- Basics of XRF - Case Studies in XRF - Future Advances in XRF For more information, visit: https://www.olympus-ims.com/en/vanta/#!cms[tab]=%2Fvanta%2Fapplications

1. 1
Nontraditional Applications of XRF
for Quality Assurance and Quality
Control
XRF beyond Alloy PMI
Olympus
ASNT | Houston | 29 October 2018
Michael W. Hull, PhD | Applications Scientist

2. Future Advances in XRF
Basics of XRF
Case Studies in XRF
Pipeline of this Talk

3. Basics of XRF
Pipeline of this Talk

4. XRF Physics
Grade MatchingCalculationMeasurementRe-EmissionExcitationX-Ray Emission
Mn
FeNi
Cr

5. Grade Matching Process

6. XRF Physics
Grade MatchingCalculationMeasurementRe-EmissionExcitationX-Ray Emission
Mn
FeNi
Cr

7. XRF Physics
Grade MatchingCalculationMeasurementRe-EmissionExcitationX-Ray Emission
Mn
FeNi
Cr

8. XRF Physics
ChemistryCalculationMeasurementRe-EmissionExcitationX-Ray Emission
Mn
FeNi
Cr

9. Thinking Beyond PMI to QA/QC

10. XRF: An Elemental Science
Image Source: Library of Congress - http://loc.gov/pictures/resource/cph.3b12511/
Dalton’s Atomic Theory
• All matter is made of extremely tiny particles called atoms
• All atoms of a given element are identical to one another
• Atoms cannot be divided, created, or destroyed
• Atoms of different elements combine in simple, whole-
number ratios to form various chemical compounds
• In chemical reactions, atoms can be combined, separated,
or rearranged, but neither created nor destroyed
Atoms make up everything…
…so what’s the signature element?

11. • Element
• “Compound”
• Ratio
• Mathematical function, ƒ(E1, E2, En)

12. Basics of XRF
Case Studies in XRF
Pipeline of this Talk

13. 1. E.g. composite decking, solid-
surface countertop, or sink basin
2. Variegated material
3. Goal: Batch consistency for resin &
filler material, color, etc.
Case #1: Composite Building Material

14. Case #1: Composite Building Material
0% 10% 20%

15. Case #1: Composite Building Material

16. Proxy values
Case #1: Composite Building Material
Grit%
Loading Level

17. QA/QC Principle #1: Representative Sampling
• Multiple tests (6x, 2–3 secs)
Case #1: Composite Building Material

18. QA/QC Principle #2: Consistency in Testing
• Multiple tests (6x, 2–3 secs)
Case #1: Composite Building Material
Align to Corner

19. QA/QC Principle #1: Representative Sampling
• Multiple tests (6x, 2–3 secs)
• Panning test (10–12 seconds)
• Inline integration
Case #1: Composite Building Material

20. • Silver nanoparticles have antimicrobial properties
• Commonly applied to fabric and garments
• Loading & retention
Case #2: Antibacterial Fabric Sample
Ag Conc.
(ppm)
Precision
(+/-)
LB4 7.4 0.6
LB4 6.1 0.5
LB4 6.1 0.5
LB4 6.4 0.5
Average 6.5 ppm
TH 2.7 0.6
TH 3.1 0.6
TH 2.8 0.6
TH 2.9 0.6
Average 2.9 ppm
0001 0055 A 2.1 0.5
0001 0055 B 2.2 0.5
0001 0055 C 1.6 0.5
0001 0055 D 1.5 0.5
Average 1.9 ppm
0002 0055 A 10.2 0.5
0002 0055 B 7.4 0.5
0002 0055 C 6.2 0.5
0002 0055 D 11.6 0.5
Average 8.9 ppm
0003 0055 A 3.1 0.5
0003 0055 B 1.5 0.4
0003 0055 C 1.6 0.4
0003 0055 D 2.2 0.5
Average 2.1 ppm

21. • Fuel cells provide clean energy from hydrogen
• Platinum serves a central catalytic role
• Catalyst membranes are loaded with colloidal platinum
• Integration into production line
Case #3a: Coatings — Fuel-Cell Membrane

22. Location Pt (mg/cm
2
)
Origin 0.428
QI 0.431
QII 0.434
QIII 0.441
QIV 0.443
• Coatings often show loading
variations across the surface
• QA/QC Principle #3:
Instrument precision should
exceed process variation
Case #3a: Coatings — Fuel-Cell Membrane
QIQII
QIII QIV
O
Process Variation

23. • Coating weight is
related to dwell time
in the coating bath
Case #3b: Coatings – Ceramics

24. Goldilocks Principle: Not too much, not too little!
QA/QC Principle #4:
Don’t waste the expensive stuff!
Case #4: “Active” Ingredient – Formulation Control

25. • Additives affect plastics
properties
• Pigments/color intensity
• XRF is tied to sample
density
Case #5: Plastics Additive
Reading # Test Label Bi Conc ±σ Nb Conc ±σ Sb Conc ±σ S Conc ±σ
1 1-RP1 <LOD 0.0186 0.0003 0.0000 <LOD 0.0460 0.0347 0.0013
1 1-RP2 <LOD 0.0180 0.0003 0.0000 <LOD 0.0454 0.0349 0.0013
1 1-RP3 <LOD 0.0181 0.0003 0.0000 <LOD 0.0461 0.0310 0.0013
1 1-RP4 <LOD 0.0185 0.0003 0.0000 <LOD 0.0455 0.0351 0.0013
1 1-RP5 <LOD 0.0186 0.0003 0.0000 <LOD 0.0457 0.0329 0.0013
1 1-RP6 <LOD 0.0183 0.0003 0.0000 <LOD 0.0458 0.0333 0.0013
Average <LOD 0.0184 0.0003 0.0000 <LOD 0.0458 0.0338 0.0013
3 3-RP1 19.4136 0.2550 0.0108 0.0008 0.0725 0.0016 5.0014 0.0657
3 3-RP2 19.1715 0.2517 0.0097 0.0007 0.0705 0.0016 4.9635 0.0652
3 3-RP3 18.9926 0.2524 0.0093 0.0007 0.0706 0.0016 5.1646 0.0687
3 3-RP4 19.7717 0.2644 0.0106 0.0008 0.0727 0.0017 5.1473 0.0689
3 3-RP5 18.6864 0.2429 0.0094 0.0007 0.0692 0.0015 4.9865 0.0648
3 3-RP6 19.1825 0.2551 0.0106 0.0007 0.0676 0.0016 5.1647 0.0687
Average 19.2331 0.2538 0.0102 0.0007 0.0708 0.0016 5.0613 0.0668
5 5-RP1 24.6089 0.3377 0.0043 0.0010 0.0722 0.0019 11.4055 0.1564
5 5-RP2 24.4812 0.3357 0.0048 0.0010 0.0718 0.0019 11.4309 0.1566
5 5-RP3 24.7353 0.3390 0.0047 0.0010 0.0731 0.0019 11.4474 0.1568
5 5-RP4 25.5074 0.3564 0.0039 0.0010 0.0763 0.0020 11.6307 0.1624
5 5-RP5 25.5384 0.3528 0.0059 0.0011 0.0800 0.0020 11.6592 0.1609
5 5-RP6 25.2726 0.3508 0.0049 0.0010 0.0773 0.0020 11.5855 0.1607
Average 24.9647 0.3443 0.0047 0.0010 0.0747 0.0019 11.5092 0.1586
Santoprene
Extruded Pellets
(loose)
Product (solid)

26. Case #6: Construction Aggregates – Materials Science
Image Source: Creative Commons, https://en.wikipedia.org/wiki/Limestone#/media/File:Limestone_Mines_at_Cedar_Creek.jpg
• Lime (stone) [CaO]
• Clay [(Al2Si2O5(OH)4]
• Iron-rich (Fe2O3)
Controls for Concrete Raw Materials
Lime Saturation Factor
!"# =
%&'
(2.8 ∗ "-'. + 1.2 ∗ 12.'3 + 0.65 ∗ #7.'3)
Alite [Ca3SiO5]
Belite [Ca2SiO4]

27. Case #6: Construction Aggregates – Materials Science
• Lime(stone) [CaO]
• Clay [(Al2Si2O5(OH)4]
• Iron-rich (Fe2O3)
Controls for Concrete Raw Materials
Lime Saturation Factor
!"# =
%&'
(2.8 ∗ "-'. + 1.2 ∗ 12.'3 + 0.65 ∗ #7.'3)
Image Source: Creative Commons, https://en.wikipedia.org/wiki/Limestone#/media/File:Limestone_Mines_at_Cedar_Creek.jpg
"9 =
"-'.
12.'3 + #7.'3
19 =
12.'3
#7.'3
Silica Ratio
Alumina Ratio
0. %

28. • Sulfur content
• Ash content
• Caloric value
Case #7: Coal Lifecycle – Energy Science

29. Case #7: Coal Lifecycle – Ash Content
Ash Content ∝ (Mg+Al+Si+P+S+K+Ca+Ti+Fe)

30. Case #7: Coal Lifecycle – Caloric Value
Caloric Value ∝ Ash Content

31. Case #7: Coal Lifecycle – Caloric Value
Caloric Value ∝ (Mg+Al+Si+P+S+K+Ca+Ti+Fe)

32. Alternative to fire assay
Fire assay is:
• Labor-intensive
• Time-intensive
• Energy-intensive
Case #8: Gold on Carbon

33. Future Advances in XRF
Basics of XRF
Case Studies in XRF
Pipeline of this talk

34. Advanced Testing
Wireless
Bluetooth®
Cloud
Connectivity
IoT
Manufacturing
4.0
Inline Testing
XRF Integrations What property do you want to measure?
What’s your signature element?

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Bluetooth SIG, Inc. and any use of such marks by Olympus Corporation is
under license.
Olympus is a registered trademark of Olympus Corporation.