 Introduction:

o Process Mineralogy:
Process Mineralogy is the practical application of mineralogical knowledge. Mineral exploration,
optimizing processes, analyzing complex ore bodies.
o Advanced Characterization Techniques;
1. Scanning Electron Microscope
2. X-ray diffractometer (XRD)
3. X-ray Fluorescence (XRF)
4. Electron probe micro-analysis (EPMA)
5. Secondary ion mass spectrometer (SIMS),
6. Infra-red analysis (IRA), Raman Spectroscopy
7. Image Analysis System
o Analytical Chemistry: Chemical Analysis
 Qualitative:
 Quantitative
a. Gravimetric: weight of precipitate left
b. Volumetric volume of precipitate left or increase
c. Absorption Photometry:
Lambert-Beer law states absorbance is proportional to concentration.

o Mineral Characterization: [ ICQ-PLC]

 Identities of major, minor and trace minerals,
 Compositions of minerals that bear on the process,
 Quantities of minerals,
 Particle size distributions, textures of the minerals
 Liberations analysis
 Surface coatings on mineral
o Unique Physical Properties of minerals:
 Fluorescence
 Acid Response
 Magnetism
 Radioactivity
o Types of Signals in SEM:
 Elastic Scattering: BSE , electron diffraction
 Inelastic scattering: SE , augar electron, ….. xray
o Problems in Analysis:
 Cost of databases access
 Non representative sample
 Calibration
 Inadequate training
o Questions:
 What particles etc can you detect when irradiating a sample with an electron beam?
Emits SE, BSE, X-ray, Auger, etc can be detected.
 What information do you mainly obtain by SEM?
Size, morphology, coating, chemical composition (by EDS atomic number)
 How can you monitor insects or other non-conductive materials in SEM?
 For insects:----“critical point drying” to displace the water and evaporate the fluid in a controlled
way that won’t collapse the fine biological structures such as cell walls.
Create a connection to the ground using metallic tape and image your sample in the nearby area;
Sputter coat your sample with gold or other conductive coating materials; Operate at a lower
vacuum level.
 What effect is responsible for generation of X-Rays by electron beams?
Characteristic x-rays are produced by the primary electron beam displacement of an electron in
the valence shell of the specimen. As the electron is displaced, an electron from a higher valence
shell must fill its orbit. The result is a small amount of energy loss in the form of an x-ray photon.

 What kind of information can you obtain by EDX?

Chemical composition
Chemical mapping
Image analysis
 Is it possible to do chemical mapping with EDX?
Yes 2D resulotion chemical mapping

o

 Process Analytical Technology: (PAT)

Monitoring, analyzing and optimization of the process using in situ and online analytical tools. E.g. thermocouple,
sensors, etc.
o Advantages:
 Process Optimization
 Process Control, Risk management,
 Scale up
o
 Particle Size Reduction:
Equivalent volume of particle expressed in micron or mm. Size reduction is crushing particle to have a consistent
PSD ( particle size distribution)
o Different Sizes:
 Crushing: 0-4 mesh
 Grinding: 5 -25 mesh
 Pulverizing: 25 mesh and beyond.
o Fineness modulus:
Measure aggregate quality. F.M. = (total cumulative % weight retained) / 100
o Mesh:
Number of holes per square inch.
o Mean Size:
Either linear diameter (linear intercept measurement) is measured OR area is measured and considered as
diameter (size of the particle)… Means can be weighted by number, surface area or volume. The volume-
based mass moment mean popular in light scattering devices.
1. Dcircle : placing circle on the particle and measuring its diameter
2. Dsquare: placing square…..
3. Dmean: diameter of 16 samples are measured and taking its mean
4. Dmax: diameter of 16 samples are measured and taking maximum of it.

Diameter:
If a single number is desired to represent a particle’s size, it will be diameter; however it is often unclear
where to make this measurement and several options have been formalised over the years:-
1. Equivalent sphere diameter:
If the particle is considered sphere, so deriving its diameter from sphere volume formula or sphere
surface area formula. Utilized in Coulter Counter Equipment.

2. Equivalent Disc Diameter:

The projected area (A) of a particle, can be expressed as the diameter of a disc with equivalent
projection area. Utilized in image analysis.

3. Derived Diameter:
a. Feret Diamter:
Particle is rotated 8 or 16 times then taken max height and width.

b. Maximum inscribed disc diameter:

The Maximum Inscribed Disc Diameter (dIN) is the diameter of the largest disc that fits
entirely within the particle.
 c. Martin Diameter:
Martin’s diameter is the length of any chord that divides the projected areas into equal
halves. It is also rotated 8,16 times than taken max, min.

d. Hydro-dynamic diameter:
From drag force formula (stoke law). Should be dispersed, note less than 1 micron, and
consistent density particles.

o Taking representative Sample for analysis:

According to end use, if suspension then taking sample in suspension form means dispersed in
suspension. Sampling is done by splitting process, dry by cone-quarter technique (modern riffle splitter)
and wet by rotary splitter.

o PSA (Particle size analysis) :

Procedure to determine the size range or mean size of particle of sample. The following are used:
1. Sieve Analysis
2. Laser Diffraction
3. Light Scattering:
4. Gravity Sedimentation
5. Image Analysis
Sn Technique
1 Sieve The sieve have under root Optimal weight often less than 100g
Analysis 2 sequence.
Finer than 50 microns; wet
screening.
Poor performance below
50 micron and rare less
than 10 micron.

2 Laser Dispersed in liquid, laser Particle size is inversely proportional to the

Diffraction at high intensity and fixed angle , while intensity increase with size.
wavelength, an array of
detectors measures light
intensity at a wide range of
angles, and resulting
spread is put into the
model (Mie & Fraunhofer)
results the size distribution
of the particles.
1 to 1000 micron [than the
wavelengths of visible
light, Brownian motion Limitations:
dominate gravity 1_Overestimation of fine b/c of multiple
downfall] scattering
2_ Non-spherical particles
3_Agglomeration causes non-smooth
distribution.
3 Light Nano-particles Limitations
Scattering 0.3nm to 10 micron Same as laser diffraction
Sample is illuminated by a
laser beam and the
scattered light is recorded
at one detection angle
Movement of the particles
causes intensity
fluctuations in the
scattered light and is
detected to
determine particle size
4 Gravity Settling is movement of This is only valid for a laminar flow regime
Settling particles to the bottom of a : Re < 2000
liquid and form a Limitations:
sediment. Particle 1_Flatness 10 % settles with half the
experience either gravity velocity
or centrifugal motion. 2_Interaction with wall of container
3_
In water , measurable limit for D is 60 µm
5 Image Size , shape and amount. Shape Analysis: Binary images of each
Analaysis By Optical Microscopy. mineral is taken to obtain values for
parameters as area/perimeter, aspect ratio,
Image Acquisition: (static circularity….then binary thining to erode 1
or dynamic) … pixel so to remove grain boundaries
Dynamic: 104 irregularities.
p/min..mechanical
dispersion Delesse Principle: the area occupied by
Static: 105 p/min…vaccum each mineral is the volume of that mineral
dispersion. in the rock. Two requirments:
1_ Section of particle be random (resin)
Static: Steps 2_The particles should have well defined
1_ Sampling boundary
2_Sample >Amsler grid
Preperation…resin...(avoid
preferential plucking, or Delesse 1st Principle :
segregation by vibrating).. (Stereology)..estimating 3D info from 2D
3_Mineralogical sample.
Imaging…SE & BSE We actually need 3D property of material.
4_Image
Segmentation…noise Petrography: thin section rock with
removal algorithim to polarized light microscope.
remove 1 pixel of the
boundary of
mineral….enhance
gradient and contrast.
5_Image Analysis…..
measurements of
geometry, distribution,
spatial variablity
 6_Stereology Statistic

6 Coulter Particles suspended in an The instrument records electronically all Limitations:

Counter… electrolyte forced to pass those particles producing pulse that are 1_ Calibration is required for each
through a calibrated within or between two threshold values of
(aka aperture. the analyizer electrolyte and aperture (threshold)
electrical Each particle induces a 2_ Twin particles same size…+/- at
sensing change in resistance with result
zone) an amplitude proportional 3_Largest
to the particle volume.
10k particle/sec
particles are limited to 40% 60% of
aperture….smallest 2%
7 Ultrasonic Decrease of flux intensity Suitable for online.
Extinction of ultrasound in a 0.01 to 1000 micron.
suspension is particle size
dependent.

 Microscope:
30micron thin section (transparent) or resin matric (opaque).
o Criteria for identification of opaque minerals: (RCB – Paish)
1. Reflectance
2. Colour
3. Bireflectance………...RI change with orientation
4. Pleochroism…………color change with orientation
5. Anisotropism………..Properties changes with orientation e.g. structure and color
6. Internal reflection……internally glows
7. Shape of mineral…….triangular, lamellar, botryoidal
8. Hardness
 Notes:
o Surfometry:
Surfometry is a special case of 2D imaging where the pixel intensity is expressed as an altitude. For
topography as black and white.
o 3D imaging:
It is made out of volume elements (voxels) or by tomography (drawing, if material is transparent e.g by
radiograph)
o Henry Clifton Sorby:
father of microscopical petrography.
o Digitial image:
is made of picture elements (pixels;)which has spatial coordinates (x,y) and attributes.
o Color image:
Three different ways of getting a colour image of a scene:-
1. Filter mosaic; (Bayer filter)
2. Prism
3. CCD
o Calibration:
It protocol of a process.
1. Geometrical calibration is proper distance.
2. Spectral Calibration is proper segmenting
o Future Process Mineralogy:
 In Mining:
a. Help utilized low grade mines
b. Merging standard and new processes
c. Optimum grinding
Techniques Other Beam Emission Detection Necessary Diagrams Sample preparation Type of Comments
names material

IR IR photons Vibration (stretching, Absorptions made by each Pellets composed of about 1 mg For tightly Gives
Spectroscopy bend, type of bond in the of pulverized material and about bonded absorption
(IR Spectra) twisting,rocking) compound. This produces a 300 to 400 mg of KCl. molecules. band by
spectrum, Organic absorbing IR
normally a 'plot' of % compounds at different
transmittance against wavelength.
wavenumber.

XRD By Max X-ray X ray itself is -Fast analysis

1913 using diffracted then using -Two hour
vasuvianite Bragg law h,l,k unit -Low cost
cell are located. per analysis
The peaks in graph
shows the 202 plane
from which xray is
diffracted.

XRF X-ray Photon Two types based on catching Even though the energy E of a photon Heavier
detecting photon: and its wavelength λ are virtually A WD wavelength-dispersive than
Energy Dispersive (EDXRF) or exchangeable (because of the fixed spectrometer treats the X-rays oxygen.
Wavelength Dispersive relation E = (c∙h)/λ, with c being the as waves and uses some regular
(WDXRF) speed of light and hth Planck constant) structure (gratings or crystals) to
the way of sorting the photons with cause interference patterns that
Two basic quality principles respect to either E or λ is quite different: allow for remarkably high
with XRF analysis are spectral resolution. Has analyzer
precision and accuracy. The selection of the optimal crystals to separate X ray
spectrometer is driven by the analytical photons emitted by the samples
requirements: based on their wavelength,
•Portable, benchtop, or lab-based following Bragg’s law.
element analysis
•Number of samples to measure per day The ED energy-dispersive
•Material/sample type and preparation detectors treat the X-rays as
•Elements of interest, concentration particles. (electrons) are ejected
ranges & limits of detection by each impact. Heavier or
•Accuracy and precision faster bowling electrons impact
•Sample structure and structure size more.
XRF (Portable) Even lighter elemets Mg, Al, No need of vaccum or helium Alloy,
Si atomosphere. coating,
Precious
metals.
EPMA Beam of X-ray EDS (energy dispersive 2micron best.
(Electron electron, spectrometer) counts 30 micron normal.
probe micro- modified by number and energy of xray
analysis) current and photon. Must be carbon coated and
voltage. -Morphology, coating and vaccummed.
chemical composition can be
detected.
-Also chemical mapping
SEM Similar to Electron SE: topography of sample Raman can be integrated with SEM Thin section or resin
EPMA, BSE: atomic number based (Scanning Electron Microscopy) for Polished to 20 steps glos
forms on relative density of sample SEM SCA (structural and chemical
image using atoms(chemical analysis), which has applications in Must be carbon coated and
SE and BSE. composition) means more geology & mineralogy. vaccummed.
BS electron are released For example, you can then study opaque
minerals and petrographic thin sections
that do not transmit light.
Secondary Ion Primary ion Secondary ions (the At deflection, mass/charge SIMS analyses are performed on Trace
Mass beam by a sample itself into ratio is detected. individual grains, larger than 40 elements in
Spectroscopy process molecules ions to 50 microns, minerals,
(SIMS) termed forming crater) the The depth of the sputter mounted in polished sections. Gold ( less
"sputtering“. gas phase ion crater is measured with a 0.1 ppm) ,
produce from profibneter , and the sputter isotpes
molecules. So time is converted to depth.
vaporized-ionized-
accelerated-
deflected-detected
Raman It is due to Photons Changes in Chemical analysis, Thin section, polished surface Minerals Fast analysis,
spectroscopy the polarization of Crystalinity (distinquish usually less
scattering molecules, which is polymorphs) than 1
of light by deformation in minute
the electron clouds. Each The vibration is
vibration molecule raises to
molecules. specific energy
The transition level, then
vibration is return releasing the
Raman spectrum. (raman
active if it spectrum)
cause
polarization
.
Image Electron SE & BSE 30mm Resin 3D info from
Analysis 2D