ORBIS MicroEDXRF System XRF Advantages Nondestructive No beam

ORBIS — Micro-EDXRF System

XRF Advantages Non-destructive: No beam damage or coating of sample Minimal Sample Preparation: • conductivity not required • sample shape can be irregular Detection limits improve: 10 x or better (vs. SEM-EDS) Navigation by Optical Microscope Low Vacuum (~ 300 m. Torr) or No Vacuum (Air) More appropriate than SEM for larger scale features X-rays are penetrating (microns to millimeters)

Sample Chamber / XYZ Stage Chamber Door • Width ~ 500 mm • Height ~ 515 mm • Can be set up to swing: • Right to left (as shown) • Left to Right • Open access to sample chamber

Manual Control and Analysis

Spectral Mapping: Mapping Examples

Elemental Spatial Distribution Maps: Paper Fe X-rays penetrate paper Mg Map Al Map • Generation of BMP Elemental Maps Fe Map

Mapping Metal Analysis: Coins (Non. Destructive) * Rare Coin (2 Reichsmark - 1927? ) Conclusion: * Pixels: 64 x 50 Map * Dwell time: 0. 3 s/pixel * Total time ~ 20 minutes Counterfeit Coin

Cl Mapping of Cement Core: Filtered Excitation Cross Section Surface Treatment Cement Core • • Goal: To access diffusion of Cl into cement from deicing agent where Cl could corrode supporting steel Cores are cross-sectioned Rough cut (often there is a desire to avoid polishing to minimize sample preparation or corruption of the sample) Acquisition of data with Rh-tube, poly-capillary optic and Al(thin) filter to remove interfering scatter from Rh(L) tube line

Cement Chemistry – Road Salt: Filtered Excitation Surface Treatment Data courtesy of J. M. Davis, Microanalysis Research Group – NIST Map images processed and displayed using Lispix SW

Spectral Mapping - Bone Fossilization Fe K P Si Na Data courtesy of George Havrilla, LANL

Map Tool: Substitution Map Image Overlay Fe – Red K – Blue Si – Yellow P – Gray Na - Green Bone Fossilization

Map Tool: Elemental Image Overlay – RGB Phase Analysis Bone fossilization Ca – Red • Bone Si – Green • mineral P – Blue • Bone Substitution Overlay Image: Ca-Si-P

Map Tool: Elemental Image Overlay – RGB Phase Analysis Bone fossilization Bone – purple (Ca, P) New mineral – orange (Ca, Si)

Spatial Distribution Maps: Facial Tissue • Tissue masked with carbon tape for Si-free zone • Mapping region 15. 6 mm x 11. 3 mm

Map Tool: Data Mining • Recall spectra from mapped pixels • Hot Si spots hide low-level Silicone coverage

Map Tool: 3 -Log Band Image Scaling • 3 individual color logarithmic scales (NIST) • Low level Silicone distribution exposed in Green

and Filter – Alumina supported Catalysts Ag supported on Alumina Spheres Pd supported on Alumina pellets Objective: Measure metal distribution in ceramic support Samples: Embedded in epoxy and cross-sectioned on one side (no polish) Ag(L), Pd(L) versus Ag(K), Pd(K) • L-lines probe ~ 20 mm into ceramic; no need to make a thin section • K-lines probe ~ 4 mm into ceramic; interference from opposite surface Map Acquisition: Rh tube excitation requires filter to remove Rh(L) interference • Poly-capillary: ~ 55 mm FWHM lateral resolution at Ag(L), Pd(L) • Thin Al filter to remove Rh(L) from exciting spectrum • True Analytical flexibility in micro-XRF beam

Spectral Mapping – Alumina supported Catalysts Ag(L) Map: Thermal Image Scaling Pd(L) Map: Thermal Image Scaling Objective: Measure metal distribution in ceramic support Samples: Embedded in epoxy and cross-sectioned on one side (no polish) Metal is concentrated in the exterior shell of the ceramic support

Spectral Mapping – Alumina supported Catalysts Ag(L) Map: 3 Log Band Image Scaling Pd(L) Map: 3 Log Band Image Scalin Objective: Measure metal distribution in ceramic support Samples: Embedded in epoxy and cross-sectioned on one side (no polish) Specialized Image Scaling reveals important distributional details • Ag(L) map shows interior ring of Ag at weaker concentration, but no internal Ag • Pd(L) map shows the interior pellet has weak, uniform concentration of Pd

High Resolution Spectral Mapping – Odessa Meteorite (20 mm x 16 mm) Fe – green Ni – blue Cr – cyan S – magenta Cl – yellow P - red Total Spectral Count Image (TSC Image) Area ~ 20 mm x 16 mm Elemental Image Overlay RGB Merge Fe – Red Ni – Green P - Blue

Fe High Resolution Spectral Mapping – Odessa Meteorite (20 mm x 16 mm) Fe Elemental Image Overlay Cl Ni P S

High Resolution Spectral Mapping – Odessa Meteorite (20 mm x 16 mm) * * * RGB Merge * * Fe: Ni (Kamacite) * * Fe: Ni (Taenite) * Fe – Red Ni – Green P - Blue Fe: Ni: P( *) (Schreibersite)

High Resolution Spectral Mapping – Odessa Meteorite (20 mm x 16 mm) RGB Merge Fe – Red Ni – Green S - Blue Fe: Ni (Kamacite) Fe: Ni (Taenite) Fe. S (Troilite)