State of the art X-ray fluorescence imaging facilities · 2018. 2. 16. · XFM: Aquatic Ecosystems...

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State of the art X-ray

fluorescence imaging facilitiesLINXS Workshop on X-ray Fluorescence imaging:How to plan and execute the perfect experiment

David Paterson

synchrotron.org.au

Fast X-ray fluorescence microscopy

2

1 Gigapixel image 40×9 mm = 66667×15000 (600 nm) pixels, 133 µsec, raw data 250 GB, 38 hrs. Petrographic section high grade ore, Sunrise Dam gold deposit, WA. Fisher et al., Miner. Deposita 50, 665-674 (2015).

Sr:Fe:Rb

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• Major (mainly) hard X-ray facilities

• Ptychography for super resolution

X-ray Fluorescence Microscopy

• Macro large objects fast, high sensitivity

• Micro microprobes, versatile, in-situ environments

• Nano nanoprobes, ultimate resolution <10 nmResolution

• Tomography

• Chemical speciation XAS

• XANES imaging

3D

Energy range

• Specialised environments and cells

• Cryostream

• Frozen hydrated

In situ

Cryo

State of the art X-ray fluorescence imaging

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Selenium toxicity in aquatic environments

Zn Se S

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Eye lensIris Brain

Liver

Gallbladder

Lung

Gut interior

Notochord

Tadpole exposed to SeIV (30 µg/L) for 7 days

Zinc

SeleniumSulphur

XFM: Aquatic Ecosystems Selenium

Bioaccumulation on the Micron Scale

Chantal Lanctôt (Griffith University),

Tom Cresswell (Environmental Research

ANSTO) et al.

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State of the art XFM facilities

• ESRF ID21*, ID16A*, ID16B

• PETRAIII P.06* microprobe and nanoprobe

• Diamond ID14 nanoprobe, ID18 microprobe

• Soleil Nanoscopium

• APS 2ID, 26ID 13IDE, Bionanoprobe*

• NSLSII HXN, SRX

• AS XFM*

• Asia Japan, China, South Korea, Taiwan

• MAXIV Up next!

• Elletra TwinMic

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ID21 ESRF

• Sulfur mapping and speciation

• Volcanically-induced drainage of

divalent iron-rich waters during

the Last Glacial Maximum

significantly contributed to the

global carbon cycle. Evidence

provided by micro X-ray

fluorescence and XANES

coupled to petrographic,

geochemical and DNA studies

of subglacial calcites from the

East Antarctic Ice.

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ID16 - Nanoprobes ESRF

• ID16A - Nano-imaging

• ID16B - Nano-analysis

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APS

Biological samples (primarily)

• 2-ID-D sub-micron fluorescence, XANES and

ptychography

• 2-ID-E well automated high throughput

Hard materials (mainly)

• 26-ID nanoprobe

GeoSoilEnviroCARS best geology

• 13 IDE

– Compositional analysis and mapping ~ 2-28 keV.

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Micro/Nano-Probe P06 at PETRA III

Micro/nanoscopic spatial resolution with XRF, XAS and XRD.

Ptychographic schemes => increased spatial resolution to

low nm range

Maia detector on microprobe

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HXN, SRX at NSLS-II

• Hard X-ray Nanoprobe (HXN) 3-ID structural

and X-ray fluorescence imaging.

– hard X-ray imaging of structure, elements, strain

and chemical states with spatial resolution

ranging from 10 to 30 nm

• Primarily materials research.

• Multilayer Laue Lenses (MLLs)

– spot size of 8.4 nm by 6.8 nm

Saša Bajt et al.;

Light: Science and Applications,

2017; DOI: 10.1038/lsa.201

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Submicron Resolution X-ray Spectroscopy SRX

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Bionanoprobe APS

Subcellular imaging, frozen hydrated

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X-ray Fluorescence Microscopy AS

Energy range: 4 to 25 keV

• Hard x-ray microprobe ΔE/E ~10-4

• X-ray fluorescence mapping (µ-XRF)

• X-ray fluorescence µ-XANES => XANES imaging

Only hard X-ray microprobe servicing Australasia

Martin de Jonge (Physicist)

• biological, biomedical and life science, tomography

Daryl Howard (Chemist)

• cultural heritage, forensic and mm-scale investigations

Cameron Kewish: AS fellow (Physicist)• XFM + ptychography

Juliane Reinhardt: AS fellow (Physicist)• XFM + ptychography with chemical contrast

David Paterson (Physicist)

• environmental and geological science

Probe Resolution Field of View H X V

KB Microprobe 1 µm 150 X 100 mm

Milliprobe 50 µm 600 X 1200 mm

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Macro scale XRF Imaging

Fred McCubbin “North Wind”

mercury: arsenic :iron

Hg: As: Fe

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Megapixels/hour:

bio-fortification of cereal grains

ZincIronManganese

10 keV incident

PotassiumCopperCalcium

Lombi et al.J. Exp. Botany 62, 273 (2011).

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Enzo Lombi, et al. Journal of Experimental Botany 62, 273 (2011).

“Megapixel imaging of micronutrients in mature barley grains.”

High definition analysis of elemental correlations

a

cb

Background

20

40

60

80

Zn-C

u f

req

uency

0.01 0.1 1 10 100

Cu (mg/kg)

0.01

0.1

1

10

Zn

(mg

/kg

)

a

b

c

100

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99

High-definition fast fluorescence tomography

= 2 µm, = 2 ms

2291 pixels, 2001 projections (4.6 Mpix).

3 hrs meas time

Rice grain with husk,

Compton

Ge

Zn

600 µm

10 µm

Compton

Ge

Zn

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Wheat roots exposed

2 µM As(V) ca. 24 hrA. Light micrograph taken

after completion of the

XANES imaging

B. Elemental map showing

total As distribution after

the XANES imaging.

C. Spatial distribution of

pixel-populations

identified by comparing

energy intensities.

D. Concentrations of

uncomplexed As(V) and

As(III)-thiol complexes in

the transect = red

rectangle in B.

Detailed XANES analysis in hydrated roots

Kopittke et al. New Phytologist 201, 1251-1262 (2014).

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Normalized As Kα-edge XANES

Energy (keV)

11860 11865 11870 11875 11880 11885 11890

Deriva

tive o

f no

rmaliz

ed x

µ(E

)

-0.4

-0.2

0.0

0.2

0.4

0.6

0.8

(i) Wheat As(V) - Outer

As(III)

As(III)-GSH

Energy (keV)

11.86 11.87 11.88 11.89 11.90

Norm

aliz

ed x

µ(E

)

As(III)-GSH

As(III)

As(V)-DMA

As(V)

[i] Wheat As(V) - Outer

[ii] Wheat As(V) - Inner

[iii] Wheat As(III)

[iv] Rice As(V) - Outer

[v] Rice As(V) - Inner

[vi] Rice As(III)

Wheat As(V) - Plaque

(i) Wheat As(V) – Outer

4 standards whitelines: As(V); As(V)-DMA; As(III); As(III)-GSH.

Kopittke et al., Laterally-resolved speciation of arsenic in roots of wheat and rice using fluorescence-XANES imaging, New Phytologist 201, 1251-1262 (2014).

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Fast efficient XFM: Strength

In situ and time-based studies

Mn Ca Compton

Images, data Peter Kopittke & Pax Blamey (U. QLD) Paper submitted PNAS

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Ca Ni

Mn

Alyssum leaf

van der Ent, Harris (2016)

2300 * 3500 pix = 8 Mpix,

dwell = 200 µs, dx = dy = 2 µm

Exposure time = 25 min

Duration = 31 min

Estimated duration without RASCAN = 46 min

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TwinMic: Elletra

• European Soft X-ray Transmission and

Emission Microscope

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X-ray Absorption Spectroscopy @ XFM

Access to most heavy elements (4 - 25 keV)

[https://magoosh.com/ged/ged-science-periodic-table/]

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Full spectral data collection:

raster sample through beam

Conventional synchrotron approach:

Read-out N full spectra at each pixel (~1 sec)

• 150 x 150 pixels ~6-7 hours

• 15 minutes ~30 x 30 pixels

Detector array: N detectors

Raster sample in X,Y through microbeam

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Full spectral data collection:

Event-by-event processing

Nuclear physics approach:

Sample X,Y for each detected X-ray event

• Freedom to use high scan rates

• Real-time processing of event stream

List-mode data stream:

X2, Y2, E2, n2

X3, Y3, E3, n3

X4, Y4, E4, n4

X5, Y5, E5, n5

X6, Y6, E6, n6

X7, Y7, E7, n7

X1, Y1, E1, n1

Xi X coordinate

Yi Y coordinate

Ei Energy

ni Detector #

Approach used on Nuclear Microprobe and XFM at Australian Synchrotron