Verlag des Forschungszentrums Jülich
JUEL-3605
The detection limits of sector field ICP MS for actinoid nuclides of anthropogenic
origin (e.g. 240Pu, 243Am, 246Cm) are between about 0.4 and 1.1 fg/ml.
Under optimum experimental conditions (235U/238U » 1),
the precision in 235U/238U
isotopic ratio determinations has been determined as 0.06 % RSD. For the analysis
of radioactive samples, comparison measurements with alpha spectrometry have shown
good agreement between the values even for isotope ratios in the order of 10-6.
In order to reduce both the dose rate for the operator and radioactive
contaminations inside the mass spectrometer during the analysis of radioactive
sample solutions, an apparatus was constructed for flow injection analysis in
combination with a sector field ICP mass spectrometer (FI ICP MS) and optimized
with respect to minimal sample volume, low detection limits and good reproducibility
of the injection. A sample volume of 2 µl proved completely sufficient for
determining actinoids in the lower pg/ml concentration range.
For the determination of the long lived radionuclide 129I as well as the stable
127I occurring in nature, a gas-liquid separator was developed permitting the
efficient sample introduction of volatile iodine into the ICP-MS via the gas phase.
Using this sample introduction system it was possible to increase the detection
sensitivity about fiftyfold in comparison to the Meinhard nebulizer.
In addition to the analysis for radioactive sample solutions purely by mass
spectrometry, a new field of application for the on line coupling of HPLC and
ICP MS was opened up, i.e. the determination of the nuclide abundance and
concentration of lanthanoids in an irradiated tantalum target from a spallation
neutron source. Since the nuclide abundance of the lanthanoids formed in the
tantalum target differ greatly from those in nature and therefore a large number
of isobaric interferences were to be expected in the mass spectrum, it was
necessary to separate chemically the elements before analysing them by mass
spectrometry. Ion chromatography was used for this purpose.
Kerl, Wolfgang
Ultraspuren- und Isotopenanalyse langlebiger Radionuklide mittels doppelfokussierender Sektorfeld-ICP-Massenspektrometrie
122 S., 1998
Within the framework of the present study, new analytical methods were developed
for determining long lived radionuclides with the aid of double-focusing sector
field ICP mass spectrometry and applied for the analysis of various radioactive
samples. This primarily involved radioactive waste samples from the nuclear energy
sector and a tantalum target from a spallation neutron source. Major priority was
given to the ultratrace and isotopic analysis of actinoides, iodine and lanthanoids,
the latter being determined by the on line coupling of high-performance liquid
chromatography (HPLC) and sector field ICP MS.
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