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

1. Utilizing Handheld X-Ray Fluorescence
for In-Process Steel Slag Monitoring
Alex Thurston
Olympus Scientific Solutions Americas, Inc
Applications Engineering Manager

2. Overview
XRF Theory and Handhelds
Introduction to HHXRF Slag Analysis Application
Raw Data and Treatment
Data Regression and Verification
Other Considerations

3. XRF Theory
K
L
M

4. XRF Theory
Magnesium through plutonium detection

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. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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. 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. Other Considerations
Sample preparation
Data transfer from instrument to Operations/product
management system

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.