1. Scott Curry & Cindy Collins Innov-X Canada
An Introduction to Portable XRF for Exploration, Mining and Geochemistry Applications
Scott Curry & Cindy Collins
Innov-X Canada

2. Presentation Outline 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

3. 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)

4. Fundamental Concepts

5. 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 semi-quantitative to quantitative data sets.

6. Sample Applications

7. History of XRF
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

9. Energy Dispersive XRF

10. Energy Dispersive XRF

11. Energy Dispersive XRF

12. Energy Dispersive XRF

13. EDXRF Spectral Capture
Example of export format (csv file)

14. Applications

15. 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

16. 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
The EPA provides a recommended soil testing method for XRF, EPA Method 6200

17. Hazardous Waste Screening
Debris for hazardous or non-hazardous 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

18. 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

19. Published SOP Methods EPA 6200 HUD PCS for testing Pb in Paint
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

20. Peer Reviewed Tech Articles
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

21. 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

22. 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

23. 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

24. Sampling, Project Planning and Tips

25. XRF Sampling and Planning
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:
min 5% up to 20% for checking calibrations 25

26. 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 26

27. 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!

28. 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 28

29. Sample Preparation
5 mm
Mg Andesite
(In Situ)
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
Soil Sample
Sieved to 250 micron
5 mm 29

30. Sample Method In-situ analysis with FPXRF Collect 50g of sample
Split sample into two equal portions of at least 25g each
Re-analyze sample in the field using FPXRF
Store sample for laboratory analysis (XRF, ICP-MS)
Wash through a sieve to isolate the silt and clay sized fractions
Re-analyze using the FPXRF in the field
Store for laboratory analysis (XRD, ICP-MS)

31. 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!

32. 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 32

33. 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

34. Innov-X - Choosing an Analyzer

35. Innov-X Systems Existing Products

36. Introducing the handheld
David Pawliuk, Vice President, Exploration,
SILVER QUEST RESOURCES LTD., Vancouver, BC
“We acquired an Innov-X Omega XRF unit early in the 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

37. 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.

38. 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

39. 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 Closed
Lid Open

40. Introducing the original portable bench top X5000
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 X-5000 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

41. 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.

42. New X-5000 for Oils, Fuels & Liquids
Transportation
Power Generation
Petrochemical
Aerospace
Mining
Element
X-50
(ppm)
Wear Metals
Titanium
Chromium
Iron
Nickel
Copper
Lead 10 3 1
Fuels, Additives Analysis
Sulfur
Calcium
Vanadium Zn
Molybdenum
Barium
500 30 5 20
Other Applications
Hg, in aqueous solns
P, in aqueous solns
Cl, in process fluids
1000
200
Rapid on-the-spot elemental analysis for oils, fuels and other liquids
Unique fluid handling system
Uses 50 KeV tube, 10 Watt power rating

43. Flexibility in application
Easily test liquids, soil bags, metals and core.

44. 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 turn-around time.”

45. The Essential Mobile GIS Solution for Real-Time FPXRF
Delta Xplorer System
A Total Field Data Collection Solution Consisting Of:
Ruggedized Innov-X Systems Delta Portable XRF Analyzer
Ruggedized TRIMBLE NOMAD or YUMA Field Computer with built in GPS +/- Optional High Accuracy DGPS
ESRI ArcPAD or ENCOM Discover Mobile – Field Mobile GIS Integration Package
Mobile GIS extension software – Bluetooth communication software between Delta XRF, Trimble GPS and GIS software.
The Essential Mobile GIS Solution for Real-Time FPXRF

46. Delta Xplorer Overview

47. In-field example: Tritton Cu NSW
Nominal 50m x 50m Sample Grid Designed
Actual Sample Location Taken By DGPS
Sample Chemistry Registered Real-Time

48. Xplorer Workflow Xplorer - Simplified Workflow:
Innov-X Delta & TRIMBLE Nomad are Bluetooth paired for Communications
Mobile GIS started on Trimble Nomad
Soil Readings taken outside in open air & Result Received on Nomad
GPS Position Confirmed on finalization of result
Data is exported from Trimble Nomad
to Mapinfo or ArcPad
to ioGAS
Data presented graphically in Parent GIS

49. Delta Xplorer - Output

50. Delta Xplorer - Output Google Earth Export From ioGAS WGS84 Locations
Full Chemistry
from FPXRF
Google Earth Export
From ioGAS

51. Thank you 1201 W. Georgia St, Suite 2 Vancouver , BC V6E 3J5 CAN
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VANCOUVER
1201 W. Georgia St, Suite 2
Vancouver , BC V6E 3J5 CAN T F W.
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