RAW MATERIALS XRF APPLICATION USING A

Transcription

1 RAW MATERIALS XRF APPLICATION USING A UNIVERSAL BORATE FUSION METHODOLOGY Anne-Catherine Breton, Mathieu Bouchard, John Anzelmo and Sébastien Rivard Corporation Scientifique Claisse, Québec, Canada Corporation Scientifique Claisse, All Rights Reserved.

2 2 21 ST 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

3 3 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

4 4 PRESSED 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

5 5 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 simpler and flexible

6 6 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.

7 7 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

8 8 THE EQUIPMENT USED Muffle Furnace: Automatic Fluxer: Spectrometer: - Fisher Scientific Isotemp Programmable - Max. Temp.: 1125 C - Power: 50/60 Hz 208/240 VAC - Claisse M4 or TheOx Fluxer - Bruker S4 Explorer - WDXRF - Tube: 1000 Watts

9 11 THE EQUIPMENT USED - FLUXER Automatic Gas Fluxer: Automatic Electric Fluxer: - Claisse M4 TM Fluxer - Propane/Air Heating - 3 Positions - Claisse TheOx TM Fluxer - Electrical Heating - 6 Positions

10 10 CEMENT AND RAW MATERIALS FUSION METHOD Ignition: Necessary for All Cement related and Raw Materials 950 o C for 1 hour Crucible: Claisse Optimix crucible, Pt-Au alloy (95%-5%) Mold: 32mm Pt-Au alloy (95%-5%) Flux: Li 2 B 4 O 7 / LiBO % / 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

11 12 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

12 12 CALIBRATION STANDARDS RM element concentration as an oxide equivalent

13 13 Easy to fuse MATERIAL TYPES Not included in this analytical process 1) Copper Slags 2) Other samples with copper at higher level than traces 3) Some Iron Ores

14 14 CALIBRATION Inter-element corrections and squarred correlation coefficients for raw materials application

15 15 SENSITIVITY, PRECISION AND ACCURACY RESULTS Raw Materials application results

16 16 CONCLUSION Borate fusion allows to developed a robust and universal sample preparation method which is able to fuse the large range of raw materials and cements It is possible to obtain a precise and accurate universal calibration, able to cover a wide range of raw materials Precise and accurate results can be obtained using both type of fluxers: TheOx or M4.

17 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! Corporation Scientifique Claisse 2012, All Rights Reserved.