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Mike Beauchaine
TXRF Product Manager, Bruker AXS Inc.
Madison, Wisconsin
Low Z
High Z
LK transition
= K line
MK transition
= K line
ML transition
= L line
NL transition
= L line
Ii = f (ci, cj)
secondary fluorescence
enhancement
and
ci = f (Ii, cj)
detector
monochromator
o
o
Beam angle: 0 / 90
sample disc
X-ray tube
C IS N i S IS
Ci =
N IS S i
Ci: Element concentration
CIS: Internal standard concentration
Ni: Element net countrate
NIS: Internal standard net countrate
Si: Element sensitivity factor
SIS: Internal standard sensitivity factor
Element sensitivity
K-lines
L-lines
Direct preparation
Simple quantification
Matrix effects are negligible
due to thin layer
Quantification is possible by internal
standardization
TXRF Spectrum
Multi-element standard
Element
Ca
Ti
V
Cr
Mn
Fe
Co
Ni
Cu
Zn
As
Se
Sr
Conc./(mg/l)
0.991
0.997
0.986
0.994
1.015
0.996
1.006
1.005
1
0.989
1.019
1.1
0.987
LLD/(mg/l)
0.003
0.003
0.002
0.002
0.002
0.001
0.001
0.001
0.001
0.001
0
0
0
Environmental /
Ecology
Nanoparticles
Clinical Research /
Biology
Forensics
Semiconductor
Food/Beverage
Pharmaceutical/
Nutraceutical
University
Research
Sample preparation
Liquid and digested samples
Youll need just a few steps for the preparation of liquid samples
pipette on carrier
Sample preparation
Final steps
Liquid Samples
Trace Element Analysis in Serum & Blood
Measurements and sample preparation
Blood Serum
Whole Blood
Digestion, 10%
tetramethylammonium
hydroxide @ 1 hr
Dilute in 2% HCl
solution
Int. Standard, Ga
TXRF
Liquid Samples
Trace Element Analysis in Serum & Blood
Liquid Samples
Trace Element Analysis in Serum & Blood
Application studies
Sample preparation for solids
Sample preparation of
plants, tissues, grains
Application studies
Sample preparation for solids
Application studies
Sample preparation for solids
Application Studies
Wheat Flour
Source
Announcement of the
Federal Reserve Bank Of
Minneapolis
Application studies
Wheat Flour
Requirements
High sensitivity/accuracy
Application studies
Wheat Flour
10000
Results
element
concentrations
1000
P
Cl
Ca
100
Fe
Zn
Mn
10
Se
Cu
Ba
Br
Rb
Ni
0
0
10
100
1000
10000
Application studies
Wheat Flour
Results
10000
element
concentrations
TXRF-value:
Reference:
3 LLD:
S
1000
Cl
Ca
100
Fe
Zn
Mn
Se
Cu
Ba
Br
Rb
Ni
0
0
10
100
1000
10000
Application studies
Palladium Analysis
Introduction:
Looking for an easy to use technique with fast sample prep and little to no
consumables that can be implemented on the manufacturing floor
Study:
Standards
Determine linearity, sensitivity, accuracy, and precision for Pd plus Cr, Fe,
Cu, Rh, and Pt
Application studies
Palladium Analysis
Diluent Choice
Detector
Sample
5 10 mg
of Sample
14.02.2012
Internal
Standard(s)
Sample Prepared in
Organic Solvent /
Dilute Acid Diluent
Sample Solution
Spotted
and Dried
on Substrate
TXRF
Sample Spot
Analysis
Application studies
Palladium Analysis
Conclusion
o The choice of the X-ray target is very important for Pd
analysis because of the Pd-L line interferes with Ar-K line
o TXRF can accept organic solvent-based diluents
o Instrument is easy enough for a technician to be able to run
samples at or near the plant floor
o Also allows for fast analysis of impurities with small sample
size requirements
Acknowledgments: Bradley Shaw, David Semin, et.al Analytical and Research Development, Amgen Inc.
Thousand Oaks, CA Comparison of Total Reflection X-Ray Fluorescence (TXRF) to Inductively-Coupled
Plasma Spectrometry (ICP-MS): Applicability of TXRF for Open-access
14.02.2012
Sample preparation
Microparticles
Microparticles are measured semi-quantitatively and
non-destructively
Particles
Characterization of nanoparticles
Analytical question
element ratios in CdSe nanoparticles
coated with ZnS
Analytical issues
extremely small sample amount (R&D)
non-destructive method preferred
TXRF measurement
transfer of nanoparticles to quartz carrier
by cotton bud
standardless quantification
Results
even smallest sample amounts allow the
determination of element ratios in
nanoparticles
Particles
Characterization of nanoparticles
Results
S2 PICOFOX
Standardless
analysis applied
12
Sample 1
10
Sample 2
10
Ratio (wt.-%)
Sample 3
8
6
4
4
2
0
Zn/S
Cd/Se
Zn/Cd
Application Examples
Conclusion
Accuracies and Sensitivities comparable to AAS or ICP without the need for
complex and time-consuming sample preparation and instrument calibration
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