Metal Analysis & Quality Control at the point of -

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  • Jun 18, 2015
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1 Abstract No. 59 Metal Analysis & Quality Control at the point of Manufacture: The Evolution of the 15 Modern Handheld XRF & its Uses in the Steel Industry. EsaNUMMI,ThermoScientificPortableAnalyticalInstruments Handheldxrayfluorescence(HHXRF)analyzershavebecomethestandardfornondestructive qualitycontroltestingofferrousandnonferrousalloyproducts.Thesesystemsareroutinely utilizedforrapidqualitycontrolinspectionandanalysistoensureproductchemistry specificationsaremet.Likemostscientifictechnologies,XRFinstrumentshaveevolved 20 dramaticallyoverthelastfortyyearstoharnessminiaturizationandcomputeradvancements andtomeetincreasingdemandsfromtheindustry. Mostrecently,theintroductionofnewproprietarylargeareasilicondriftdetectors(SDD)into HHXRFinstrumentshasproducedsignificantperformanceimprovementsovertraditionalXRF capabilities.Asaresult,ahandheldXRFcannowbeusedfortheanalysisoftrampelementsin productionfacilitiesandultralowresidualelementdetectioninspecializedinspectionwork. Coupledwithahighoutput,50kV,miniaturizedxraytube,themodernhandheldXRFsystem canalsoperformlightelementanalysisworkwithoutvacuumorheliumpurge.Silicon,sulfur andphosphorousandotherlightelementscanbemeasuredinsteelalloysdirectly,withlittleif S anysamplepreparationnecessary.ThispresentationwillofferanexplanationoftheXRF techniqueandtheevolutionofHHXRFsystems.Performanceconsiderationsandspecificsteel applicationswillbeexplored. TA CE

2 15 CETAS 2015 9th International Conference Progress in Analytical Chemistry & Material Characterisation in the Steel and Metal Industries Metal Analysis & Quality Control at the point of manufacture. The evolution of the modern handheld XRF and its uses in the steel industry 20 Dusseldorf, Germany May 19-21, 2015 Esa Nummi Thermo Fisher Scientific The world leader in serving science 1 S Presentation Outline TA Portable Analytical Instruments Handheld X-ray Fluorescence (XRF) Handheld XRF Metal analysis Metals application examples CE 2

3 Thermo Scientific Portable Analytical Instruments 15 Industry Trend Increasingly, the lab is moving to the field Our Strategy If you take a product thats historically been large, expensive and complicated to use and you make it small, affordable, rugged and easy-to-use, you can dramatically expand your addressable market 20 Our Solution Deliver traditional laboratory quality testing results to the palm of the operators hand, giving our customers low-cost, reliable, real-time results and transforming the way they do business 3 S Thermo Scientific Portable Analytical Instruments TA Regulatory Metal Alloy ID Lead paint, Recycling, PMI, environmental, fabrication, consumer product safety QC/QA (lead in toys) Safety & Security Explosives identification, CE unknown threat screening Accelerating Lab to Field Pharma/Chem Raw Material ID, counterfeit drugs Food/Feed/Ag Moisture, fat, protein Mining for feed producers Narcotics Exploration, ore New application Crime scene grading, ore trading Developing Markets investigation, local police. 4

4 15 Basics of Handheld XRF 5 20 S Brief History Of Field Portable XRF TA 1960s 1998 2001 2008 CE First Multiple isotope 35kV X-ray tube 50kV X-ray tube commercial sources Ergonomic Silicon drift field portable Improved Si- pistol type detector XRF PIN detector design Light element Isotope based Pre-installed Si-PIN detector capability without Non-dispersive alloy calibration Multiple He or Vacuum scintillation applications detector No calibrations 6

5 Evolution of Handheld XRF Performance 15 Introduction of new technologies rapidly changed the HHXRF Modern electronics SDD-detector Mini X-ray tube Silicon drift detectors 20 (SDD) X-ray tube 7 S Handheld XRF Technology TA CE 8

6 Working Principle Of Handheld XRF 15 9 20 S From Spectra To Results TA CE 10

7 Handheld XRF Total Element Range 15 11 20 S Some Handheld XRF Applications TA Precious metals Oil and Gas Fabrication CE Scrap sorting Mineral Exploration Art and Conservation Mining Lead in paint Heavy metals 12

8 15 Metal Applications 13 20 S Metals Cycle Overview TA CE 14

9 HHXRF solutions for steel industry Scrap Raw material Sorting of incoming scrap raw material. Identification of tramp elements to ensure 15 correct melt chemistry Metal production Fast, on-the-spot analysis of melt charge material Slag and ferro alloy analysis Nondestructive chemistry and grade 20 verification Coating thickness / Coating weight On-the-spot coating thickness analysis directly from finished product, sheet or coil Hot dip galvanizing, Electrolytic Zinc-Iron coating. 15 S Analytical Capabilities TA Iron and C-steels Low alloy steels (LAS) Cr-Mo Steels (Cr-Mo) Ferrous Metals High alloy steels (HAS) Iron-based matrix Stainless steels (SS) Duplex & Super Duplex Tool steels (TS) Specialty steels Superalloys CE Ni alloys Ni-Co alloys Co alloys Ti alloys Non-Ferrous Al & Mg alloys (white metal) Metals Exotic alloys (W, Ta, Hf, Zr) Non iron matrix Precious metals (Au, Ag) Cu alloys Brass, Bronze, Cupro-nickels Red & Yellow metals 16

10 Analytical Performance For analytical performance both Precision and Accuracy are 15 important. Limit of detection (LOD) is the estimate of the smallest concentration which can be detected. LOD depends on element, measurement time and sample matrix. Typical LOD varies from 5 ppm to 20 1000ppm depending on element (1000ppm = 0.1%) Precision and LOD can be improved by extending the measurement time. STDEV=f (SQRT(T)). 17 S Handheld XRF Limitations TA XRF Element Range Almost all elements used in metal alloy production can be seen with portable XRF. The main limitation is carbon (C), which portable XRF cannot see. Other elements that XRF cant detect include Boron, Nitrogen, Lithium XRF is surface measurement CE XRF penetration depth depends on element of interest and material density In metal analysis, typical penetration depth is less than 50um (0.05mm) Measurement depth of selected elements in SiO2 and Fe matrix. 18

11 Sample forms and shapes Recycled metal is often in all shapes and forms. 15 Handheld XRF analyzer can automatically correct results for size, shape, curvature and distance. Modern HH-XRF can measure all sample types effectively. Turnings Powders 20 Mesh and wires Drill bits Slags and ferro-metals Welds and weld rods 19 S TA Application Examples CE 20

12 Alloy sorting Close grade specifications Excellent accuracy and precision 15 is required to separate many close grades, such as Nickel superalloys Modern handheld XRF instruments can separate many close grades, such as SS303 / SS 304 (1.4305 / 1.4301) Users can add their own grade 20 definitions or modify existing grade limits. 21 S Weld analysis TA The integrated color CCD camera & small spot, built into the nose of the analyzer Allow the user to View a live picture of the analysis area, Save the image along with the elemental analysis results and CE spectra. Accurate small spot analysis helps to ensure correct weld composition. 22

13 Tramp and Trace Element Analysis Scrap selection is complicated by the wide variety of steel products. For instance deep drawing steels 15 limit the maximum residual (%Cu +%Sn + %Ni +%Cr +%Mo) content to less than 0.13%. In conventional stainless steel making, Phosphorus is a most undesirable element since it makes the alloy brittle. Typical penalty level for P is 0.035%, The common stainless steel problem today is the increasing Cu content. Steel plants get penalty 20 fees if the concentration of Cu is more than 0.5%. Other tramps include S, Sn, Sb, As, Zn and Pb. Modern SDD detector based handheld XRF is able to measure all of these tramp elements. 23 S Slag analysis TA During the fluxing process, slags remove the non- ferrous constituents from the molten iron, which purifies the product. Slags are composed primarily of silica and lime, alumina, magnesia, and other compounds. Traditionally, slag analysis was done by taking a sample from the furnace and analyzed using a laboratory XRF. Handheld XRF can bring analysis closer to the CE furnace saving cost, time, and improve productivity. 24

14 XRF Coating thickness principle X-rays penetrate through the Zn layer and into the Fe substrate generating Zn and Fe X-ray signals 15 As the Zn layer gets thicker, the Zn intensity increases as more Zn X-rays are generated. Eventually, intensity becomes insensitive to thickness as Zn X-ray signals from greater depths are absorbed within the thick Zn layer itself. 25 20 S Steel passivation coating weight measurement TA Passivation coating layer protects galvanized steel rolls during the transport and storage New coatings are replacing Cr IV Coating contains typically Cr, Ti, P and sometimes also Si. Continuous strip plating process can be stopped, which enables HH-XRF measurements directly from the coil after the drying. CE Typical Zr thickness 26

15 Summary Handheld XRF is a fast and reliable tool for on-site alloy 15 identification and analysis Handheld XRF can analyze most alloy types and identify hundreds of different alloy grades Modern handheld XRF analyzers are versatile analytical tools which can be used for wide variety of applications such as slag, ferro alloy and coating weight analysis 27 20 S TA Thank You! CE Esa Nummi [email protected] +358 50 594 0536 28

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