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Materialien/Werkstoffe Poster: Do., 13:00–15:30 D-P397
In-house Certification of a Reference Material by Neutrons, Ions, Synchrotron
Radiation and ICP-IDMS
Heinrich Riesemeier 1 , Achim Berger 1 , Klaus Ecker 1 , Wolf Görner 1 , Wolfgang
Pritzkow 1 , Martin Radtke 1 , Uwe Reinholz 1 , Jochen Vogl 1
1 BAM Unter den Eichen 87 12205 Berlin
The certification of reference materials (CRMs) is the core task of the department Analytical
Chemistry; Reference Materials of the Federal Institute for Materials Research
and Testing (BAM). They are used for quality assurance in chemical analytical laboratories.
Rutherford backscattering spectrometry (RBS), instrumental neutron activation
analysis (INAA), inductively coupled plasma isotope dilution mass spectrometry
(ICP-IDMS) and X-ray fluorescence based on synchrotron radiation (SyXRF) have
already successfully contributed to the BAM programme of certifying reference materials.
With the thin film reference material Molybdenum implanted in Silicon for the
first time the combination of these techniques, which are all available at the Division
I.4 Nuclear Analysis , has been used to certify a reference material completely in-house.
RBS was performed at the 2 MV tandem ion accelerator of BAM, INAA at the irradiation
facilities (BER II reactor) of the Hahn-Meitner Institute in Berlin for neutron
activation analysis. SyXRF was carried out at the Beamline of the BAM at the Berlin
Synchrotron BESSY.
While RBS, INAA and ICP-IDMS are accepted methods for certification, the use
of SyXRF is quite new. To meet the requirements for the certification of reference
materials, a new quantification method, based on Monte Carlo Simulations and pure
element samples, has been established. This method is characterized by the minimization
of the influence of the uncertainty of fundamental and geometric parameters and
the elimination of the influence of the detector response. Drawbacks are the need to
measure additional spectra and the required computing time if an iteration scheme
must be applied.
The measured values for the areal density of Mo are given here:
ID-ICPMS 3.43 (±0.04)E + 16atoms/cm 2
INAA 3.38 (±0.05)E + 16atoms/cm 2
RBS 3.56 (±0.03)E + 16atoms/cm 2
SyXRF 3.47 (±0.03)E + 16atoms/cm 2
Mean value 3.46 (±0.07)E + 16atoms/cm 2
(2 chips, 2 measurements each)
(2 chips)
(4 chips , 2 measurements each)
(20 chips, 2 measurements each)
Additionally the property of SyXRF to measure non-destructive and fast, opened the
possibility to analyse all available chips, to determine homogeneity. As a result of this
measurements a number of chips with aberrant values have been excluded from further
use. The work on the certification report is in progress.