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Grade Verification and Compositional Analysis
Using On-Line XRF as Part of 100% Inspection
Joel Kenyon
Olympus Scientific Solutions Americas
Global Product Manager
Overview
ö100% testing
öX-ray fluorescence (XRF)
öThe FOX-IQ® on-line XRF analyzer
öTest procedure
öResults
öConclusions
öQuestions
Introduction
öA single manufacturer can produce hundreds of different alloy
grades
öMixes have consequences
− Aerospace, oil and gas, automotive, etc.
ö100% inspection is ideal but not realistic without automation
öAutomated NDT systems already in use as part of 100%
inspection protocols (visual inspection, eddy current, etc.)
öXRF can be a part of this as well
X-ray Fluorescence
öFluorescence = radiation
absorbed and re-emitted at a
different energy level
öX-ray fluorescence (XRF)
− Illuminate sample with X-rays
− Ionization occurs
− Characteristic X-rays emitted
− Characteristic X-rays used to
determine chemistry
Ni
Fe
Cr
Mo
X-ray Fluorescence
öWidely accepted technique for positive material
identification (PMI)
− Benchtop
− Handheld
The FOX-IQ XRF Analyzer
öFactory On-line XRF
− 40 kV X-ray source
− Silicon drift detector
− Factory installed grade library (400+ grades)
− Automated (PLC) or manual (PC) operation
The FOX-IQ XRF Analyzer
öElements visible with the FOX-IQ analyzer
Test Procedure
öTwo questions:
− Can the FOX-IQ analyzer successfully identify and
differentiate the grades of interest?
− How accurate/precise is the instrument?
öPass/fail analysis with chemistry done manually
öMatch cutoff set to 5 (default)
− Match number closer to 0 = better match
− Match cutoff = highest match number that can pass
öTen repeat tests, 3 seconds each
Test Procedure
öSamples: 6 CRMs
− Tested in pairs
according to base
− Already in library
− All contain
molybdenum (Mo)
Grade Name Manufacturer Batch Number
304SS ARMI IARM 162D
316SS ARMI IARM 5D
2.25Cr 1Mo Brammer BS 46A
C 0.5Mo ARMI IARM 229B
Hast C276 Brammer BS H2C
Monel K500 Brammer BS 500D
öMo used as an indicator for accuracy and
repeatability across grades.
Results: Identification and Differentiation
ö316 vs. 304
Selected Grade for Comparison Sample Tested Match Number Result FOX-IQ Suggested Match
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 304 0 PASS 304
304 316 8.46456 FAIL 316
304 316 8.6275 FAIL 316
304 316 8.89219 FAIL 316
304 316 8.4471 FAIL 316
304 316 8.71435 FAIL 316
304 316 8.57747 FAIL 316
304 316 8.73063 FAIL 316
304 316 8.44093 FAIL 316
304 316 8.45447 FAIL 316
304 316 8.4523 FAIL 316
Results: Identification and Differentiation
ö2.25Cr 1 Mo vs. C 0.5 Mo
Selected Grade for Comparison Sample Tested Match Number Result FOX-IQ Suggested Match
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly
Carb 1-2 Moly 2 1-4 Cr 17.0007 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 17.8751 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 16.9834 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 17.815 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 18.0241 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 17.3453 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 17.5918 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 18.076 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 16.806 FAIL 2 1-4 Cr
Carb 1-2 Moly 2 1-4 Cr 17.5637 FAIL 2 1-4 Cr
Results: Identification and Differentiation
öHast C276 vs. Monel K500
Selected Grade for Comparison Sample Tested Match Number Result FOX-IQ Suggested Match
HastC276 HastC276 0 PASS HastC276
HastC276 HastC276 0.241774 PASS HastC276
HastC276 HastC276 0.214841 PASS HastC276
HastC276 HastC276 0.217483 PASS HastC276
HastC276 HastC276 0 PASS HastC276
HastC276 HastC276 0.824648 PASS HastC276
HastC276 HastC276 0.70246 PASS HastC276
HastC276 HastC276 0 PASS HastC276
HastC276 HastC276 0 PASS HastC276
HastC276 HastC276 0.842044 PASS HastC276
HastC276 MonelK500 906.043 FAIL MonelK500
HastC276 MonelK500 941.067 FAIL MonelK500
HastC276 MonelK500 928.415 FAIL MonelK500
HastC276 MonelK500 952.743 FAIL MonelK500
HastC276 MonelK500 914.355 FAIL MonelK500
HastC276 MonelK500 908.606 FAIL MonelK500
HastC276 MonelK500 870.115 FAIL MonelK500
HastC276 MonelK500 880.951 FAIL MonelK500
HastC276 MonelK500 918.61 FAIL MonelK500
HastC276 MonelK500 1205.69 FAIL MonelK500
Results: Identification and Differentiation
öFOX-IQ analyzer successfully identified all 6 grades
öThe analyzer successfully differentiated grades with
same base
öThe analyzer accurately suggested the correct
grade when the sample did not match the selected
grade
Results: Accuracy
0.4
0.45
0.5
0.55
0.6
0.65
0.7
0.75
0.8
1 2 3 4 5 6 7 8 9 10
MoConcentration(%)
Test
Mo in 304SS
Mo Measured
Mo Assay
1.5
1.6
1.7
1.8
1.9
2
2.1
2.2
2.3
2.4
2.5
1 2 3 4 5 6 7 8 9 10
MoConcentration(%)
Test
Mo in 316SS
Mo Measured
Mo Assay
0.6
0.7
0.8
0.9
1
1.1
1.2
1 2 3 4 5 6 7 8 9 10
MoConcentration(%)
Test
Mo in 2.25Cr 1Mo
Mo Measured
Mo Assay
Results: Accuracy
0.3
0.35
0.4
0.45
0.5
0.55
0.6
0.65
1 2 3 4 5 6 7 8 9 10
MoConcentration(%)
Test
Mo in C 0.5Mo
Mo Measured
Mo Assay
14.5
14.7
14.9
15.1
15.3
15.5
15.7
15.9
16.1
16.3
16.5
1 2 3 4 5 6 7 8 9 10
MoConcentration(%)
Test
Mo in HastC276
Mo Measured
Mo Assay
0
0.02
0.04
0.06
0.08
0.1
0.12
0.14
0.16
0.18
0.2
1 2 3 4 5 6 7 8 9 10
MoConcentration(%)
Test
Mo in MonelK500
Mo Measured
Mo Assay
Results: Accuracy
y = 0.9845x + 0.0128
R² = 0.9999
0
2
4
6
8
10
12
14
16
18
0 2 4 6 8 10 12 14 16
Avg.MoMeasured(XRF)
Mo Assay
Mo results with FOX-IQ
öMo results are close to assay for all samples
öExcellent linearity relative to assay across all samples
Results: Repeatability
öMo used as indicator across grades
ö%RSD <2% for 5/6 grades
öHigh %RSD for Monel due to low levels present
− Only 0.007% difference from assay
öLonger test times could improve precision
Grade Name Mo Assay Avg. Measured Mo (XRF) %RSD
304SS 0.57 0.586 1.95
316SS 2.11 2.184 1.42
2.25Cr 1Mo 0.93 0.876 1.29
C 0.5Mo 0.49 0.458 1.98
Hast C276 15.36 15.13 0.69
Monel K500 0.024 0.031 23.95
Conclusions
öXRF and the FOX-IQ analyzer can be an effective part
of 100% inspection protocol
öFast testing with accurate, repeatable results
− ID/differentiation
− Chemistry data
öAbility to automate can improve process
− Short test times
− Greater reliability and repeatability of results
− Increased safety for inspectors
− Test moving samples
Questions?
Joel Kenyon
Global Product manager
Olympus Scientific Solutions Americas
Olympus and FOX-IQ are registered trademarks of Olympus
Corporation.

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Grade Verification and Compositional Analysis Using On-Line XRF as Part of 100% Inspection

  • 1. Grade Verification and Compositional Analysis Using On-Line XRF as Part of 100% Inspection Joel Kenyon Olympus Scientific Solutions Americas Global Product Manager
  • 2. Overview ö100% testing öX-ray fluorescence (XRF) öThe FOX-IQ® on-line XRF analyzer öTest procedure öResults öConclusions öQuestions
  • 3. Introduction öA single manufacturer can produce hundreds of different alloy grades öMixes have consequences − Aerospace, oil and gas, automotive, etc. ö100% inspection is ideal but not realistic without automation öAutomated NDT systems already in use as part of 100% inspection protocols (visual inspection, eddy current, etc.) öXRF can be a part of this as well
  • 4. X-ray Fluorescence öFluorescence = radiation absorbed and re-emitted at a different energy level öX-ray fluorescence (XRF) − Illuminate sample with X-rays − Ionization occurs − Characteristic X-rays emitted − Characteristic X-rays used to determine chemistry Ni Fe Cr Mo
  • 5. X-ray Fluorescence öWidely accepted technique for positive material identification (PMI) − Benchtop − Handheld
  • 6. The FOX-IQ XRF Analyzer öFactory On-line XRF − 40 kV X-ray source − Silicon drift detector − Factory installed grade library (400+ grades) − Automated (PLC) or manual (PC) operation
  • 7. The FOX-IQ XRF Analyzer öElements visible with the FOX-IQ analyzer
  • 8. Test Procedure öTwo questions: − Can the FOX-IQ analyzer successfully identify and differentiate the grades of interest? − How accurate/precise is the instrument? öPass/fail analysis with chemistry done manually öMatch cutoff set to 5 (default) − Match number closer to 0 = better match − Match cutoff = highest match number that can pass öTen repeat tests, 3 seconds each
  • 9. Test Procedure öSamples: 6 CRMs − Tested in pairs according to base − Already in library − All contain molybdenum (Mo) Grade Name Manufacturer Batch Number 304SS ARMI IARM 162D 316SS ARMI IARM 5D 2.25Cr 1Mo Brammer BS 46A C 0.5Mo ARMI IARM 229B Hast C276 Brammer BS H2C Monel K500 Brammer BS 500D öMo used as an indicator for accuracy and repeatability across grades.
  • 10. Results: Identification and Differentiation ö316 vs. 304 Selected Grade for Comparison Sample Tested Match Number Result FOX-IQ Suggested Match 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 304 0 PASS 304 304 316 8.46456 FAIL 316 304 316 8.6275 FAIL 316 304 316 8.89219 FAIL 316 304 316 8.4471 FAIL 316 304 316 8.71435 FAIL 316 304 316 8.57747 FAIL 316 304 316 8.73063 FAIL 316 304 316 8.44093 FAIL 316 304 316 8.45447 FAIL 316 304 316 8.4523 FAIL 316
  • 11. Results: Identification and Differentiation ö2.25Cr 1 Mo vs. C 0.5 Mo Selected Grade for Comparison Sample Tested Match Number Result FOX-IQ Suggested Match Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly Carb 1-2 Moly 0 PASS Carb 1-2 Moly Carb 1-2 Moly 2 1-4 Cr 17.0007 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 17.8751 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 16.9834 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 17.815 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 18.0241 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 17.3453 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 17.5918 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 18.076 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 16.806 FAIL 2 1-4 Cr Carb 1-2 Moly 2 1-4 Cr 17.5637 FAIL 2 1-4 Cr
  • 12. Results: Identification and Differentiation öHast C276 vs. Monel K500 Selected Grade for Comparison Sample Tested Match Number Result FOX-IQ Suggested Match HastC276 HastC276 0 PASS HastC276 HastC276 HastC276 0.241774 PASS HastC276 HastC276 HastC276 0.214841 PASS HastC276 HastC276 HastC276 0.217483 PASS HastC276 HastC276 HastC276 0 PASS HastC276 HastC276 HastC276 0.824648 PASS HastC276 HastC276 HastC276 0.70246 PASS HastC276 HastC276 HastC276 0 PASS HastC276 HastC276 HastC276 0 PASS HastC276 HastC276 HastC276 0.842044 PASS HastC276 HastC276 MonelK500 906.043 FAIL MonelK500 HastC276 MonelK500 941.067 FAIL MonelK500 HastC276 MonelK500 928.415 FAIL MonelK500 HastC276 MonelK500 952.743 FAIL MonelK500 HastC276 MonelK500 914.355 FAIL MonelK500 HastC276 MonelK500 908.606 FAIL MonelK500 HastC276 MonelK500 870.115 FAIL MonelK500 HastC276 MonelK500 880.951 FAIL MonelK500 HastC276 MonelK500 918.61 FAIL MonelK500 HastC276 MonelK500 1205.69 FAIL MonelK500
  • 13. Results: Identification and Differentiation öFOX-IQ analyzer successfully identified all 6 grades öThe analyzer successfully differentiated grades with same base öThe analyzer accurately suggested the correct grade when the sample did not match the selected grade
  • 14. Results: Accuracy 0.4 0.45 0.5 0.55 0.6 0.65 0.7 0.75 0.8 1 2 3 4 5 6 7 8 9 10 MoConcentration(%) Test Mo in 304SS Mo Measured Mo Assay 1.5 1.6 1.7 1.8 1.9 2 2.1 2.2 2.3 2.4 2.5 1 2 3 4 5 6 7 8 9 10 MoConcentration(%) Test Mo in 316SS Mo Measured Mo Assay 0.6 0.7 0.8 0.9 1 1.1 1.2 1 2 3 4 5 6 7 8 9 10 MoConcentration(%) Test Mo in 2.25Cr 1Mo Mo Measured Mo Assay
  • 15. Results: Accuracy 0.3 0.35 0.4 0.45 0.5 0.55 0.6 0.65 1 2 3 4 5 6 7 8 9 10 MoConcentration(%) Test Mo in C 0.5Mo Mo Measured Mo Assay 14.5 14.7 14.9 15.1 15.3 15.5 15.7 15.9 16.1 16.3 16.5 1 2 3 4 5 6 7 8 9 10 MoConcentration(%) Test Mo in HastC276 Mo Measured Mo Assay 0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.16 0.18 0.2 1 2 3 4 5 6 7 8 9 10 MoConcentration(%) Test Mo in MonelK500 Mo Measured Mo Assay
  • 16. Results: Accuracy y = 0.9845x + 0.0128 R² = 0.9999 0 2 4 6 8 10 12 14 16 18 0 2 4 6 8 10 12 14 16 Avg.MoMeasured(XRF) Mo Assay Mo results with FOX-IQ öMo results are close to assay for all samples öExcellent linearity relative to assay across all samples
  • 17. Results: Repeatability öMo used as indicator across grades ö%RSD <2% for 5/6 grades öHigh %RSD for Monel due to low levels present − Only 0.007% difference from assay öLonger test times could improve precision Grade Name Mo Assay Avg. Measured Mo (XRF) %RSD 304SS 0.57 0.586 1.95 316SS 2.11 2.184 1.42 2.25Cr 1Mo 0.93 0.876 1.29 C 0.5Mo 0.49 0.458 1.98 Hast C276 15.36 15.13 0.69 Monel K500 0.024 0.031 23.95
  • 18. Conclusions öXRF and the FOX-IQ analyzer can be an effective part of 100% inspection protocol öFast testing with accurate, repeatable results − ID/differentiation − Chemistry data öAbility to automate can improve process − Short test times − Greater reliability and repeatability of results − Increased safety for inspectors − Test moving samples
  • 20. Joel Kenyon Global Product manager Olympus Scientific Solutions Americas Olympus and FOX-IQ are registered trademarks of Olympus Corporation.