Transcript An Introduction to Portable XRF for Exploration, Mining and Geochemistry Applications Scott Curry & Cindy Collins Innov-X Canada Presentation Outline • • • • • • Fundamental XRF Concepts and Sample Data Limitations.

An Introduction to Portable XRF
for Exploration, Mining and
Geochemistry Applications
Scott Curry & Cindy Collins
Innov-X Canada
Presentation Outline
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Fundamental XRF Concepts and Sample Data
Limitations of Portable XRF
Xplorer - Seamless XRF/GPS/GIS Integration
Sample Applications
Sampling, Project Planning and Tips for XRF
Questions
What can XRF do for reclamation?
• Tailings
• Chemical disposal
• Soil and water contaminant analysis for mine site and
perimeter monitoring
• Provide large inexpensive datasets continuously from
environmental baseline data to clean up and monitoring
• Be an integral part of the mine reclamation plan
• Be part of the tool chest of technologies and methodologies
for reclamation during and after life of mine from removal
of structures (Pb paint testing & metals recycling) to
analyzing tailings and waste rock disposal (hydrological and
soil testing)
Fundamental Concepts
What does XRF do?
• Portable XRF can quickly and
effectively Detect and Quantify the
elements from Mg to U on the
periodic table.
• Non destructive – can test the same
sample multiple times.
• Fast – data can be achieved in
seconds resulting in large and
inexpensive data sets.
• Portable – get results at the actual
sample location
• Accurate - Can develop semiquantitative to quantitative data sets.
Sample Applications
History of XRF
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From the discovery of x-rays in 1895 to the quantification of x-rays
in 1913 and the development of early XRF Spectrometers in the
50’s, XRF research and development continued has become what it
is today
Early spectrometers were WDXRD measuring wavelength for one
element at a time
With the need for smaller sized equipment, lower costs, and use by
less skilled operators came the EDXRF in the 60’s; EDXRF measures
the characteristic energy of an element
Subsequent improvement in detectors and signal resolution lead to
measurement of several elements in one sample
Early EDXRF use radioisotopes for excitation requiring recycling of a
depleted radioactive source, recalibration and replacement at
significant costs
Current state-of-the-art EDXRF includes x-ray tubes, solid-state
components, electronics, computers and software
Now this mature technology is routinely used for R&D, QC,
production support and regulatory compliance
Energy Dispersive XRF
Energy Dispersive XRF
Energy Dispersive XRF
Energy Dispersive XRF
EDXRF Spectral Capture
Spectra from Contaminated Soil Sample
12
Fe Ka
Intensity (Counts per second)
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8
6
Mo Ka
4
Pb La
Pb Lb
Tube Lines
and scatter from sample
Sr Ka
Fe Kb
2
Cu Ka
Rb Ka
Zn Kb
0
5
10
15
20
Energy (KeV)
Example of export format (csv file)
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30
Applications
General Environmental Applications
• Mine reclamation
• Environmental baseline data over
large areas with large inexpensive
datasets
• Liquid analysis
• Pb paint analysis
• Filter analysis
• Soil and other materials
Pb in soils
• Blacksmith Institute working to limit Pb
poisoning plaguing remote villages in Nigeria
• In seconds the XRF analyzer identifies
pollutant metals including Pb as low as 0.001%
• Remediation begins and processing
procedures are altered to avoid a recurrence
Hazardous Waste Screening
• Debris for hazardous or nonhazardous disposal in lieu of TCLP
testing (toxicity characteristic
leaching)
• Extreme weather debris migration
• Construction or demolition project
waste
• Waste streams and oil pools
• Industrial and mining process on
community perimeters
Property Assessment
• Immediately identify heavy metals
in soil at low ppm levels
• Real-time metal screening at
construction or disposal sites – Pb,
U, RCRA, Priority Pollutants
• Brownfields Phase I/II/III
• Lead (Pb) clearance failure
avoidance
• Tube-based Pb Paint Analysis
• Airborne metals in mining,
welding, construction, fabrication,
maintenance and repair, paint
removal and renovation
Published SOP Methods
• EPA 6200
– XRF soil testing
• HUD PCS for testing Pb in Paint
• NIOSH Method for Pb in filters
• OSHA Method ID204
– Quantitative X-Ray Fluorescence Analysis of Workplace
Substances ID204. (Air or wipe filter & bulk material)
• RWM-DR-025
– Metals in solid media
Peer Reviewed Tech Articles
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Arsenic in Hurricane Katrina Wood Debris
Determination of Br in Regulated Foods
Determination of Soil Calcium Using FPXRF
Evaluation of New XRF Instrumentation at Hazmat and
Abandoned Mine Land Site – Hazardous Materials
Evaluation of Portable XRF for Gypsum Quantification in Soils
Evaluation of Technologies for Sorting CCA-Treated Wood
Identification and mapping of heavy metal pollution in soils
Identification through XRF of Dental Restorative Resins
Presence and Breakdown of BFRs in Vehicles
Reclaiming Military Bases from Tungsten Takeover
Triad Case Study: Former Small Arms Training Range
CCA – Identify Toxin-Treated wood products
• Screen recycled wood mulch, pellets
& other by-products for toxic metals
• EPA compliance & label confirmation
at wood treaters, lumberyards, retail
centers
• Screen in-coming wood at municipal
incinerators, landfills & recycling
facilities
• Determine effectiveness of protective
coatings & sealants from CCA & other
toxins
• Test for arsenic leaching out of
unlined landfills & around residential
wood structures
Lead Inspection
• Lead Inspection :Classify definitive
positive/negative results for Pb in seconds
• Comply with restrictions on lead exposure
during building demolition & construction
• Use in manufacturing, homes or commercial
buildings
Innov-X System Environmental Analyzers
• A Field-Proven, X-ray Tube-Based System: No Radioactive
Isotopes!
• Accurate Analysis of RCRA (Resource Conservation & Recovery
Act) Metals & Priority Pollutant Metals in Seconds
• Meets OSHA Methods OSA1 & OSS1 and EPA Method 6200 and
NIOSH Method 7702!
• In-situ Tests: Rapid, thorough site investigations, delineation
and contamination patterns
• Confirm the minimally required samples to drive investigation
• Avoid confirmatory lab testing of high-concentration samples
• Establish area contamination boundaries and depth profiles
• Dock into convenient testing stand for bagged or liquid samples
• Test directly thorough corings for depth profiles
Sampling, Project Planning and
Tips
XRF Sampling and Planning
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Clearly establish project & sampling objectives
Determine the level of data quality required by XRF: field
screening or lab quality? Is it FIT FOR PURPOSE?
Establish an appropriate procedure (test times, number of
tests etc.)
Correct & Appropriated Use of Calculation Modes (CN & FP)
Always keep good records of Field Work
Incorporate QA/QC Protocols: Test relevant Matrix Matched
Standards, Blanks & Field Duplicates
• Dispatch a proportion of samples for confirmatory analysis:
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min 5% up to 20% for checking calibrations
XRF Sampling – Tips in the field
• Decide on sample spacing/density prior to heading into field –
• Regular Grid? Staggered Grid? How does my grid fit the existing
geology, background and the project?
• Grid Systems & Projections– Lat/Long WGS84? Or Local Grid?
• Be Prepared:
• Do not forget Standardization Materials
• Pack extra batteries & Windows (Kapton or PP?) +
Screwdriver to remove Window Assembly
• Include a soft lens cloth for cleaning the Window –
always good to check the window after every analysis
to remove contamination & inspect for damage/holes
• Carry necessary standards / blanks
Which Horizon?
• The surficial geology (regolith) is extremely
variable dependant on environment,
underlying rock type and contamination
sources (mining, farming, manufacturing)
• Important to ensure consistent approach to
sampling horizons – sample the same
horizon(s) at each location
• Common to sample several horizons at one
sample location ie. Soil A, Soil B, Saprolite,
Bedrock or Cap-rocks…etc.
• Documentation is Integral! – Store these
observations with Chemistry to enable later
correlation.
• Make sure you are comparing apples with
apples when analyzing data!
Sampling Considerations
• Remember, typical sample size is
around 1cm2 – Collimated X-RAY Beam
usually <3mm in Width
• Depth of Penetration is generally
limited to the surface of most samples
– up to 2-5mm in very light Matrix
samples
• Need to get the detector as close to
samples as possible – Built In safety
Feature for “Air Shots” (based on lack of
count rates received back)
• Use Matrix specific calibrations for
specific sites and known areas of matrix
variation
Sample Preparation
Mg Andesite
(In Situ)
5 mm
Soil Sample 5 mm
Sieved to 250
micron
Preparing your sample can significantly
enhance the result quality:
 Crushing /milling / pulverizing of the sample
for smaller particle sizes, sample uniformity &
increased homogeneity
 Take advantage of new portable & mobile field
preparation devices – such as Rocklabs / Essa
portable Crushers & Mills
 Potential to setup Miniaturized /
Containerized sample prep facilities in the
Field to support XRF Sampling programmes
 For less homogenous samples – multiple
readings & averaging can be effective
 Dry the sample to take away moisture effects
Sample Method
In-situ analysis with FPXRF
Collect 50g of sample
Split sample into two equal portions
of at least 25g each
Wash through a sieve to isolate the
silt and clay sized fractions
Re-analyze sample in the field using
FPXRF
Re-analyze using the FPXRF in the
field
Store sample for laboratory analysis
(XRF, ICP-MS)
Store for laboratory analysis (XRD,
ICP-MS)
Addressing Issues
• Problem Samples do exist – ie: Oxidized surfaces, very light
matrices, very dense matrices…etc.
• Variations due to Sample Type & Homogeneity – ie: Fine
Dust vs Chips vs Core vs in-situ Rock. Vertical Segregation /
Stratification of sample into bags & speared samples splits.
• Other effects do exist and can be corrected for if known,
such as moisture & attenuation through plastic/calico
bags…etc.
• Ensure the instrument has the correct elements configured
(are they turned on?) and correctly calibrated. DO NOT
simply attempt to turn an element on!
Key Points to Remember
• Factors can adjust for matrix effects - Use LAB data
to verify chemistry and correct via the User Factor
set
• Can also use Matrix Matched certified standards to
correct factors if the matrix is consistent
• Chemistry results are only from what the X Rays
see. Beware of homogeneity and surface effects.
• Longer Tests = better precision within limits
Adding Value to XRF Data
How can I add value to my XRF Data?
• XRF Sampling is NO Different to any other sampling regime
you adopt!... Remember the Data is very valuable (& costly)!
• So, Use good QA/QC Protocols & Data Validation
• Incorporate Standards, Blanks, Field Duplicates and Check
Samples to increase your understanding & confidence
• Rank & Store the Data in a well ordered & structured DB
Innov-X - Choosing an Analyzer
Innov-X Systems Existing Products
David Pawliuk, Vice President, Exploration,
SILVER QUEST RESOURCES LTD., Vancouver, BC
“We acquired an Innov-X Omega XRF unit early in the 2010 field
season. The unit went to Yukon, where it was used to test soils in
the Dawson Range for the pathfinder elements (As, Sb)
associated with gold mineralization. By using the Omega our crew
could immediately identify and follow-up on mineralized trends
exposed in our backhoe trenches. The trenching was more efficient
and focused than it otherwise would have been, saving precious
time and thousands of dollars. The Omega may have paid for itself
already.”
Introducing the handheld
New Delta Handheld XRF
• Launched globally Feb 1, 2010 as superior XRF
platform to Alpha and Omega systems.
• 4Watt System = most powerful Hand Held XRF
on the market.
• Large Area SDD = highest count rate and lowest
signal to noise ratio on the market. Light element
measurement capability in air (Mg, Al, Si).
• Design Brief
– Smaller / Faster / Cooler / Tougher
– Upgradeable
– Tube anode optimization (Ag, Au, Ta, Rh)
– Capable of incorporating a camera and
collimator for targeting smaller (<1cm2)
analysis areas on samples (grain size issues)
– Leap frogs existing technology in as many
ways as possible
– Add innovations as appropriate and make
expandable and adaptable.
Delta Handheld XRF Product Models
• Premium Vacuum (for low level Mg)
– Large Area SDD and vacuum.
• Premium
– Large Area SDD detector
• Standard
– Typical SDD Detector
• Classic
– PIN diode detector
• Range of tube anode materials available
SDD = New Silicon Drift Detector Technology
PIN = Older Silicon PIN Detector – as used in Alpha
Portable Test Stand for Handhelds
• Portable Test Stand for the Omega and Delta
• Allows use of the Handheld like a bench top to obtain maximum
flexibility, in field or fixed in camp or lab
• Can be operated from laptop computer
Lid Open
Lid Closed
Dr. Trevor MacHattie, Mineral Deposits Geologist,
NOVA SCOTIA DEPT. of NATURAL RESOURCES
“The X-5000 produces rapid, amazingly accurate, and
precise geochemical data for us. We’ve recently discovered
new rare earth element mineralization with the aid of the X5000 and it has now become an essential tool in our field
work and mineral deposit research, every geologist should
have one!”
Introducing the original portable bench top
X5000
New X-5000 Portable Bench Top
• 10 Watt System = most powerful portable XRF
on the market.
• SDD detector = Lowest LOD’s achievable. Light
element measurement capability in air (Mg, Al,
Si). Better lower limits of detection than Hand
Held for some elements (Au, Sb, Sn, Cd, Rare
Earths)
• Range of tube anode materials available for
optimization for application.
• Ideal for basing in an exploration camp, sample
prep facility or lab where samples are collected
and brought back to a central location for
sample preparation and analysis.
• Ideal as a back-up system to lab based
equipment and online/on-stream systems.
• No operator licence required in Canada.
• Completely portable with battery pack.
New X-5000 for Oils, Fuels & Liquids
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Transportation
Power Generation
Petrochemical
Aerospace
Mining
Element
X-50
(ppm)
Wear Metals
Titanium
Chromium
Iron
Nickel
Copper
Lead
10
3
1
1
1
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Fuels, Additives Analysis
• Rapid on-the-spot elemental analysis for
oils, fuels and other liquids
• Unique fluid handling system
• Uses 50 KeV tube, 10 Watt power rating
Sulfur
Calcium
Vanadium
Zn
Molybdenum
Barium
500
30
5
10
20
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Other Applications
Hg, in aqueous solns
P, in aqueous solns
Cl, in process fluids
10
1000
200
Flexibility in application
Delta Xplorer System
Seamless XRF/GPS/GIS/
Geochemical Analysis Integration
Ross Sherlock Exploration Manager, Gold Fields Canada, “We have
used the Omega XRF fairly extensively in our Canadian exploration efforts
and are pleased with the results. In the right environment the tool provides
fast and reliable geochemical information reducing lab costs and turnaround time.”
Delta Xplorer System
A Total Field Data Collection Solution Consisting Of:

Ruggedized Innov-X Systems Delta Portable XRF Analyzer
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Ruggedized TRIMBLE NOMAD or YUMA Field Computer
with built in GPS +/- Optional High Accuracy DGPS
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ESRI ArcPAD or ENCOM Discover Mobile – Field Mobile
GIS Integration Package
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Mobile GIS extension software – Bluetooth
communication software between Delta XRF, Trimble
GPS and GIS software.
The Essential Mobile GIS Solution for Real-Time FPXRF
Delta Xplorer Overview
In-field example: Tritton Cu NSW
Nominal 50m x 50m
Sample Grid Designed
Actual Sample Location
Taken By DGPS
Sample Chemistry
Registered Real-Time
Xplorer Workflow
Xplorer - Simplified Workflow:
1. Innov-X Delta & TRIMBLE Nomad are Bluetooth paired for Communications
2. Mobile GIS started on Trimble Nomad
3. Soil Readings taken outside in open air & Result Received on Nomad
4. GPS Position Confirmed on finalization of result
5. Data is exported from Trimble Nomad
• to Mapinfo or ArcPad
• to ioGAS
6. Data presented graphically in Parent GIS
Delta Xplorer - Output
Delta Xplorer - Output
WGS84 Locations
Full Chemistry
from FPXRF
Google Earth
Export
From ioGAS
ANCHORAGE
VANCOUVER
1201 W. Georgia St, Suite 2
Vancouver , BC V6E 3J5 CAN
T. +1 778 960 6279
F. +1 888 873 6598
W. www.innovx.ca