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The Centre for Microscopy & Microanalysis NanoSIMS 50 nanoSIMS: a new analytical tool for ultra-fine feature analysis using secondary ion emission R.

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Presentation on theme: "The Centre for Microscopy & Microanalysis NanoSIMS 50 nanoSIMS: a new analytical tool for ultra-fine feature analysis using secondary ion emission R."— Presentation transcript:

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2 The Centre for Microscopy & Microanalysis NanoSIMS 50 nanoSIMS: a new analytical tool for ultra-fine feature analysis using secondary ion emission R. Stern* and Peta Clode The University of Western Australia Centre for Microscopy and Microanalysis

3 The Centre for Microscopy & Microanalysis NanoSIMS 50

4 The Centre for Microscopy & Microanalysis NanoSIMS 50 nanoSIMS labs #10

5 The Centre for Microscopy & Microanalysis NanoSIMS 50 SIMS Secondary Ion Mass Spectrometry probing analytical technique for measuring the surface or near surface chemical or isotopic composition of solids uses probe ions to sputter target ions in laterally microscale or smaller regions (ion microprobe) analytical characteristics: nm depth resolution lateral resolution 10s nm to m most sensitive of the probing analytical techniques, ppb-ppm entire periodic table, H to U simple sample preparation

6 The Centre for Microscopy & Microanalysis NanoSIMS 50 SIMS Data Dimensions: 1 dimension depth profile: composition along a line normal to the surface line scan: composition along a line parallel to the surface 2 dimensions image (map) of the surface distribution of secondary ion species 3 dimensions a stacked series of secondary ion images collected at discrete depths into the target Image Depth profile Line scan ratios 1816 O/O 24 Mg/ 28 Si Mass spectrum cps,ppm Se Basic from tiny mass consumed

7 The Centre for Microscopy & Microanalysis NanoSIMS 50 Sample under vacuum Ion source Primary ion column Secondary ion Collection Optics Energy Analyzer Detector Mass Analyzer SIMS analytical

8 The Centre for Microscopy & Microanalysis NanoSIMS 50 Ion sources: O -, Cs + Normal, co-axial primary & secondary ions Detector array: 5 isotopes acquired simultaneously High mass resolution analyzer samples Sample introduction

9 The Centre for Microscopy & Microanalysis NanoSIMS 50 Features of NanoSIMS dynamic SIMS for bulk sample ion chemical/isotopic characterization not for molecular identification or oxidation state probe lateral resolution 50 nm for 133 Cs nm for 16 O - ability to scan the primary beam and record secondary ion images at ultra- fine-scale lateral resolution very low eroson rate, ~nm/hr (sample preservation) simultaneous multicollection of up to 5 isotope species routine high mass resolution resolve isobaric interferences

10 The Centre for Microscopy & Microanalysis NanoSIMS 50 Ion imaging of TiCN alloy demonstrating sub-50 nm edge resolution with Cs + 10 x 10 um, 24 C 2 3 x 3 um, 26 CN

11 The Centre for Microscopy & Microanalysis NanoSIMS 50 BIOMATERIALS BIOMATERIALS sub-cellular imaging sub-cellular imaging biochemical function biochemical function cancer research cancer research pharmaceuticals pharmaceuticals

12 The Centre for Microscopy & Microanalysis NanoSIMS Harvard Medical School/ MIT, Boston USA National Resource for Mass Spectrometry Imaging, NIH NCRR 1. Washington University, Saint Louis, MO 2. Max Planck Institute, Mainz, Germany 3. Institut Curie, Paris, France 4. Oxford University, U.K 5. Lawrence Livermore National Lab, Livermore, CA, USA University of California, Davis 6. National Institute for Materials Science, Tsukuba, Japan 7. LAM, Centre de Recherche Public-GL, Luxembourg 8. ExxonMobil, New Jersey, USA 9. University of Tokyo 10. The UWA 11. Rouen Univ, France NanoSIMS labs bio-SIMS program

13 The Centre for Microscopy & Microanalysis NanoSIMS 50 Naturally-occurring isotopes 12 C – all cell organelles 14 N – DNA, RNA, proteins 31 P – DNA, RNA (nucleic acids) 32 S – proteins Artificial isotopes (stable or radioactive) 14 C – turnover/pathways of C 15 N – turnover/pathways of labelled amino acids (proteins), nucleic acids 17 F – Fluoracil, cancer drug targetting chromosomes 81 Br – in Bromodeoxyuridine (BrdU), specifically incorporated into DNA during DNA synthesis 123, 125, 127 I – in Iododeoxyuridine Non-metallic elements used in SIMS biological analysis

14 The Centre for Microscopy & Microanalysis NanoSIMS 50 Examples of metallic elements used in SIMS biological analysis Li, Na, K, Rb, Cs Be, Mg, Ca, Sr, Ba Ti, Cr, Mn, Fe, Ni, Pb, Al, In Au, Ag Sc, lanthanides, actinides to date, few studies, poor sensitivity and spatial resolution

15 The Centre for Microscopy & Microanalysis NanoSIMS 50 O - primary ion bombardment, positive secondary ions, and a silicon matrix

16 The Centre for Microscopy & Microanalysis NanoSIMS 50 Cs + primary ion bombardment, negative secondary ions, and a silicon matrix

17 The Centre for Microscopy & Microanalysis NanoSIMS 50 cortex cuticle Scanning electron microscopy images Example of human hair cross-section deposited on Si (Hallegot and Corcuff, 1993) Sample preparation must be dehydrated, +/- fast freezing, chemical fixation (glutaraldehyde, Os tetroxide), epoxy embedding, cryo-sectioning (0.3 – 1 µm) will feature of interest be preserved? other documentation techniques to map features (confocal, VPSEM, TEM, etc.)

18 The Centre for Microscopy & Microanalysis NanoSIMS 50 nanoSIMS samples Thin membranes on Si wafer Sample holder for 1 cm samples

19 The Centre for Microscopy & Microanalysis NanoSIMS 50 Imaging of resin embedded biological tissues 150 m A mucous-producing cell in coral tissue Scale = 3um Primary ions: Cs + 12 C 14 N 32 S 12 C 14 N 31 P A symbiotic algae in coral tissue Scale = 2um Primary ions: Cs +

20 The Centre for Microscopy & Microanalysis NanoSIMS 50 Imaging isotopic tracers in resin embedded biological tissues 150 m Coral epithelium 44 Ca 1 min Scale = 5um FOV = 35um Primary ions: O Ca / 40 Ca 44 Ca used as a tracer of calcium ( 40 Ca) to determine pathways of movement & uptake Region 44 Ca/ 40 Ca Natural abundance Mucous cell Spiked Seawater Epithelial cells Stinging cell0.02 Significant 44 Ca uptake

21 The Centre for Microscopy & Microanalysis NanoSIMS 50 Mouse cochlea cells

22 The Centre for Microscopy & Microanalysis NanoSIMS 50 Heavy metal exposure Audinot et al. (2003) Imaging of As within human hair

23 The Centre for Microscopy & Microanalysis NanoSIMS 50 Analytical Issues: will the metal ions be detectable? are there non-metallic ion labels that can be used as proxies for the metals? quantitation: how important? sample preparation to avoid element migration or loss

24 The Centre for Microscopy & Microanalysis NanoSIMS 50 nanoSIMS & ARC Metals in Medicine is capable of playing a vital role the analytical capabilities and experience with metals in biological media needs to be developed R. Stern and P. Clode are here to enter into research partnerships with you

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