1Scott Curry & Cindy Collins Innov-X Canada An Introduction to Portable XRF for Exploration, Mining and Geochemistry ApplicationsScott Curry & Cindy CollinsInnov-X Canada
2Presentation Outline Fundamental XRF Concepts and Sample Data Limitations of Portable XRFXplorer - Seamless XRF/GPS/GIS IntegrationSample ApplicationsSampling, Project Planning and Tips for XRFQuestions
3What can XRF do for reclamation? TailingsChemical disposalSoil and water contaminant analysis for mine site and perimeter monitoringProvide large inexpensive datasets continuously from environmental baseline data to clean up and monitoringBe an integral part of the mine reclamation planBe 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)
5What 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 locationAccurate - Can develop semi-quantitative to quantitative data sets.
7History of XRFFrom 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 todayEarly spectrometers were WDXRD measuring wavelength for one element at a timeWith 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 elementSubsequent improvement in detectors and signal resolution lead to measurement of several elements in one sampleEarly EDXRF use radioisotopes for excitation requiring recycling of a depleted radioactive source, recalibration and replacement at significant costsCurrent state-of-the-art EDXRF includes x-ray tubes, solid-state components, electronics, computers and softwareNow this mature technology is routinely used for R&D, QC, production support and regulatory compliance
15General Environmental Applications Mine reclamationEnvironmental baseline data over large areas with large inexpensive datasetsLiquid analysisPb paint analysisFilter analysisSoil and other materials
16Pb in soilsBlacksmith Institute working to limit Pb poisoning plaguing remote villages in NigeriaIn seconds the XRF analyzer identifies pollutant metals including Pb as low as 0.001%Remediation begins and processing procedures are altered to avoid a recurrenceThe EPA provides a recommended soil testing method for XRF, EPA Method 6200
17Hazardous Waste Screening Debris for hazardous or non-hazardous disposal in lieu of TCLP testing (toxicity characteristic leaching)Extreme weather debris migrationConstruction or demolition project wasteWaste streams and oil poolsIndustrial and mining process on community perimeters
18Property AssessmentImmediately identify heavy metals in soil at low ppm levelsReal-time metal screening at construction or disposal sites – Pb, U, RCRA, Priority PollutantsBrownfields Phase I/II/IIILead (Pb) clearance failure avoidanceTube-based Pb Paint AnalysisAirborne metals in mining, welding, construction, fabrication, maintenance and repair, paint removal and renovation
19Published SOP Methods EPA 6200 HUD PCS for testing Pb in Paint XRF soil testingHUD PCS for testing Pb in PaintNIOSH Method for Pb in filtersOSHA Method ID204Quantitative X-Ray Fluorescence Analysis of Workplace Substances ID204. (Air or wipe filter & bulk material)RWM-DR-025Metals in solid media
20Peer Reviewed Tech Articles Arsenic in Hurricane Katrina Wood DebrisDetermination of Br in Regulated FoodsDetermination of Soil Calcium Using FPXRFEvaluation of New XRF Instrumentation at Hazmat and Abandoned Mine Land Site – Hazardous MaterialsEvaluation of Portable XRF for Gypsum Quantification in SoilsEvaluation of Technologies for Sorting CCA-Treated WoodIdentification and mapping of heavy metal pollution in soilsIdentification through XRF of Dental Restorative ResinsPresence and Breakdown of BFRs in VehiclesReclaiming Military Bases from Tungsten TakeoverTriad Case Study: Former Small Arms Training Range
21CCA – Identify Toxin-Treated wood products Screen recycled wood mulch, pellets & other by-products for toxic metalsEPA compliance & label confirmation at wood treaters, lumberyards, retail centersScreen in-coming wood at municipal incinerators, landfills & recycling facilitiesDetermine effectiveness of protective coatings & sealants from CCA & other toxinsTest for arsenic leaching out of unlined landfills & around residential wood structures
22Lead InspectionLead Inspection :Classify definitive positive/negative results for Pb in secondsComply with restrictions on lead exposure during building demolition & constructionUse in manufacturing, homes or commercial buildings
23Innov-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 SecondsMeets OSHA Methods OSA1 & OSS1 and EPA Method 6200 and NIOSH Method 7702!In-situ Tests: Rapid, thorough site investigations, delineation and contamination patternsConfirm the minimally required samples to drive investigationAvoid confirmatory lab testing of high-concentration samplesEstablish area contamination boundaries and depth profilesDock into convenient testing stand for bagged or liquid samplesTest directly thorough corings for depth profiles
25XRF Sampling and Planning Clearly establish project & sampling objectivesDetermine the level of data quality required by XRF: fieldscreening or lab quality? Is it FIT FOR PURPOSE?Establish an appropriate procedure (test times, number oftests etc.)Correct & Appropriated Use of Calculation Modes (CN & FP)Always keep good records of Field WorkIncorporate QA/QC Protocols: Test relevant Matrix Matched Standards, Blanks & Field DuplicatesDispatch a proportion of samples for confirmatory analysis:min 5% up to 20% for checking calibrations25
26XRF 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 MaterialsPack extra batteries & Windows (Kapton or PP?) + Screwdriver to remove Window AssemblyInclude a soft lens cloth for cleaning the Window – always good to check the window after every analysis to remove contamination & inspect for damage/holesCarry necessary standards / blanks26
27Which 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 locationCommon 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!
28Sampling Considerations Remember, typical sample size is around 1cm2 – Collimated X-RAY Beam usually <3mm in WidthDepth of Penetration is generally limited to the surface of most samples – up to 2-5mm in very light Matrix samplesNeed 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 variation28
29Sample Preparation5 mmMg 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 homogeneityTake advantage of new portable & mobile field preparation devices – such as Rocklabs / Essa portable Crushers & MillsPotential to setup Miniaturized / Containerized sample prep facilities in the Field to support XRF Sampling programmesFor less homogenous samples – multiple readings & averaging can be effectiveDry the sample to take away moisture effectsSoil SampleSieved to 250 micron5 mm29
30Sample Method In-situ analysis with FPXRF Collect 50g of sample Split sample into two equal portions of at least 25g eachRe-analyze sample in the field using FPXRFStore sample for laboratory analysis (XRF, ICP-MS)Wash through a sieve to isolate the silt and clay sized fractionsRe-analyze using the FPXRF in the fieldStore for laboratory analysis (XRD, ICP-MS)
31Addressing IssuesProblem 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!
32Key Points to RememberFactors can adjust for matrix effects - Use LAB data to verify chemistry and correct via the User Factor setCan also use Matrix Matched certified standards to correct factors if the matrix is consistentChemistry results are only from what the X Rays see. Beware of homogeneity and surface effects.Longer Tests = better precision within limits32
33Adding 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 ValidationIncorporate Standards, Blanks, Field Duplicates and Check Samples to increase your understanding & confidenceRank & Store the Data in a well ordered & structured DB
36Introducing 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
37New Delta Handheld XRFLaunched 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 BriefSmaller / Faster / Cooler / TougherUpgradeableTube 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 possibleAdd innovations as appropriate and make expandable and adaptable.
38Delta Handheld XRF Product Models Premium Vacuum (for low level Mg)Large Area SDD and vacuum.PremiumLarge Area SDD detectorStandardTypical SDD DetectorClassicPIN diode detectorRange of tube anode materials availableSDD = New Silicon Drift Detector TechnologyPIN = Older Silicon PIN Detector – as used in Alpha
39Portable Test Stand for Handhelds Portable Test Stand for the Omega and DeltaAllows use of the Handheld like a bench top to obtain maximum flexibility, in field or fixed in camp or labCan be operated from laptop computerLid ClosedLid Open
40Introducing 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
41New 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.
42New X-5000 for Oils, Fuels & Liquids TransportationPower GenerationPetrochemicalAerospaceMiningElementX-50(ppm)Wear MetalsTitaniumChromiumIronNickelCopperLead1031Fuels, Additives AnalysisSulfurCalciumVanadiumZnMolybdenumBarium50030520Other ApplicationsHg, in aqueous solnsP, in aqueous solnsCl, in process fluids1000200Rapid on-the-spot elemental analysis for oils, fuels and other liquidsUnique fluid handling systemUses 50 KeV tube, 10 Watt power rating
43Flexibility in application Easily test liquids, soil bags, metals and core.
44Delta 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.”
45The Essential Mobile GIS Solution for Real-Time FPXRF Delta Xplorer SystemA Total Field Data Collection Solution Consisting Of:Ruggedized Innov-X Systems Delta Portable XRF AnalyzerRuggedized TRIMBLE NOMAD or YUMA Field Computer with built in GPS +/- Optional High Accuracy DGPSESRI ArcPAD or ENCOM Discover Mobile – Field Mobile GIS Integration PackageMobile GIS extension software – Bluetooth communication software between Delta XRF, Trimble GPS and GIS software.The Essential Mobile GIS Solution for Real-Time FPXRF
47In-field example: Tritton Cu NSW Nominal 50m x 50m Sample Grid DesignedActual Sample Location Taken By DGPSSample Chemistry Registered Real-Time
48Xplorer Workflow Xplorer - Simplified Workflow: Innov-X Delta & TRIMBLE Nomad are Bluetooth paired for CommunicationsMobile GIS started on Trimble NomadSoil Readings taken outside in open air & Result Received on NomadGPS Position Confirmed on finalization of resultData is exported from Trimble Nomadto Mapinfo or ArcPadto ioGASData presented graphically in Parent GIS