pH to 10.0 – 10.5, with measured lime
additions.
5) Put bottle on rolls (with variable speed setting set at zero – this is sufficient agitation) –
if using two bottles, place caps away from each other, and start timing.
8) Filter pregnant solution from pulp, retaining and labeling the solution. 40-50 mls of
pregnant solution is required.
9) When final sample (72 hours usually) has been taken, the residual cyanide must be
determined. Procedure for this determination is outlined elsewhere.
10) Wash solids with warm water and dry, setting aside for final residue.
Comments:
In lieu of cyanidation by bottle leaching on rolls, it may also be more convenient to bottle
leach using magnetic stirrers with necessary air bubbled using flexible air lines.
1) Agglomerate ore if required. Cure for recommended time period. During this time the
ore should be kept damp via a wet cloth spread over it.
2) Load ore into the column. This should be done with the column on an angle, and the ore
poured gently in to prevent packing. The nylon mesh filter should be placed in position
prior to filling the column.,
3) The column should be placed in position and cyanide solution made to concentration
(usually 0.1% - ie. 1 gm/litre). Allow for 1 container (5 litres) of cyanide per day (plenty).
The flow-rate from the top should be carefully adjusted to give a constant drip
approximately 2 ml/min. Slightly more is acceptable. Periodic checks should be made to
ensure an even flow rate, and also to check if percolation through the bed into the
container below has actually occurred. This percolation time should be noted.
4) After 24 hours, and every 24 hours thereafter, the following procedure should be
followed:
ii. The feed flow rate can be measured by the volume loss incurred in the feed cyanide
bottle. This should be reported as volume flow over an hourly period, say. The
percolation flow rate can be measured by collecting an underflow sample over a 2 or
5) When the test has been run for the appropriate number of days the bed should be
flooded with hot water and left to percolate through. The ore can be removed and spread
upon sheet plastic to dry.
6) Once a day, the sample should be riffled down to several kg size, crushed and riffled
down further to produce a sample for assay.
Note:
1. The endpoint is indicated by the first sign of a change from clear to slightly turbid
conditions. A black background helps to perceive this transformation, and a comparison
with a sample at equivalence point is also useful. If solution is already slightly turbid, a
greed tinge will be noted at equivalence point.
2. Reagent Preparation:
a) Bulk flotation
b) Differential flotation
While all flotation processes are selective or differential in that one mineral or group of
minerals is floated away from accompanying gangue, bulk flotation generally refers to
separation of unlike mineral types such as sulfides from non-sulfides. Differential flotation
(exemplified, for instance, by the concentration and subsequent successive removal of Cu,
Pb, Zn and Fe sulfides from a single ore) on the other hand, is restricted to operations
involving separation of similar mineral types.
Froth flotation is a means of treating a pulp of finely ground ore so that it yields the valuable
or desired mineral in a concentrate that will be amenable to further processing. The process
involves the imparting of a water repellent (hydrophobic) character to the wanted mineral
particles by chemicals that are called collectors or promoters. Under favorable conditions,
these chemically coated particles become attached to the air that is bubbled through the
pulp, and will thus “float” on the surface.
If the surface tension of the pulp is then reduced by a second chemical, called a frother, a
stabilized froth containing the wanted mineral particles will form on the surface of the pulp.
This froth can then be skimmed off to yield a concentrate in which the desired mineral is
present in a much higher percentage than in the original ore.
The test objectives and therefore information required from the results should be established
(e.g. sizings, assays, rates of flotation and treatment of products, etc). Knowing the
information that is required, the test can be planned with regard to the following:
12.2.1.2 Reagents
All reagents to be used during the test should be prepared at the required strengths prior to
commencement. The freshness of some reagents is important. Remember the more dilute
the reagent, the more accurate is the addition rate but the higher the volume addition to the
cell.
All equipment should be thoroughly cleaned prior to the test (and after completion of the
test), and all product trays and reagent dispensers properly labeled.
It is sometimes helpful to gain information from previous tests of a similar type or performed
on the same feed source, to become aware of any problems which may occur during the test
(e.g. amount and nature of sulphides, feed size distribution, frothing problems, etc.)
12.3.1.1 Reagents
a) Collector
The collector is a most important reagent as it determines froth grade and recovery. The
optimum addition is controlled by several factors; ore type, head grade, product grade
and recovery. The collectors used in cassiterite floation often have an effect on the froth
properties. Excessive collector additions can give froth properties. Excessive collector
additions can give froth stability problems (bubbles too stable) and hence selectivity
problems. The types of collectors used in the flotation of cassiterite are varied. A
number of factors control the choice of collectors used. The following is a list of some of
the collectors which are available:
OH
2. Sulfosuccinamates
e.g. S3903 – Cyanamid CH2 - COONa
CA540 – Allied colloids
CH COONa
R- N
C SO3Na
CH2 - CH
COONa
b) Frothers
A frother should be used with extra caution in oxide flotation as excessive amounts of
frother will alter the froth composition, increasing the recovery of water and hence
increase the recovery of the gangue minerals. The choice of frother for cassiterite
flotation as recently become an important variable as the effects of various frother and
concentrations have been investigated. The frother MIBC has historically been the
frother used but recent limitations with this reagent have led to the use of alternatives
such as Aerofroth 65, Senfroth 41G and Dowfroth 250.
The reagent sodium silico fluoride (Na2SiF6) is the most commonly used depressant in
B B B B
cassiterite flotation, acting both as a slime dispersant and also reducing the floatability of
certain minerals, especially fluorite, tourmaline and other silicates. It is also thought to
activate cassiterite in some circumstances. This reagent is added prior to the collector
addition, but further additions in the cleaning stages can be of benefit. The rate of
addition varies depending on the ore source, but 0.3-0.4 kg/tonne of feed is a good
starting point.
d) Modifiers (Acid)
e)
It is necessary for the pH of the flotation pulp to be at the correct value and held relatively
constant, for maximum selectivity and recovery.
Cassiterite flotation is nearly always performed in an acid environment, the exact value
depending on the ore source and collector to be used. Sulphuric acid is used for pH
adjustment in most cases. Changes in pH can cause changes to the froth. A reduction
in pH will give better selectivity but usually at a lower recovery. If the pH is increased the
opposite will occur as persistent froths are formed.
Alkali (NaOH)
The addition of NaOH is sometimes used to increase the pH in the cleaning stages. The
higher pH helps in dispersing slime and improving the % Sn grade.
Readers are also referred to mining chemicals handbook, revised edition Cytec 2002.
The nominal size range for cassiterite flotation is between 2 and 100 microns. The top size
is variable depending upon the liberation of the cassiterite particles. Cassiterite grains
coarser than 100 microns are difficult to float whilst grains finer than 2 microns give
selectivity problems. Hence the feed for cassiterite flotation should be reduced to 95% minus
100 microns and then deslimed at 2 microns to give a feed containing no more than 8%
minus 2 microns. Information on techniques to achieve this feed size is given in page 34.
When a number of tests are to be performed, a bulk sample of flotation feed is placed in a
well agitated vessel (cyclone rig) at the required density for flotation and the required volume
It is important to have adequate sample for the number of tests required and to maintain the
same sample quality, which will deteriorate with time.
12.3.2.1 Introduction
Scheelite (CaWO4) and Wolframite ((Fe,Mn)WO4) are the principal minerals of tungsten, but
other important minerals include ferberite (FeWO4) and huebnerite (MnWO4). The high
specific gravity of these minerals makes many of these ores amenable to gravity
concentration methods, however, the fine dissemination of mineral in gangue for some ores
may require finer grinding and recovery of mineral by flotation at finer sizes.
Wolframite exhibits very similar flotation properties to that of cassiterite; hence it is floated in
an acid medium using sulphosuccinimates (Cyanamid S3903 or Allied Colloids CA 540) or
styrene phosphonic acid (SPA), and is floated as cassiterite.
1) General practice for flotation of scheelite is in alkali circuit using either soda ash or lime
for pH control.
2) Plant practice at King Island scheelite involves conditioning of feed pulp to 10.2 pH using
NaCO3 and floating a scheelite concentrate using oleic acid emulsified with akypomine.
Rayflo-C, a wood derivative is used to control calcite and sodium silicate is used as a
gangue dispersant. This produces a 15-20% WO3 concentrate which is then leached to
produce an artificial scheelite product assaying 75% WO3.
3) The Tempiute process is one approach used for the flotation of scheelite from ores
having appreciable quantities of calcareous and siliceous gangue minerals. The process
basically consists of conditioning the ore with lime, followed by soda ash and sodium
silicate as modifiers. Scheelite is then floated using a mixture of oleic and naphthenic
acids as collectors. The addition of lime is not only useful for pH control but apparently
aids in selectivity over gangue minerals. 50-56% WO3 concentrate grades have been
reported to 95% recovery.
Sulphide minerals possess excellent flotation properties; hence the prime importance of
flotation as a concentration technique for sulphides.
a) Collectors for sulphide minerals : Anionic collectors are most commonly used for
sulphide minerals. By reference to the table (below) it will be note that they are all
structurally similar, each having a single sulphur atom double bonded to either a carbon
or phrosphorus atom, hence all of the sulphide minerals can be floated with varying
success by any of the sulfydric collectors.
S
Thionocarbamates ||
RHN-C-0R1
S
Dithiophosphates RO ||
P SNa
RO
S
Thionocarbanilide ||
H5C6 - HN-C-NHC6H5
S O
Xanthogen Formate || ||
ROC - S - COR
a. pH
e.g. Lime (CaO), Soda Ash (Na2CO3), B B B B
Since almost all sulphide flotation circuits operate with an alkaline pulp for optimum
metallurgy and the prevention of metallic corrosion, lime or soda ash for alkalimity
regulation are employed. Where the ore is very acid and lime difficult to obtain or
where the minerals are floated from acid leached pulp, acid pH control is usually
obtained with dilute H2SO4. B B B B
Examples of re-surfacing agents are the use of CuSO4 in the flotation of sphalerite B B
depressants for Cu, Fe and Co sulphides in lime alkaline pulps; reducing agents like
sodium sulphite (Na2SO3), or sodium bisulphate (NaHSO3) to prevent excessive
B B B B B B
ii. Copper Zinc ores, typically combinations of some or all of the following:
Chalcocite Cu2S
Chalcopyrite CuFeS2
Sphalerite ZnS
Pyrite FeS2
Pyrrhotite FeS
Lead and copper minerals are usually separated into a join lead-
copper concentrate.
IV (i) copper-Nickel
Feed Preparation:
Prepare a 3 kg charge from the weekly Que River ore sample. This sample has been roll
crushed to 80% - 1mm.
Grinding:
Using the 1 kg mill, grind the feed in three separate batches. The grinding time for each
batch is 14 minutes using 75% solids and 5 ml of 5% Na2S2O5 (0.25 kg/t).
Screen the mill product with a 106 micron screen and reject the oversize.
Cu Flotation:
Using the 5.2 litre Agitair flotation cell make the flotation feed up to 45% solids with the –106
micron fraction.
Conditioning:
Add Na2CO3 (10%) if the pulp pH falls below 6.0 and condition for five minutes.
Aeration:
Add 1 ml of 5% sodium aerofloat collector (0.017 kg/t) and aerate for two minutes. Again,
add Na2CO3 if the pH falls below 6.0.
Rougher Float:
Add 0.05 ml of cresylic acid frother (0.0167 kg/t) and float for approximately six minutes.
Record the wet rougher weight, label the pan and dry.
Pb Flotation:
Conditioning: Bring the pulp level up to the 5.2 litre mark by adding water. Record the
volume of water added. Add 5 ml of 5% Zinc Cyanide depressant (0.083 kg/t) and increase
the cell pH to 9.2 by adding Na2CO3. Condition for five minutes.
Pb Scavenger: Bring the pulp level up to the 5.2 litre mark, recording the volume of water
added and adjust the pH to 9.2 if necessary. Add 0.4 ml of Sodium Isopropyl Xanthate
together with 0.02 ml of cresylic acid and float for a further 5-6 minutes. Record the wet
scavenger weight, label the pan and dry.
Zn Flotation
Conditioning: Bring the pulp level up to the 5.2 litre mark, recording the volume of water
added. Add 30 ml of 5% CuSO4 (0.5 kg/t) and bring the pulp pH up to 10.0 using a 5% lime
solution. Record the volume of lime added. 1.5 ml of 5% Sodium Aerofloat collector (0.025
kg/t) should also be added and the pulp conditioned for a period of six minutes.
Zn Rougher: Add 0.02 ml of Dowfroth 250 (0.007 kg/t) and float for 15 minutes. Record the
wet rougher weight, label the pan and dry.
Zn Scavenger: Bring the pulp level up to the 5.2 litre mark, recording the volume of water
added. Using lime adjust the pulp pH to 10 if necessary. Add 0.2 ml of Sodium Aeroflaot
together with 0.02 ml of Dowfroth 250 and float till the froth is barren. This should take
approximately eight minutes.
Flotation Tail
Preparation of Assay
Cut out a minimum of 20 g from each of these productions for XRF analysis at the Cleveland
laboratory.
All test results and assays should be recorded in the Que River log book.
1) - Fill the flotation cell to the predetermined level and position the pH probe. The
calibration of the pH meter should be checked. Note. The level of the pulp will
change when agitation is commenced and air introduced to the cell.
3) Oxide Flotation
- Adjust pH to required value with H2SO4 / NaOH solutions and maintain
throughout. The pH value varies with the collector used.
- Add depressant (usually sodium silico fluoride) and condition for 5 minutes.
- Add collector and condition for 10 minutes
- Add frother as required and introduce air to produce bubbles.
- Remove the froth consistently and at a fixed depth.
- Collect concentrates at predetermined times.
- Add further collector and continue flotation if required.
- Vanning of concentrate and tails gives an idea of the performance.
A complete record of the entire procedure used from sample preparation to treatment of
products must be maintained. Included in this should be all reagent additions (and solution
strengths), conditioning times and pH. A standard log sheet is available for this purpose.
1. Flotation Mechanisms:
There are two main mechanisms by which a mineral can be recovered into the froth. The
first is a “true” flotation mechanism, where the mineral surface becomes hydrophobic,
due to absorption of collector ions, attaches itself to an air bubble, and rises to the
It is important to accurately know the pulp density for the flotation test to achieve both
optimum flotation performance and the correct reagent additions. The pulp density can
be obtained by using Marcy density scales, or simply weighing a certain volume of pulp,
wet and dry. From the pulp density, the amount of dry solids in the cell can be
calculated.
If one wished to alter the pulp density in the cell, it is a simple calculation to determine the
amount of water to be added or taken from the cell to achieve the new density required.
The exact addition of reagents is very important as the effect of reagents on the overall
results has previously been shown to be critical., Knowing the amount of dry solids (in
gms) in the flotation cell and the strength of the prepared reagents, the addition of
reagent can be calculated.
e.g. if cell contains 1.2 kgs of dry solids and an addition rate of 0.3 kg/tonne is
required and the reagent has been prepared to a 5% solution (i.e. 5 g of dry reagent,
made up of 100 mls of solution).
Following the completion of the test it will be found that the total dry weight of all
products is different from the earlier estimation. One should then recalculate reagent
additions using the exact dry weight figure, to find the exact addition rate of each
reagent.
Sampling is the means whereby a small amount of material is taken from the main bulk in
such a manner that it is representative of that larger amount.
Sampling is dependent on probability; the sampling method devised by Gy being most often
used to calculate the size of sample necessary to give the required degree of accuracy. This
method take into account the particle size of the material, the content and degree of
liberation of the minerals, and the particle shape.
S2 P P
And s is the measure of the statistical error or the error committed by sampling,
ie. The standard deviation of a normal distribution curve representing the
random assay-frequency data for a large number of samples taken from
the ore.
The sampling constant C is specific to the material being sampled, taking into account the
mineral content, and its degree of liberation.
C = fxgxƐxm
Where f is a shape factor (0.5 normally except for gold ores, where it is 0.2)
g is a particle distribution factor, usually 0.25, unless the material is closely
sized, in which case a factor of 0.5 is used; and Ɛ is a liberation factor (0
for completely homogeneous material and 1.0 for completely
heterogeneous material).
Gy devised a table (shown below) based on d, the dimension of the largest pieces in the ore
to be sampled, which can be taken as the screen aperture which passes 90-95% of the
material, and L, the size in cm at which, for practical purposes, the mineral is essentially
liberated. This can be estimated microscopically. Values of Ɛ correspond to the values of
Top Size/Liberation Size, i.e. d/L, and can be estimated from the table:
m= 1 – a x [(1 – a) r + at]
U U
where r and t are the mean densities of the valuable mineral and gangue
minerals respectively, and
a is the fractional average mineral content of the material being sampled.
Gy’s equation assumes that samples are taken at random, and without bias, and is most
applicable to streams of ore transported on conveyors or in pulp streams rather than heap
deposits which are inaccessible to the sampler.
The equation gives the minimum theoretical weight of sample which must be taken.
Example: Consider a lead ore, assaying about 5% Pb, which must be routinely sampled for
assay to a confidence level of ± 0.1%. Pb 95 times out of 100. The galena is essentially
liberated from the quartz gangue as a particle size of 150 microns.
If sampling is undertaken during crushing, when the Pb size of the ore is 25mm, then
d = 2.5 cm
2s = 0.1
U U = 0.02. Therefore s = 0.01
5
d = 2.5 =
U U U U 167, therefore from the table, Ɛ = 0.05
L 0.015
Assuming the galena is stochiometrically PbS, then the ore is composed of 5.8%
PbS.
Cd3 = 114 kg
M = U UP UP
s2 P P
In practice, therefore, about 300 kg of ore would have to be sampled in order to give the
required degree of confidence.
If, however, the sampling takes place from the pulp stream after grinding to the liberation size
of the ore, then d = 0.015 cm, and assuming that classification has given fairly close sizing,
Therefore M = 0.8 g.
Such a small weight of sample would, however, not be cut from a pulp stream as it ;makes
no provision for segregation within the stream, variations in assay and particle size et. With
time however, it could be a guide for the increment to be cut at each passage of the cutter,
the interval between cuts being decided from the fluctuations in the quality of the pulp
stream.
Readers are also referred to Sampling of Particulate Materials, Theory and Practice, Pierre
M Gy. Elsevier.