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Innovation with Integrity
Rare Earth Element Prospecting and Production,Starring Analytical X-ray as Indiana Jones!
Bruker AXSMadison, WI
Today’s Topics
• Introduction to the Rare Earth Elements
• What, where, and other important facts
• Economics and uses
• Deposits, resources and production
• Analytical Tools
• Mineralogical Analysis
• Chemical Analysis
Welcome
20.05.2011 2
Speakers
Alexander SeyfarthProduct Manager, XRFMadison, WI USA
Holger CordesApplications Scientist, XRDMadison, WI USA
Introduction to Rare Earth ElementsWhat are they?
Rare Earth Elements (REE) are a group of chemical elements that occur together in the periodic table: 15 Lanthanide elements + Sc and Y
REE are soft, malleable, ductile and usually quite reactive metals.
MP range from 798 to 1663 deg C(CORDIER & HEDRICK, 2010)
All REE are classified as metals. Chemical properties are similar and often all of them occur together in the same minerals.
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20.05.2011 4
Use of Individual Rare Earth Elements
Usage of rare earth minerals by gigagrams (Gg). Credit: Xiaoyue Du and T. E. Graedel
InnovationNewsDaily Senior Writer Jeremy Hsu on Twitter @ScienceHsu
• Importance and use of REE grows with increased use of ―battery‖ and ―Clean Air‖ related technology
Clean Air and Hybrid Car TechnologyRequire REE
© GM 2011
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• Applications lack substitutes
• Linked to global supply chain
National Security is Impacted by REE
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World REE Mineral Reserves and Production
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U.S. Geological Survey, Mineral Commodity Summaries, January 2011
• In 2010, China announced it would significantly restrict REE exports to ensure supply for Chinese domestic manufacturing
• 72% REE export reduction in 2010
• 35% REE export reduction in 2011
• Quota reduction officially to curb ―rampant and unregulated‖ production over the last few years, which has caused significant environmental problems
Chinese Era of REE Domination
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• The New York Times reported that the Chinese Central Government is placing all ―provincial‖ districts under oversight, removing local officials and taking steps towards a ―National Rare Earth Mining Area‖
• US Government is pressuring China for assurance on exports; China is leery of international commitments
• Most Chinese deposits are unique with very high concentrations of heavy REE, such as Sm and Dy, and lowest contamination of Th
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Chinese Mining Under Government Control
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Demand and Production
Are Rare Earth Elements Rare?
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REE
Where Can We Find REE?
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• REE are relatively abundant in the earth’s crust, but discovered mineable concentrations are less common than other ores
• Main minerals within the ore resources are bastnaesite and monazite
• Mineralizations are associated with:
• Carbonatite complexes
• Bauxite/laterites
• Absorbed in clays (IAClays)
• Magnetite
• Uranium deposits
• Vein (hydrothermal)
• Placer (residual)
• Peralkaline Igneous deposits
REE Ores and Minerals Are Very Complex
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• What tools are there for the characterization of minerals and ores?
The Instrument-Makers’ Solutions
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• Traditional mineralogical analysis is done by microscopy or phase separation
• Shape, color, symmetry, refractive index, etc.
• For complex rocks, an electron microprobe is used, combining imaging with elemental analysis
• There is a direct way to identify minerals as well!
Mineralogical Analysis
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Mineral Identification by XRD
50484644424038363432302826242220181614
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Bastnaesite
Monazite
Image: www.mindat.org\ min-2751.html
Image from www.wikipedia.org
Unit cells Powder diffraction patterns
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What Kind of Information Can Be Obtained From a Powder Diffraction Pattern?
• Peak position dimension of the unit cell, lattice parameters, space group
• Peak intensity content of the unit cell, atomic positions
• Peak broadening strain/crystallite size
• Scaling factor weight percent of phase
• Background degree of crystallinity
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Powder Diffraction BasicsSample
Diffraction of an ideal powder
Diffraction of a small number of crystallites ("spotiness effect")
Diffraction of textured materials
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Point detectors • Scintillation
detector• XFlash® detector
PSD• VÅNTEC-1• LYNXEYE
Area detectors• VÅNTEC-500• VÅNTEC-2000
Detector Options for Mineral Analysis
Commonly used for routine Rietveld analysis with Bragg-Brentano geometry
Can be used for Rietveld analysisof small spots,micro-diffraction, mapping, non-ideal powders
High speed analysis, quality control
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Bastnaesite Ore Measured in D2 PHASER
• D2 PHASER
• LYNXEYE detector with 5.6 opening and Ni filter
• 0.6 mm divergence slit
• 2.5 primary Soller, 4 secondary Soller
• 0.02 steps, 0.5 s/step
• 25 minutes
• XFlash® detector
• 2 mm divergence slit
• 0.2 mm receiving slit
• 2.5 primary Soller, 2.5 secondary Soller
• 0.02 steps, 10 s/step
• 8 hours, 30 min
Lin
(C
ounts
)
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2-Theta - Scale
15 20 30 40 50 60 70
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REE Concentrate Measured in D2 PHASERPhase Identification with EVA
• D2 PHASER
• LYNXEYE detector with 5.6 opening and Ni filter
• 0.6 mm divergence slit
• 2.5 primary Soller, 4 secondary Soller
• 0.02 steps, 0.5 s/step
• 25 minutes
00-005-0586 (*) - Calcite, syn - CaCO3
00-036-0426 (*) - Dolomite - CaMg(CO3)2
01-071-2393 (C) - Strontianite - SrCO3
00-046-1295 (I) - Monazite-(Ce) - (Ce,La,Nd)PO4
01-083-0077 (C) - Synchysite-(Ce) - CeCaF(CO3)2
00-038-0400 (I) - Hydroxylbastnasite-(Nd) - NdCO3(OH)
00-011-0340 (I) - Bastnasite-(Ce) - CeCO3F
File: sample 180071 0.6mm lynxeye 5.6dg 4dg soller_disc0.19.raw
Lin
(C
ounts
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2-Theta - Scale
10 20 30 40 50 60 70 80 90
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Phase Identification Using DIFFRAC.EVA Software and Elements as Filter Criteria
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Phase Identification Using DIFFRAC.EVA Software
05000
10000
15000
Counts
10 20 30 40 50 60 70
2Theta (Coupled TwoTheta/Theta) WL=1.54060
01000
2000
3000
16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33
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Element Identification Using D2 PHASER with XFlash® Detector, Bastnaesite Deposit
• Collected at 45incident angle for
10 minutes
• Ce and Nd can be identified, possibly Pr and very minor Y
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Element Identification Using D2 PHASER with XFlash® Detector, Concentrate
• Collected at 45incident angle for
10 minutes
• La, Ce, Pr, Nd, Smcan be distinguished
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Quantitative Mineral Analysis Using X-ray Diffraction
Standard-based methods
• Conventional method (DQuant): Calibration curve with standards required, mostly used for quality control, accurate but problematic with peak overlap between phases
• Reference intensity ratio method: Quick semi-quantitative method for many minerals using the I/Icor values from the ICDD database (can be done in EVA program)
• Full pattern analysis: Scaling of full patterns of standard minerals, very consistent sample preparation and standard minerals necessary
Standardless methods
• Rietveld analysis with TOPAS: standard-less, peak overlap between phases can be resolved, all crystal structures have to be known
20.05.2011 26
The Rietveld Method
• Standardless full-profile approach to quantitative phase analysis• Uses every data point as a unique observation and least-squares methods to
minimize the difference between calculated and measured intensities• Residual of Least Square Refinement
R = Σ wi(yi – yci)2
Rietveld Analysis requires: • The crystal structure data for every phase in a mixture (unit cell and atomic
positions) • A model for the peak shapes and widths and a model for any aberrations• A model for the background
The relative masses of all phases contributing to the diffraction pattern can be derivedfrom the refinement using the simple relationship:
Wr = Sr (ZMV)r / t St (ZMV)t
Wr is the relative weight fraction of phase r in a mixture of t phasesS is the scale factor derived from Rietveld refinementZ is the number of formula units per unit cellM is the mass of the formula unit (atomic mass units)V is the volume of the unit cell (Å3 ).
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Bastnaesite Deposit Quantitative Analysis Using TOPAS Software
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Bastnaesite DepositQuantitative Analysis Using TOPAS Software
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Bastnaesite DepositQuantitative Analysis Using TOPAS Software
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Bastnaesite DepositQuantitative Analysis Using TOPAS Software
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Bastnaesite DepositQuantitative Analysis Using TOPAS Software
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Bastnaesite DepositQuantitative Analysis Using TOPAS Software
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Bastnaesite DepositQuantitative Analysis Using TOPAS Software
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ConcentrateQuantitative Analysis Using TOPAS Software
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Solid Solution EffectsSchematical Representation
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Solution PhasesQuantitative Analysis Using TOPAS Software
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• Absolute method for direct and highly accurate quantitative phase analysis of mineral mixtures, if the crystal structures are known
• Standardless method for determination of phase amounts, lattice parameters, crystallite size and much more
• Independent of equipment and sample properties such as tube aging, solid solution effects, and preferred orientation
• Intrinsic handling of solid solution and preferred orientation effects
• Operator-independent
• Can be operated without human interaction (TOPAS BBQ)
Quantitative Rietveld AnalysisAbsolute and Standardless
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• R & D, Centralized Lab
• Most flexible unit, capable of all shown applications
• Widest range of components
• Highest power/flux and smallest spot sizes
• Process Analysis
• Quantification with large, sturdy sample changer
• Ease of use
• High power
• Tie into automated concepts
InstrumentationLaboratory or Process Instrumentation
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• Fastest desktop X-ray diffractometer
Choice of
• LYNXEYE detector
• Scintillation counter
• XFlash® detector
• Completely self-contained, including cooling and PC
• Rugged instrument with high resolution for complex minerals
• Highest resolution XRD/XRF unit
Benchtop Diffractometer
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In Addition to Minerals, We Need to Know the Chemistry!
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• Classical ―wet‖ chemical approach
• Atomic Spectroscopy approaches:
• Beers Law (absorption proportional to concentration)
• Free atoms (outer electron shell interactions)
• Detection with a variety of detectors
• Different techniques
• AAS
• ICP
• ICP MS
• LIBS
• LA-ICP-MS
• X-ray Spectroscopy
Elemental Analysis for REE
NEW ICP-MS M90
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XRF is the method for:
• doing qualitative and quantitative analysis of elemental composition
• by excitation of atoms and detection of their characteristic X-rays
XRF: X-ray Fluorescence Analysisor X-ray Spectrometry
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XRF Sample Preparation Approaches
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45
How Characteristic X-rays are Generated in an Atom
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X-ray Energy Distribution from an X-ray Tube (Rh)
46
mA setting
controls
number of
photons
kV setting
determines
excitation
energy
20.05.2011
Bond energy of the electron
Absorption edge/ Excitation Potential
Excitation / Emission of Characteristic X-ray Radiation
Energy of incoming photon
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X-ray Emission Energies
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• Excitation Voltage: Rule of thumb is minimum 3x higher than emission line energy
• Detection of characteristic lines requires adequate resolution of the instrument
• The higher the emission energy the larger/thicker the analyzed layer of sample
• Calibration based on matrix matched reference material or by means of FP (makes possibly semi quantitative)
Exciting Rare Earth Elements… Using X-rays
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XRF: X-ray Fluorescence Analysis
Energy of X-ray photons• Which element
• Qualitative analysis
Number of X-ray photons at a given energy • What concentration
• Quantitative analysis
Sample
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Energy-Dispersive XRF
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Wavelength-Dispersive XRFSequential
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Wavelength-Dispersive XRFSimultaneous, Multielement Channel™
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EDXRF versus WDXRF
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XRFSelecting the Right Tool for the Job
• What equipment can be used where?
• What can we determine?
• Which tool to use for the job?
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REE Exploration
Search for deposits
Qualification of deposits
“accelerating” discovery
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• Usually, all REE are present, with various ratios in high concentrations
• Light REE vs. Heavy REE are of economic interest
• Y, Sc is indicator for HREE presence
• Detecting Y, Ce, La is critical for REE exploration
• Detecting Th is important as well since it ―penalizes‖ the value due to increased processing:
• Th concentration is low!
• Most ores are very high in Fe, Ca and also contain Sr and Nb(more interferences on EDX)
• Matrix affects quantification, and reference samples should be used for calibration which potentially matches the unknowns:
• Chicken or Egg Question?
• Data needs to be related to 3-D space / map
Exploration: Analytical Challenge
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Excitation in Practice
• EDXRF units: 50 kV max. (HH units around 45 kV)Resolution < 150 eV at >100,000 total cps with XFlash® detector
• Power level from 1 Watt (HH) to 50 Watt (Benchtop)
• K-Lines for Ce, Pr, Nd can be detected and easily separated, but yield is low
20.05.2011 58
• Using best-in-class resolution (<145 eV at 100,000 cps), L-lines cannot be easily separated
EDXRF Detection of REE L-Lines
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Ce, Pr, Nd Detection on 45-kV EDXRF (1.2 Watt)
15 20 25 30 35
- keV -
10
102
103
104
105
Pulses
Ce Ce Ca Gd Gd La La
Y Y Pr Pr
Sr Sr
Rb
Rb
Fe Yb Yb Tm Tm
Er
Er
Ho
Ho
Dy
Dy
Pb Pb Nd
Nd
Sm
Sm
Eu
Eu
Tb
Tb
Sn Sn Rh
Rh
15 20 25 30 35 40
- keV -
102
103
104
105
Pulses
Ce Ce Ca Gd Gd La La
Y Y Pr
Pr
Sr Sr
Rb
Rb
Fe Yb Yb
Tm
Tm
Er
Er
Ho
Ho
Dy
Dy
Pb Pb Nd
Nd
Sm
Sm
Eu
Eu
Tb
Tb
Sn
Sn
Rh
Rh
Y K1 Sum
Y KB Sum
LOG Scale
LOG Scale
For best yield, we need
higher power…
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K-Lines Using 60-kV WDXRFBastnaesite Ore
01
02
03
04
05
01
00
20
03
00
KC
ps
Pr
KA
1
Ce K
A1
Ce K
B1Pm
KA
1
Nd K
A1
La K
A1
La K
B1
Pressed 1 60 KV None XS-400 0.23 degr.
Pressed 1 60 KV None LiF200 0.23 degr.
Pressed 1 60 KV None LiF220 0.23 degr.
Pressed 1 60 KV None LiF420 0.23 degr.
28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49
KeV
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Gadolinite Mineral on Handheld Unit
5 6 7 8
- keV -
0
1
2
3
4
5
x 1E3 Pulses
Ce Ce Ce Ca Ca Gd Gd Gd La La La
Rh Rh Rh Y Y Y Pr Pr Pr Sr Sr Sr
Rb Rb
Rb
Fe Fe
Yb Yb Yb Tm Tm Tm
Er Er Er Ho Ho Ho Dy Dy Dy
Pb Pb Pb Nd Nd Nd Sm Sm Sm Eu Eu Eu
Tb Tb
Tb
5 10 15 20 25 30
- keV -
102
103
104
105
106
Pulses
Ce Ce Ce Ca Ca
Gd Gd Gd La La
La
Rh Rh Rh Y Y Y
Pr Pr Pr
Sr Sr
Sr
Rb
Rb Rb
Fe Fe
Yb Yb
Yb
Tm Tm
Tm
Er Er Er
Ho Ho
Ho
Dy Dy
Dy
Pb Pb Pb
Nd Nd
Nd
Sm Sm
Sm
Eu Eu
Eu
Tb
Tb
Tb
20.05.2011 62
WDXRF L-Line Separation0
.20
.30
.40
.51
23
45
67
81
02
03
04
05
06
01
00
20
03
00
KC
ps
Pr
LA
1
Pr
LB
1
Ce L
A1
Ce L
B1
Pm
LA
1
Pm
LB
1
Nd L
A1
Nd L
B1
La L
A1
La L
B1
La L
B2,1
5C
e L
B3
Ce L
B2,1
5S
m L
A1
Sm
LB
1
Fe K
A1
Pr
LA
1
Pr
LB
1
Pr
LG
3
Fe K
A1
Pr
LA
1
Pr
LB
1
Ce L
B1
Pm
LA
1
Pm
LB
1
Nd L
A1
Nd L
B1
Eu L
A1
Eu L
B1
Sm
LA
1
Sm
LB
1
La L
A1
La L
B1
Gd L
A1
Gd L
B1
Pressed 1 50 KV None XS-400 0.23 degr.
Pressed 1 50 KV None LiF200 0.23 degr.
Pressed 1 50 KV None LiF220 0.23 degr.
La L
G1
4.5 4.6 4.7 4.8 4.9 5 5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 6 6.1 6.2 6.3 6.4 6.5 6.6 6.7
KeV
20.05.2011 63
WDXRF L-Line Separation 0
12
35
10
20
30
40
50
60
70
80
90
10
02
00
30
0
KC
ps
Pr
LA
1
Pr
LB
1
Ce L
A1
Ce L
B1
Pm
LA
1
Pm
LB
1
Nd L
A1
Nd L
B1
La L
A1
La L
B1
La L
B2,1
5C
e L
B3
Ce L
B2,1
5S
m L
A1
Sm
LB
1
Fe K
A1
Fe K
B1
Pr
LA
1
Pr
LB
1
Pr
LG
3
Fe K
A1
Fe K
B1
Pr
LA
1
Pr
LB
1
Ce L
B1
Pm
LA
1
Pm
LB
1
Nd L
A1
Nd L
B1
Eu L
A1
Eu L
B1
Sm
LA
1
Sm
LB
1
La L
A1
La L
B1
Gd L
A1
Gd L
B1
Nd L
G3
Nd L
G2
Pressed 1 50 KV None XS-400 0.23 degr.
Pressed 1 50 KV None LiF200 0.23 degr.
Pressed 1 50 KV None LiF220 0.23 degr.
4.5 4.6 4.7 4.8 4.9 5 5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 6 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8 6.9 7 7.1
KeV
20.05.2011 64
Particle Size Effects of HeterogeneousPowder Samples
Compound Line Concentration
[%]
Energy
[keV]
Layer
Thickness [m]
Fe2O3 Fe KA1 0.722 6.40 174
MnO Mn KA1 0.016 5.89 139
TiO2 Ti KA1 0.016 4.51 66
CaO Ca KA1 30.12 3.69 104
K2O K KA1 0.103 3.31 77
SO3 S KA1 0.000 2.31 27
P2O5 P KA1 0.004 2.01 19
SiO2 Si KA1 1.130 1.74 13
Al2O3 Al KA1 0.277 1.49 8
MgO Mg KA1 21.03 1.25 7
Na2O Na KA1 0.029 1.04 4
CO2 46.37
Thickness of the
sample from which
90% of the
measured intensity
is derived
NBS 88b dolomite
Pressed pellet
without binder
Especially for the lines of light elements,
average grain size layer thickness
(typically grain sizes vary between : 20 - 200 m)
20.05.2011 65
• Direct measurements on rock face are limited by the analyzed layer of the sample (physics) and is independent of instrumentation
• Homogeneity is important: analysis of powders is best done on a portable stand setup!
• Factory calibration with type standardization for custom materials using one or two samples will have only limited accuracy
• Using generic ―non-calibrated‖ approach and using element ratios enables universal mapping of relative abundance
• Ideally, a custom calibration of major formations is done using characterized reference material for best accuracy!
Prospection for REE with Geochemical Exploration Tools:Recommendations for Portable or HH-XRF
20.05.2011 66
Prospection for REE with Geochemical Exploration Tools:Recommendations for Portable or HH-XRF
• 45 kV or higher excitation
• Resolution of detector <145 eV also at high count rates
• Higher power (BT) unit for Th and more K signal
Direct mapping data from the field can be averaged and reprocessed in camp
Loose powder or pellet approach yields better data than rock face
FP-based calibrations
Matrix matched calibrations for best performance
Customized calibration approaches
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Mining
20.05.2011 68
• High variable matrix for some locations
• All REE need to be quantified
• Th, U and other elements as well
• High precision
• Easy to use in ―challenging location‖
• Cost effective – less consumables
Mining Samples Analytical Challenge
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The Solution Lies in the Sample Preparation
20.05.2011 70
www.bruker-axs.com/webinars_xrf
MiningRecommendation for XRF
Where to mine and what?
HH-XRF or pXRF for grade control in the pit/mine
WDXRF for blast-hole screening
Mined ore can be
• Product
Accurate analysis for value
• Feed to processing plant
Variable ore requires sturdy calibration
model with screening for all elements
Various methods need to be applied,
elemental flexibility from F to Am!
WDXRF is most-suited tool
20.05.2011 71
Processing and Recovery
20.05.2011 72
The ability to process is very, very critical and very, very complex”Mark Smith of Molycorp
’5th International Rare Earths Conference’ Hong Kong, 2009
• Producing rare earth oxides is considerably harder than other mining processes
• Rare-earth element extraction involves many steps. In the case of bastnaesite, usually found in igneous rock formations, the ore is mined using traditional open-pit techniques. The bastnaesite is then removed from the rock by crushing the ore into a small gravel, and then grinding the crushed ore in a mill until it becomes a fine sand. That sand, or silt, gradually separates into different mineral grains — bastnaesite and other generally less valuable minerals. The silt is then run through a floatation process wherein a liquid element is added, and air bubbles introduced. The finer bastnaesite silt sticks to the bubbles and rises to the top of the liquid where it is skimmed off.i
• That is the first process. The bastnaesite must now be separated into its constituent rare earth elements. The mineral is usually sent to a separation plant where each element is separated using an acid or solvent extraction process.
“It’s a very long and involved process. That’s one of the biggest risks.It can take dozens, hundreds of steps to separate the rare earths.”
Yaron Vorona, Executive Director Institute for the Analysis of Global Security’s Technology and Rare Earth Metals Center
The Washington Independent, October 25, 2010
Mining is Easy… Processing is Not…
20.05.2011 73
• Instrument needs to be protected against spills, operator mistakes
• Direct, easy access to measurement position
• Protection over tube and secondary side
• Flexible setup requires that solid samples and liquid samples are processed on same system
• Fast change-over
• Fail-safe operation
• Helium purge needs to be at atmospheric pressure
• Sample needs to stay cool
Processing of the Ore UsingOrganics and Acids
20.05.2011 74
• Widest dynamic range: % to PPM
• Best resolution (High conc. next to low conc.)
• Better than 0.1% relative for concentrates and minors
• Configuration tunable for desired element combinations
• Solid and liquid samples can be analyzed directly
• Calibrations built once, then operational for years!
• QA/QC done by stable monitor samples
• Can be operated by… operators
• ―Retools‖ to different applications
• Universal Calibration Mode enables measurement and quantification of complete unknowns (e.g. process issue samples)
• Cost of operation/consumables much lower than atomic spectroscopy!
Process Control / Beneficiation of REEWDXRF Advantages
20.05.2011 75
• X–ray techniques are ideal complements for both field- and lab-based prospecting campaigns:
• Elemental quantification
• Mineral identification and quantification
• Mining and processing
• X-ray techniques are ideal to:
• Quantify: lower operating cost than ICP/AAS and less consumables
• One calibration is stable for years!
• Optimizing the processing chemistry for the mineralization
• XRD is used in the Cu mining industry as primary tool for leaching
SummaryREE Prospecting & Production
20.05.2011 76
Q & A
Any Questions?
Please type any questions
you may have for our speakers
in the Q&A panel and
click Send.
20.05.2011 77
For more information:
Check out Bruker Training Central (BTC) online training courses on www.brukersupport.com
• XRF Basics I: From Theory to Intensity (two 1-hr videos)
• XRF Basics II: From Intensities to Concentrations (two 1-hr videos)
• XRF Sample Preparation (two 1-hr videos)
• Fundamentals of Powder XRD (two 1-hr videos)
• Powder XRD Data Collection and Analysis (two 1-hr videos)
• Basics of Two-Dimensional XRD (two 1-hr videos)
Register for our upcoming webinar:
• XRF and Microanalysis in Geoscience, Jun 21, 2011
Visit us at:
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• Geological Society of America, Minneapolis, MN, Oct 9-12, 2011
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