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Utilizing Handheld X-Ray Fluorescence for In-Process Steel Slag Monitoring

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Presentation Outline:

- XRF Theory and Handhelds
- Introduction to HHXRF Slag Analysis Application
- Raw Data and Treatment
- Data Regression and Verification
- Other Considerations

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Utilizing Handheld X-Ray Fluorescence for In-Process Steel Slag Monitoring

  1. 1. Utilizing Handheld X-Ray Fluorescence for In-Process Steel Slag Monitoring Alex Thurston Olympus Scientific Solutions Americas, Inc Applications Engineering Manager
  2. 2. Overview XRF Theory and Handhelds Introduction to HHXRF Slag Analysis Application Raw Data and Treatment Data Regression and Verification Other Considerations
  3. 3. XRF Theory K L M
  4. 4. XRF Theory Magnesium through plutonium detection
  5. 5. Introduction to HHXRF Slag Analysis Application Initial Data (“Out of the Box”) Rapid tests used to gather data 20–30 seconds per test for this activity Multiple tests per sample Averaging used to generate initial data Accounts for sample variability
  6. 6. Introduction to HHXRF Slag Analysis Application Initial Data (“Out of the Box”)  Olympus Vanta™ VMR XRF analyzer used  GeoChem method (i.e. non-metallic sample)  Compound feature lets oxide forms display in results in real time  Iron displayed in elemental form due to the potential of various phases present (FeO, Fe2O3, Fe3O4)
  7. 7. Raw Data and Treatment Initial Data (“Out of the Box”)  Export-collected data for analysis Al2O3 Read Al2O3 Lab CaO Read CaO Lab MgO Read MgO Lab Cr2O3 Read Cr2O3 Lab SiO2 Read SiO2 Lab Fe Read Fe Lab 4.16 4.43 43.03 40.15 10.48 12.99 0.66 0.88 19.98 18.65 10.83 12.62 3.52 3.43 38.19 34.65 11.18 13.41 0.95 1.27 18.25 15.31 15.99 17.87 6.08 6.83 43.27 41.36 11.67 13.42 0.52 0.68 21.01 19.19 6.90 7.74 7.29 9.75 40.95 39.99 16.32 19.82 0.18 0.25 25.11 25.70 2.45 2.32 5.11 6.04 44.12 40.52 12.45 13.97 0.31 0.42 25.17 23.58 6.02 6.74 3.73 4.40 39.68 37.36 10.54 11.04 0.43 0.59 23.53 22.68 6.98 7.96 4.89 6.54 42.31 40.73 15.91 17.96 0.17 0.26 27.51 27.92 3.09 3.48 5.70 7.78 39.15 37.79 16.58 18.59 0.17 0.26 28.45 29.36 3.20 3.43 4.09 4.62 46.62 43.92 9.59 11.64 0.58 0.71 19.88 18.43 8.97 10.94 4.49 4.86 41.85 38.56 9.58 10.48 1.38 1.62 22.12 19.90 8.14 9.16 4.98 6.38 45.24 43.10 13.57 14.42 0.49 0.68 25.49 25.07 2.36 2.81 5.72 7.86 44.28 42.14 15.12 16.91 0.23 0.35 25.78 26.19 1.74 1.97 3.82 3.80 46.92 44.10 10.84 12.63 1.05 1.34 14.95 12.23 10.82 12.85 8.60 8.88 44.37 42.19 11.16 14.44 1.59 2.00 16.82 14.81 7.46 7.93 5.19 5.97 40.45 39.17 13.77 16.42 1.43 2.02 19.88 18.36 6.39 7.21 6.00 7.25 42.35 39.50 14.83 16.17 1.03 1.43 23.72 22.40 4.22 4.59 4.33 4.65 41.67 39.20 10.85 12.95 0.88 1.13 18.90 17.03 9.75 11.21 4.19 4.78 42.07 39.99 10.21 12.63 0.86 1.15 18.67 17.33 9.17 10.57 4.33 5.18 41.67 41.17 10.85 13.12 0.88 0.88 18.90 18.65 9.75 8.89 5.57 7.07 43.69 42.08 12.43 14.81 0.29 0.41 23.78 23.47 3.91 4.03 3.83 4.17 42.78 40.71 9.17 11.30 0.99 1.23 15.96 14.94 12.61 15.17 4.07 4.21 39.34 36.05 8.68 9.39 1.39 1.61 18.68 16.58 11.14 12.13 4.78 6.24 41.53 40.96 12.10 14.00 0.77 1.03 22.37 22.63 3.84 4.61 5.26 7.22 42.95 41.89 13.59 16.01 0.29 0.39 23.92 24.64 1.80 2.03
  8. 8. Raw Data and Treatment Initial Data (“Out of the Box”) Plot and analyze for trends y = 1.3499x - 0.7514 R² = 0.8557 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 Lab Vanta Al2O3 Al2O3 Lab Al2O3 Read Linear (Al2O3 Read) y = 0.9809x - 1.206 R² = 0.951 28.0000 33.0000 38.0000 43.0000 48.0000 28.0000 33.0000 38.0000 43.0000 48.0000 Lab Vanta CaO CaO Lab CaO Read Linear (CaO Read)
  9. 9. Raw Data and Treatment Initial Data (“Out of the Box”) Plot and analyze for trends y = 1.0954x + 0.4701 R² = 0.9352 0.0000 5.0000 10.0000 15.0000 20.0000 25.0000 0.0000 5.0000 10.0000 15.0000 20.0000 25.0000 Lab Vanta MgO MgO Lab MgO Read Linear (MgO Read) y = 1.2074x + 0.0761 R² = 0.9696 0.0000 0.5000 1.0000 1.5000 2.0000 2.5000 3.0000 3.5000 0.0000 0.5000 1.0000 1.5000 2.0000 2.5000 3.0000 3.5000 Lab Vanta Cr2O3 Cr2O3 Lab Cr2O3 Read Linear (Cr2O3 Read)
  10. 10. Raw Data and Treatment Initial Data (“Out of the Box”) Plot and analyze for trends y = 1.2422x - 6.4146 R² = 0.9558 5.0000 10.0000 15.0000 20.0000 25.0000 30.0000 35.0000 5.0000 10.0000 15.0000 20.0000 25.0000 30.0000 35.0000 Lab Vanta SiO2 SiO2 Lab SiO2 Read Linear (SiO2 Read) y = 1.1159x + 0.0982 R² = 0.9914 0.0000 5.0000 10.0000 15.0000 20.0000 25.0000 0.0000 5.0000 10.0000 15.0000 20.0000 25.0000 Lab Vanta Fe Fe Lab Fe Read Linear (Fe Read)
  11. 11. Raw Data and Treatment Data Analysis for Sample Configuration Alignment of experimental data to lab values Large data set is helpful to understand trends Trendlines for Al2O3, CaO, MgO, Cr2O3, SiO2, and Fe are all linear, but do not match lab values Trendline’s slope and intercept can be used to apply to software “user factors” Similar to type standardization in OES
  12. 12. Raw Data and Treatment Data Analysis for Sample Configuration Calculation of “User Factors” Example—Al2O3: y = 1.3499x - 0.7514  Factor is 1.3499. Offset is -0.7514/(1.889)= -0.3978. 1.889 is the mass balance multiplier to convert Al->Al2O3. Value is calculated in %; % conversion to ppm for UF is %/10000. y = 1.3499x - 0.7514 R² = 0.8557 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 Lab Vanta Al2O3 Al2O3 Lab Al2O3 Read Linear (Al2O3 Read)
  13. 13. Data Regression and Verification Apply and Test the Configuration Software can reprocess collected spectra much faster than taking new tests Apply User Factors and regression
  14. 14. Data Regression and Verification Apply and Test the Configuration Regressed results y = 1.0021x - 0.0752 R² = 0.953 28.0000 33.0000 38.0000 43.0000 48.0000 28.0000 33.0000 38.0000 43.0000 48.0000 Lab Read CaO - UF CaO Lab CaO Read Linear (CaO Read) y = 0.9809x - 1.206 R² = 0.951 28.0000 33.0000 38.0000 43.0000 48.0000 28.0000 33.0000 38.0000 43.0000 48.0000 Lab Vanta CaO CaO Lab CaO Read Linear (CaO Read)
  15. 15. Data Regression and Verification Apply and Test the Configuration Regressed results y = 1.0007x - 0.0029 R² = 0.8554 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 Lab Read Al2O3 - UF Al2O3 Lab Al2O3 Read Linear (Al2O3 Read) y = 1.3499x - 0.7514 R² = 0.8557 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 0.0000 2.0000 4.0000 6.0000 8.0000 10.0000 12.0000 Lab Vanta Al2O3 Al2O3 Lab Al2O3 Read Linear (Al2O3 Read) BEFORE AFTER
  16. 16. Data Regression and Verification Apply and Test the Configuration Regressed results y = 1.0065x - 0.1434 R² = 0.9578 10.0000 15.0000 20.0000 25.0000 30.0000 35.0000 10.0000 15.0000 20.0000 25.0000 30.0000 35.0000 Lab Read SiO2 - UF SiO2 Lab SiO2 Read Linear (SiO2 Read) y = 1.0004x + 0.0072 R² = 0.9346 5.0000 7.0000 9.0000 11.0000 13.0000 15.0000 17.0000 19.0000 21.0000 5.0000 7.0000 9.0000 11.0000 13.0000 15.0000 17.0000 19.0000 21.0000 Lab Read MgO - UF MgO Lab MgO Read Linear (MgO Read)
  17. 17. Data Regression and Verification Apply and Test the Configuration Regressed results y = 1.0021x + 0.0037 R² = 0.9728 0.0000 0.5000 1.0000 1.5000 2.0000 2.5000 3.0000 3.5000 0.0000 0.5000 1.0000 1.5000 2.0000 2.5000 3.0000 3.5000 Lab Read Cr2O3 - UF Cr2O3 Lab Cr2O3 Read Linear (Cr2O3 Read) y = 1.0036x + 0.0206 R² = 0.9948 0.0000 5.0000 10.0000 15.0000 20.0000 25.0000 0.0000 5.0000 10.0000 15.0000 20.0000 25.0000 Lab Read Fe - UF Fe Lab Fe Read Linear (Fe Read)
  18. 18. Data Regression and Verification Use In-Process Screenshot taken after test completion (15 seconds low-energy beam, 20 seconds total test time). Al2O3 Lab CaO Lab MgO Lab Cr2O3 Lab SiO2 Lab Fe Lab 7.22 41.89 16.01 0.39 24.64 2.03
  19. 19. Use In-Process Calculate basicity ratios in real time Ex. B3: CaO/(SiO2+Al2O3) Ex. B4: (CaO+MgO)/(SiO2+Al2O3) Software feature to use live results to calculate
  20. 20. Other Considerations Larger data set is helpful y = 1.186x - 7.8518 R² = 0.7655 38 39 40 41 42 43 44 45 46 47 48 38 40 42 44 46 48 Lab Vanta CaO y = 2.0668x + 1.2485 R² = 0.9788 0 2 4 6 8 10 12 14 16 0 2 4 6 8 10 12 14 16 Lab Vanta MgO
  21. 21. Other Considerations Larger data set is helpful – more points to strengthen the trendline y = 1.0011x + 0.0356 R² = 0.7657 38 39 40 41 42 43 44 45 46 47 48 38 40 42 44 46 48 Lab Vanta CaO - UF y = 1.0003x + 0.0002 R² = 0.9788 6 7 8 9 10 11 12 13 14 15 16 6 8 10 12 14 16 Lab Vanta MgO - UF
  22. 22. Other Considerations Sample preparation Data transfer from instrument to Operations/product management system
  23. 23. Thank you for your time! Questions? Alex Thurston Applications Engineering Manager Olympus Scientific Solutions Americas, Inc Waltham, MA, USA Olympus is a registered trademark, and Vanta is a trademark of Olympus Corporation.

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