Introduction to Elemental Analysis by ED-XRF Justin Masone Product Specialist 3 June 2015
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1 Introduction to Elemental Analysis by EDXRF Justin Masone Product Specialist 3 June / 9
2 Shimadzu Corporation Established in Headquartered in Kyoto, Japan Ranked Top 5 Instrument Providers in the world by Chemical and Engineering News Offer broad range of analytical solutions and technologies 22 / / 389
3 Shimadzu Corporation Chromatography HPLC & UHPLC GPC GC Mass Spectrometry LCMS GCMS MALDI Nexera UHPLC Environmental Analyzers Total Organic Carbon Total Nitrogen Total Phosphorus Spectroscopy MALDITOF/TOF TQ GCMS8030 UVVisNIR FTIR Fluorescence AA ICP TQ LCMS / / 389
4 Shimadzu Corporation Physical Measurement Tensile/Universal Hydraulic Concrete Fatigue Hardness Static/Dynamic Jack Impact Particle Size Analyzers Thermal Analyzers HighSpeed Video Camera Xray XRD XRF EDX DSC Analytical Balance Hardness Balances & Scales 44 / / 389
5 What is XRF? Analytical method to determine the elemental composition of many types of materials Can be used to determine the thickness and composition of layers, coatings, and platings. Fast, accurate, nondestructive Requires minimal sample prep Samples can be in solid, liquid, powder, or filtered form 55 / / 389
6 What is EDXRF? EnergyDispersive XRay Fluorescence Energydispersive: Ability to discern the energies of xrays XRay: Form of energy; source of ionizing radiation Fluorescence: Phenomenon of absorbing energy (short λ) and subsequently emitting energy (longer λ) 66 / / 389
7 Basis of EDX Data Processing Unit Irradiating Xrays Fluorescent Xrays 2 3 Preamp/DPP 5 77 / / 389
8 What are XRays? Xrays are a kind of electromagnetic energy: nm kev Hard Xrays: >10 kev Soft Xrays: <10 kev 88 / / 389
9 How Do XRays Interact with Matter? When Xrays strike matter, some of them are absorbed and some pass through Absorption and penetration depend on the elemental composition, density, and thickness of matter. A consequence of absorption is that secondary Xrays are generated, which are characteristic of that matter: 99 / / 389
10 How Do XRays Interact with Matter? / / 389
11 How Do XRays Interact with Matter? Degree of fluorescence depends on: Thickness Density Sample material Xray penetration depth (RhKα; ~20 kev): Pb Fe H 2 O 25 μm 200 μm 3 cm / / 389
12 How Do XRays Interact with Atoms? Irradiating Xray Ejected Electron Fluorescent Xray / / 389
13 Types of Transitions These are Characteristic Xrays / / 389
14 Energy of XRays: Example Fe atom E = hc λ = ( kev s) ( nm s) nm = 6.40 kev Kα / / 389
15 Energy of XRays: Example / / 389
16 EDX Spectrum / / 389
17 EDX Data Output List of elements present, including carbon as a balance Amount present in sample; can be reported in various units Type of analysis Transition used for quantitative calculation / / 389
18 Analytical Range / / 389
19 EDX System Collimator Sample Filters Xray tube CMOS camera Detector (SDD) / / 389
20 Why use EDX? Elemental analysis is traditionally done by AA/ICP This requires significant sample prep and cost of analysis is high With EDX, there is: Minimal to no sample prep (solvents, TDS, etc. are not a concern) Detection limits for heavy (high Z) elements 0.1 ppm Low cost of analysis in terms of both time and money No gas requirements No exhaust No sample waste Uses less bench space Easy to use / / 389
21 Example Applications Electrical/electronic materials RoHS and halogen screening Thinfilm analysis for semiconductors, discs, liquid crystals, and solar cells Automobiles and machinery ELV hazardous element screening Composition analysis, plating thickness measurement, and chemical conversion coating film weight measurement for machine parts Ferrous/nonferrous metals Main component analysis and impurity analysis of raw materials, alloys, solder, and precious metals Composition analysis of slag Mining Grade analysis for mineral processing Ceramics Analysis of ceramics, cement, glass, bricks, and clay Oil and petrochemicals Analysis of sulfur in oil Analysis of additive elements and mixed elements in lubricating oil Chemicals Analysis of products and organic/inorganic raw materials Analysis of catalysts, pigments, paints, rubber, and plastics Environment Analysis of soil, effluent, combustion ash, filters, and fine particulate matter Pharmaceuticals Analysis of residual catalyst during synthesis Analysis of impurities and foreign matter in active pharmaceutical ingredients Agriculture and foods Analysis of soil, fertilizer, and plants Analysis of raw ingredients, control of added elements, and analysis of foreign matter in foods Others Composition analysis of archeological samples and precious stones, analysis of toxic heavy metals in toys and everyday goods / / 389
22 Ti Ka Ti Kb Cr Ka Cr Ka Mn Kb Fe Kb Ni Ka Ni Kb Zn Ka Zn Kb Mo Ka Fe Ka Application: Foreign Matter Identification Analysis Example: Foreign Matter Adhering to a Plastic Extruded Part Sample Appearance Red circle: Foreign matter Blue circle: Clean area Foreign matter Clean area Matching Results Quantitative Analysis Results for Foreign Matter by FP Method (Ti and Zn are excluded from the quantitative calculations.) / / 389
23 Cr Ka Pb La Br Ka Pb Lb1 Sb Ka Sb Kb Ba Ka Application: Hazardous Substances in Products Analysis Example: Screening Analysis for 8 Controlled Elements in Toys Overall (Paint + plastic base material) Sample Appearance Scraped paint Plastic base material Overlaid Profiles of Measured Areas PE Resin Standard Samples Containing the 8 Controlled Elements in Toys / / 389
24 Application: Thin Films Analysis Example: Film Thickness and Composition Measurements of Electroless Nickel Plating Cu substrate Ni, P, Pb Primary Xray Fluorescent Xray Peak Profiles of Ni, P, and Pb Quantitative Analysis Results by Film FP Method / / 389
25 Application: Cement Analysis Example: Qualitative Analysis of Cement / / 389
26 Application: Cement / / 389
27 Application: Cement / / 389
28 Application: Cement / / 389
29 Application: Polymer Film Analysis Example: Determination of Thickness and Concentration Shimadzu s newlydeveloped Background FP method (BGFP) incorporates Xray scattering theory into the standard FP calculation Uses Compton scattering to determine thickness of a polymer film while simultaneously determining its constituent elements / / 389
30 Application: Polymer Film Scattered Radiation Some of the Xrays from the tube do not generate fluorescent X rays when they strike the sample. Instead, they are scattered within the sample. There are two types scattering radiation: Compton Scattering: When the source characteristic Xrays (Rh) that strike the material suffer from some energy loss (inelastic scattering) Rayleigh Scattering: When the source characteristic Xrays (Rh) strike the sample without any change in energy (elastic scattering) / / 389
31 Application: Polymer Film Compton scattering Rayleigh scattering The intensity of the Compton scattering is influenced by the material/density of the sample / / 389
32 Application: Polymer Film Samples with light elements give rise to high Compton scatter and low Rayleigh scatter This is because they have more loosely bound electrons With very heavy elements, the Compton scattering disappears completely / / 389
33 Application: Polymer Film / / 389
34 Application: Polymer Film / / 389
35 Application: Polymer Film / / 389
36 Application: Polymer Film / / 389
37 Application Notes Screening Analysis with EDX7000 Navi Software Quantitative Analysis of Elements in Small Quantity of Organic Matter by EDXRF New Feature of Background FP Method Quantitative Analysis of Cement by EDX8000 Quantitative Analysis of Waste Oil by EDX7000 TC Measurement and Elemental Composition Analysis of Fly Ash Quantitation by TOC and XRF Quantitative Analysis of Tin (Sn) in Plastics by EDXRF Analysis of Aqueous Solution by EDXLE Performance in Air Atmosphere Quantitative Analysis of Fluorine ( 9 F) by EDXRF Quantitative Analysis of Antimony (Sb) in Plastics by EDXRF Qualitative and Quantitative Analysis of Seafood by EDXRF EDXRF Analysis of Arsenic and Lead in Dietary Supplement QC Analysis of Magnesium Alloy Die Castings by EDXRF EDXRF Analysis of PM2.5 (Particle Matter) EDXRF Analysis of Sulfur and Other Elements in Oil EDXRF Analysis of Lead, Cadmium, Silver, Copper in LeadFree Solder Materials Determination of Arsenic and Lead in Earth and Sand Using EDXRF [JIS K 0470] Comparison of Calibration Curves of Lead, Cadmium and Chromium in Zinc Alloy and Copper Alloy EDXRF Analysis of Lead, Cadmium, Mercury and Chromium in Zinc Alloy EDXRF Analysis of Chlorine in Irregularly Shaped Plastic Samples Analysis of Foreign Matter in Food Using EDX EDXRF Analysis of Heavy Elements in a Toy and a Cup EDXRF Analysis of Chlorine in Plastic (PE) Materials Analysis of Sulfur in Oil Using Energy Dispersive XRay Fluorescence Spectrometer Analysis of Foreign Matter Using CCD EDXRF Analysis of Arsenic in Foods / / 389
38 Additional Information Additional Information: / / 389
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