An Introduction to Portable XRF for Exploration, Mining and Geochemistry Applications

An Introduction to Portable XRF for Exploration, Mining and Geochemistry Applications

Scott Curry & Cindy CollinsInnov-X Canada

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

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 ConceptsFundamental 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 semi-quantitative to quantitative data sets.

Sample Applications

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

Energy Dispersive XRF

Energy Dispersive XRF

Energy Dispersive XRF

Energy Dispersive XRF

EDXRF Spectral CaptureSpectra from Contaminated Soil Sample

0

2

4

6

8

10

12

5 10 15 20 25 30

Energy (KeV)

Inte

nsi

ty (C

ou

nts

per

sec

on

d)

Fe Ka

Fe Kb

Cu Ka

Zn Kb

Tube Lines and scatter from sample

Pb La Pb Lb

Rb Ka

Sr Ka

Mo Ka

Example of export format (csv file)

ApplicationsApplications

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 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

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

• 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 TipsSampling, Project Planning and Tips

•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

XRF Sampling and Planning

•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

XRF Sampling – Tips in the field

• 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!

Which Horizon?

• 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

Sampling Considerations

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 PreparationMg Andesite

(In Situ)

Soil SampleSieved to 250

micron

5 mm

5 mm

Sample Method

• 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!

Addressing Issues

• 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

Key Points to Remember

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

Adding Value to XRF Data

Innov-X - Choosing an AnalyzerInnov-X - Choosing an Analyzer

Innov-X Systems Existing Products

Introducing the handheldIntroducing the handheld

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.”

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 TechnologyPIN = Older Silicon PIN Detector – as used in Alpha

• 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

Portable Test Stand for Handhelds

Introducing the original portable bench top

X5000

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!”

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.

Element X-50 (ppm)

Wear Metals

TitaniumChromiumIronNickelCopperLead

1031111

Fuels, Additives Analysis

SulfurCalciumVanadiumZnMolybdenumBarium

500305

102020

Other Applications

Hg, in aqueous solnsP, in aqueous solnsCl, in process fluids

101000200

• Transportation• Power Generation• Petrochemical• Aerospace• Mining

• Rapid on-the-spot elemental analysis for oils, fuels and other liquids

• Unique fluid handling system• Uses 50 KeV tube, 10 Watt power rating

New X-5000 for Oils, Fuels & Liquids

Flexibility in application

Delta Xplorer System

Seamless XRF/GPS/GIS/ Geochemical Analysis Integration

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.”

Delta Xplorer SystemA 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

Delta Xplorer Overview

Nominal 50m x 50m Sample Grid Designed

Sample Chemistry Registered Real-Time

Actual Sample Location Taken By DGPS

In-fieldIn-field example: example: Tritton Cu NSWTritton Cu NSW

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

Xplorer Workflow

Delta XDelta Xplorer - Outputplorer - Output

Google Earth Export

From ioGAS

WGS84 Locations

Full Chemistry from FPXRF

Delta Delta Xplorer - OutputXplorer - Output

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

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