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Comparison between pXRF measurements and MC simulations (charts,

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Rh Kβ Rayleigh

Rh Kβ Compton

Rh KαRayleigh

Rh Kα Compton

PTFE_ 40kV_150µA_2500s_ filtered

Simulated/Experimental Counts

Energy (keV)

Experimental Simulated

Figure 35. PTFE experimental over simulated at 40kV, filtered excitation

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0.1 1 10

Experimetal/Simulated Ratio

Energy (keV)

PTFE ratio_40kV_150µA_2500s_filtered

Figure 36. PTFE experimental over simulated ratio at 40kV, filtered excitation

4.2 Comparison between pXRF measurements and MC

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101 102 103 104

Ag Kβ Ag Kα

Rh Kα Au M

Ag L

Cu Kβ Cu Kα

Au Lγ Au Lβ

ABKMF_40kV_100µΑ_3000s_filtered

Experimental/Simulated Counts

Energy (keV)

experimental simulated Au Lα

Figure 37. ABKMF experimental over simulated at 40kV.

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Experimental/Simulated Counts

Cu Kα

Ag L Au M

Ag Kβ Ag Kα Rh Kα Au Lγ Au Lβ Au Lα

Cu Kβ

ABSBL_40kV_100µΑ_3000s_filtered

Energy (keV)

experimental simulated

Figure 38. ABSBL experimental over simulated at 40kV.

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Experimental/Simulated Counts

Ag L Au M

Cu Kβ

Ag Kβ Ag Kα Rh Kα Au Lγ Au Lβ Au Lα Cu Kα

ABLLI_40kV_100µΑ_3000s_filtered

Energy (keV)

Experimental Simulated

Figure 39. ABLLI experimental over simulated at 40kV.

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Experimental/Simulated Counts

Cu Kβ

Ag Kβ Ag Kα Rh Kα Au Lγ Au Lβ Au Lα

Cu Kα Au M

Ag L

ABQAQ_40kV_100µΑ_3000s_filtered

Energy (keV)

experimental simulated

Figure 40. ABQAQ experimental over simulated at 40kV.

In the following graph, the % difference between experimental and simulated net peak area intensities of the detected characteristic X ray lines are presented, as they were extracted by means of the PyMca Toolkit.

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% (exp-sim)/exp

KMF Au: 58.58 ± 0.90 Ag: 29.37 ± 0.43 Cu: 12.05 ± 0.18 LLI

Au:74.96 ± 1.11 Ag: 5.04 ± 0.15 Cu: 20.0 ± 0.3 SBL

Au: 89.99 ± 1.35 Ag: 5.04 ± 0.15 Cu: 4.97 ± 0.15 QAQ

Au: 95.04 ± 1.42 Ag: 2.46 ± 0.15 Cu: 2.50 ± 0.15

Cu-Kα Ag-Kα Au-Lα Au-Mα

Figure 41. The % difference between experimental and simulated net peak area in- tensities of the detected characteristic X-ray lines of gold alloys.

It can be concluded that the simulation overestimates systematically all elements’

major peak intensities between ~5-10%, however, the Au-M intensity is experimentally overestimated by ~10-15%.

4.2.2 Silver alloys

The silver alloys that was used are CNR-91, CNR-92, CNR-141 and CNR-152.

The chemical composition of the silver alloys is reported in detail at the Table II of the chapter 3.2 Reference materials.

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101 102 103 104 105

Experimental/Simulated Counts Ag Kβ

Ag Kα

Rh Kβ Rh Kα Pb Lγ

Pb Lβ Pb Lα

Cu Kβ Cu Kα Ag L

CNR91_40kV_100µΑ_3000s_filtered

Energy (keV) experimental

simulated

Figure 42. CNR91 experimental over simulated at 40kV.

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100 101 102 103 104 105

Experimental/Simulated Counts

Rh Kβ Ag Kβ Ag Kα

Rh Kα Pb Lγ

Pb Lβ Cu Kβ

Pb Lα Cu Kα Ag L

CNR92_40kV_100µΑ_3000s_filtered

Energy (keV) Experimental

Simulated

Figure 43. CNR92 experimental over simulated at 40kV.

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Experimental/Simulated Counts

Ag L Cu Kβ Cu Kα

Rh Kβ Rh Kα

Ag Kα Ag Kβ CNR141_40kV_100µΑ_3000s_filtered

Energy (keV) Experimental

Simulated

Figure 44. CNR141 experimental over simulated at 40kV.

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Experimental/Simulated Counts Ag Kβ

Ag Kα

Rh Kβ Rh Kα Cu Kβ

Cu Kα Ag L

CNR141_40kV_100µΑ_3000s_filtered

Energy (keV) Experimental

Simulated

Figure 45. CNR152 experimental over simulated at 40kV.

In the following graph, the % difference between experimental and simulated net peak area intensities of the detected characteristic X ray lines are presented, as they were extracted by means of the PyMca Toolkit.

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% (exp-sim)/exp

Cu-Kα Pb-Lα Ag-Ka Ag-La

CNR-91

Ag: 97 ± 1 Cu: 1.5 ± 0.1 Pb: 1.5 ± 0.1

CNR-92

Ag: 92 ± 1 Cu: 6.5 ± 0.3 Pb: 1.5 ± 0.1

CNR-141

Ag: 92.5 ± 1 Cu: 7.5 ± 0.4

CNR-152

Ag: 96.5 ± 1 Cu: 3.5 ± 0.1

Figure 46. The % difference between experimental and simulated net peak area inten- sities of the detected characteristic X-ray lines of silver alloys.

In silver alloys, the Ag is the predominant component and the Ag-Kα lines are accurately simulated with differences below ~6% between the experimental and simu- lated intensities. The Cu-Kα lines are mostly overestimated. In CNR-91, where the Cu concentration is 1.5% the Cu-Kα intensity is overestimated by ~21%, whereas for other concentrations the observed differences are less than ~5%. The deviation observed for the Cu-Kα intensity for CNR-91 reference silver alloy could be attributed to a possible inhomogeneity of the Cu distribution within the alloy. Finally, the Ag-Lα lines are un- derestimated by the simulation for about 20%.

4.2.3 Copper alloys

As copper alloys was used the BCRA, BCRB, BCRD and BCRE. The chemical composition of the copper alloys is reported in detail at the Table I of the chapter 3.2 Reference materials.

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Experimental/Simulated Counts

Sn Kβ Sn Kα

Rh Kβ Rh Kα

As Kβ Pb Lγ Pb Lβ

Pb Lα As Kα

Zn Kβ Cu Kβ Zn Kα Cu Kα

Sn L

BCRA_40kV_100µΑ_3000s_filtered

Energy (keV)

Experimental Simulated

Figure 47. BCRA experimental over simulated at 40kV.

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As Kβ Pb Lγ Pb Lβ Pb Lα As Kα

Sn Kβ Sn Kα Rh Kβ Rh Kα Zn Kβ

Cu Kβ Zn Kα Cu Kα

Sn L

BCRB_40kV_100µΑ_filtered

Simulated/Experimental Counts

Energy (keV)

Experimental Simulated

Figure 48. BCRB experimental over simulated at 40kV.

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Experimental/Simulated Counts

As Kβ

Sn Kβ Sn Kα

Rh Kβ Rh Kα Pb Lγ Pb Lβ Pb Lα As Kα

Zn Kβ Cu Kβ Cu Kα

Sn L

BCRD_40kV_100µΑ_3000s_filtered

Energy (keV)

Experimental Simulated

Figure 49. BCRD experimental over simulated at 40kV.

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Experimental/Simulated Counts

Pb Lβ Pb Lα As Kα

Zn Kβ Cu Kβ Cu Kα

Sn L

As Kβ

Rh Kβ Rh Kα

Sn Kα Sn Kβ BCRE_40kV_100µΑ_3000s_filtered

Energy (keV)

Experimental Simulated

Figure 50. BCRE experimental over simulated at 40kV.

In the following graph, the % difference between experimental and simulated net peak area intensities of the detected characteristic X ray lines are presented, as they were extracted by means of the PyMca Toolkit.

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% (exp-sim)/exp

Cu-Kα Zn-Kβ As-Kβ Pb-Lβ Sn-Kα Sn-La

BCR-A Cu: 78.726 As: 0.194 ± 0.010 Pb: 7.9 ± 0.7 Sn: 7.16 ± 0.21 Zn: 6.02 ± 0.22

BCR-B Cu: 82.651 As: 0.099 ± 0.010 Pb: 0.39 ± 0.03 Sn: 2.06 ± 0.07 Zn: 14.8 ± 0.5

BCR-D Cu: 80.267 As: 0.285 ± 0.022 Pb: 9.2 ± 1.7 Sn: 10.1 ± 0.8 Zn: 0.148 ± 0.024

BCR-E Cu: 92.445 As: 0.194 ± 0.020 Pb: 0.204 ± 0.018 Sn: 7.0 ± 0.6 Zn: 0.157 ± 0.025

Figure 51. The % difference between experimental and simulated net peak area in- tensities of the detected characteristic X-ray lines of copper alloys.

The elements Zn and As were analyzed and compared by their respective Kβ lines in order to avoid systematic errors in the analysis of their Kα peak areas due to spectral interferences (Cu-Kβ with Zn-Kα and As-Kα with Pb-Lα). In the cases where the con- centration of both elements is below 1% (close to detection limits) the experimental measurements significantly overestimated the simulated counts by ~50-54% for Zn and

~26% for As. The Sn-Kα lines are overestimated by the simulation by ~9.7%. The dif- ferences observed regarding the intensity of Cu-Kα line is generally below ~10-14%.

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