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TRANSCRIPT
RAW MATERIALS XRF APPLICATION USING AUNIVERSAL BORATE FUSION METHODOLOGY
© Corporation Scientifique Claisse®, 2013. All Rights Reserved.
Anne-Catherine Breton, Mathieu Bouchard, John Anzelmo and Sébastien Rivard
Corporation Scientifique Claisse, Québec, Canada
21ST CENTURY INDUSTRY REALITY
• Raw Materials:– Natural ores and rocks– Use of industrial by-products– Not necessarily obtain from well
known sources
• Fuels: – Less expensive fuel and waste
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LAB MANAGERS REALITY
• Analyze a very wide range of sample types(raw materials, in process samples, final products)
• Meet requirements of standard test methods
• Laboratory operators and/or technicians with limited scientific background
• Limit cost of analysis– Need safe, simple and efficient analytical methods– Need to limit the sources of manipulation errors– Need to limit the use of reference materials and/or pure
oxides
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4PRESSED POWDERS FOR XRF
Pressed pellets can generate good accuracy only when:
• A distinct calibration curve is made for every type of matrix
• Standards that match exactly the unknown samples for particle size and mineralogy are available
• Grinding and pressing conditions are optimized and rigorously repeated
• The standards and the samples can be ground enough to reduce the particle size effect significantly
• The pellets are stable enough (use of binder) to avoid causing cross-contamination
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FUSION FOR XRF
• No particle effect
• All elements transformed into simple oxides
• No mineralogical effect
• All standard and unknown specimens have the same matrix which is a borate glass
• Calibration is much simplerand flexible
MATERIAL TYPES
• Cement• Blended cement• Cement with additions• Aluminate cement• Clinker• Kiln feed• Raw Mix• Limestone
• Gypsum• Sand• Clay• Bauxite• Silica Fume• Slag• Fly ash• Iron Ore
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DEVELOPMENT OF THE GLOBAL FUSION METHOD
• 200 different samples from 14 material types
• Both ignited and non ignited samples
• 3 different sample:flux ratios
• We tried different dry oxidation methods
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THE EQUIPMENT USED
Muffle Furnace:
- Fisher ScientificIsotemp® Programmable- Max. Temp.: 1125°C- Power: 50/60 Hz 208/240 VAC
Spectrometer:
- Bruker S4 Explorer- WDXRF- Tube: 1000 Watts
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Automatic Fluxer:
- Claisse M4 or TheOxFluxer
THE EQUIPMENT USED - FLUXER
Automatic Electric Fluxer:Automatic Gas Fluxer:
- Claisse® M4TM Fluxer- Propane/Air Heating- 3 Positions
- Claisse® TheOxTM Fluxer- Electrical Heating- 6 Positions
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CEMENT AND RAW MATERIALS FUSION METHOD
• Ignition: Necessary for All Cement related and Raw Materials
950oC for 1 hour
• Crucible: Claisse Optimix crucible, Pt-Au alloy (95%-5%)
• Mold: 32mm Pt-Au alloy (95%-5%)
• Flux: Li2B4O7 / LiBO2 49.75% / 49.75% flux with integrated
LiBr non-wetting agent 0.50%
• Ratio: 1:10 sample to flux
• Mixing: 15 seconds on a vortex mixer
• Fusion time: 18 min. (including cooling) for M4 Fluxer
22 min. (including cooling) for TheOx
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CALIBRATION STANDARDS
• The calibration of the WDXRF raw materials application was executed using a wide variety of RMs
• Bureau of Analysed Samples Ltd. (BAS): British Chemical Standard Certified Reference Materials
• Domtar® Inc. Research Center: Canadian Certified Reference Materials• China National Analysis Center for Iron and Steel: NCS DC Reference Material• European Committee for Iron and Steel Standardization • European Coal and Steel Community (ECSC): Euro-Standard• Geological Institute for Chemical Minerals: GBW Reference Material• Institut de Recherches de la Sidérurgie (IRSID) : Échantillon-Type• Instituto de Pesquisas Tecnológicas (IPT) : Reference Material• Japan Cement Association (JCA): Reference Materials for X-ray Fluorescence
Analysis • National Institute of Standards & Technology (NIST): Standard Reference
Material®• Slovak Institute of Metrology (SMU): Slovak Reference Material• South Africa Bureau of Standards: SARM Certified Reference Material
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CALIBRATION STANDARDS12
RM element concentration as an oxide equivalent
MATERIAL TYPES
• Not included in this analytical process1) Copper Slags2) Other samples with copper at higher level than traces3) Some Iron Ores
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• Easy to fuse
14CALIBRATION
Inter-element corrections and squarred correlation coefficients for raw materials application
SENSITIVITY, PRECISION AND ACCURACY RESULTS15
Raw Materials application results
CONCLUSION
• Borate fusion allows to developed a robust and universalsample preparation method which is able to fuse the largerange of raw materials and cements
• It is possible to obtain a precise and accurate universalcalibration, able to cover a wide range of raw materials
• Precise and accurate results can be obtained using bothtype of fluxers: TheOx or M4.
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QUESTIONS AND COMMENTS
If you have questions, please feel free to ask me now or later at HRT Labortechnik’s booth.
Thank you for your attention!
www.claisse.com
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