xrf and txrf - features and benefits
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The Benefits of TXRF for Ultra Trace Element Analysis
Innovation with Integrity
Dr. Armin GrossBruker Nano GmbH, Berlin, GermanyAugust, 2016
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TXRF – How does it work?
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Principles of EDXRFBackground
Energy-Dispersive X-Ray Fluorescence (EDXRF) analysis works in a 45°/45°geometry• Energy of X-ray photons
Which element• Number of X-ray photons
Quantitative analysis
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Samples for common XRF spectrometry
• Solids (cut, polished and put into suitable shape)• Powders (as pressed pellets, fused beads
or loose powders in liquid cups)• Liquids (in liquid cups)
Necessary sample amount: from 1g to 10 g !!
Principles of EDXRFSamples
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absorption of primary beamand fluorescence radiation
secondary fluorescenceenhancement
Ii = f (ci, cj) and ci = f (Ii, cj)
Concentration needs to be determinedwith matrix matched standardsDO YOU HAVE STANDARDS ???
Principles of EDXRFQuantification
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Principles TXRF spectroscopyFunctional principle
X-ray tube
monochromator
detector
sample disc
Total reflection X-ray fluorescence spectroscopy
• Samples must be prepared on a reflective media• Polished quartz glass or polyacrylic glass disc • Dried to a thin layer, or as a thin film or microparticle
Beam angle: 0o / 90o
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1. excitation spectrum2. spectrum after prefiltration,
filter component invisible here3. emission spectrum of the tube4. X-ray tube5. monochromator6. monochromatized excitation
beam7. detector8. sample carrier
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Key to TXRF sensitivityHigh signal to low background
Monochromatization ofX-ray beam leads toalmost completereduction of background
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Negligible absorption of primary beam and fluorescence radiation
Negligible secondary fluorescence enhancement
Ii = f ( ci ) ci = f ( Ii )
Samples are prepared as thin films or layersmatrix effects are negligible
Principles TXRF spectroscopyMatrix effects
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iIS
ISiISi SN
SNCC
Ci: Element concentrationCIS: Internal standard concentrationNi: Element net countrateNIS: Internal standard net countrateSi: Element sensitivity factorSIS: Internal standard sensitivity factor
Element sensitivity
L-linesK-lines
Atomic number
Principles of TXRFQuantification
Lack of matrix effect allowseasy quantification by internal standardization
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Samples for TXRF• Powders: Direct preparation
or as suspension• Liquids: Direct preparation• Always as a thin film, micro fragment or
suspension of a powder• Necessary sample amount:
Low µg respectively µl range
Principles TXRFSamples
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TXRF SpectrometerS2 PICOFOX
S2 PICOFOX – Compact TXRF
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• Most compact design portable, for on-site analysis
• Fixed excitation mode easy to use, mostsuitable for teaching
• >200 installations well established world wide technology
• Attractive pricing most valuable TXRFsolution
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TXRF SpectrometerS4 TStar
S4 TStar – Advanced TXRF
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• Multiple excitation to detect most elements modes of the PSE
• Large area detectors improved sensitivity for lowest limits of detection
• Sample geometry measurement of discs, flexibility microscopy slides, wafers
• Motorized beam path automatic beam adjustment and QC procedures
• Large sample capacity up to 90 sample discs, multi-user operation
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Rigaku Nanohunter II
• Benchtop model
• Mo X-ray tube, 600 W
• 16 samples capacity
GNR TX 2000• Floor-standing model
• Mo, W double target tube, 3 kW
• 12 samples capacity
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TXRF SpectrometerOther systems
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Straight forward sample preparation
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quartz glass glass carbon sapphire acrylic glass
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acrylic glass
quartz sapphire
glass carbon
Sample carrier
Quartz glass carriersdeliver lowest detectionlimits due to lowbackground
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fill sample in micro tube
add internal standard
homogenize
Note: high matrix samples pipette on carriermay require a dilution step
You‘ll need just a few steps for the preparation of liquid samples
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Sample preparationLiquid and digested samples
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dry by heat / vacuum
load the instrument
start data aquisition
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Sample preparationFinal steps
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dilute sample with distilled water
add internal standard
homogenize
pipette on carrier
Suspensions can be analyzed just after dilution
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Sample preparationSuspensions
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fill powder in mortar
grind carefully (<50 µm)
weigh about 20-50 mg
transfer to tube
Solids are ground to fine particle size and resuspended for direct analysis without digestion
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Sample preparationSolid and powder samples I
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suspend in detergent solution
add standard
homogenize
pipette on carrier
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Sample preparationSolid and powder samples II
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Sample preparationMicroparticles
dab vacuum grease on carrier
pick-up some particles with a (glass) rod
drop particles on grease
Microparticles are measured semi-quantitatively and non-destructively
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Current application areasTime for you to start with TXRF
Environmental /Ecology
Clinical Research / Biology Forensics Semiconductor
Nanoparticles Food/BeveragePharmaceutical/
Nutraceutical Plant Research
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www.facebook.com/groups/TXRFSpectrometry
eu.wiley.com/WileyCDA/WileyTitle/productCd-1118460278.html
www.s4tstar.com
www.s2picofox.com
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TXRFMore information required?