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@ARTICLE{Becker:39797,
author = {Becker, J. S. and Dietze, H.-J.},
title = {{A}pplication of double-focusing field {ICP} mass
spectrometry with shielded torch using different nebulizers
for ultratrace and isotope analysis of long-lived
radionuclides},
journal = {Journal of analytical atomic spectrometry},
volume = {14},
issn = {0267-9477},
address = {Cambridge},
publisher = {ChemSoc},
reportid = {PreJuSER-39797},
pages = {1493 - 1500},
year = {1999},
note = {Record converted from VDB: 12.11.2012},
abstract = {The capability of double-focusing sector field ICP-MS with
a plasma-shielded torch using different nebulizers (a
Meinhard nebulizer with a Scott-type spray chamber with a
solution uptake rate of 1 ml min(-1); a MicroMist
microconcentric nebulizer used with a minicyclonic spray
chamber with a solution uptake rate of 0.085 ml min(-1); an
ultrasonic nebulizer with a solution uptake rate of 2 ml
min(-1); and a direct injection high-efficiency nebulizer
with a solution uptake rate of 0.085 ml min(-1)) for the
introduction of radioactive sample solutions into the ICP
was investigated. The total amount of analyte for each
long-lived radionuclide (Ra-226, Th-230, Np-237, U-238,
Pu-239 and Am-241; concentration of each was 1 ng l(-1) in
the aqueous solution) using different nebulizers was 5 pg
for the Meinhard nebulizer, 0.4 pg for the MicroMist
microconcentric nebulizer and 10 pg for the ultrasonic
nebulizer. The application of the shielded torch yielded an
increase in sensitivity for all these nebulizers of up to a
factor of 5 compared with the original configuration without
a shielded torch. Sensitivities of about 2000 MHz ppm(-1)
were measured for the radionuclides investigated (except for
Ra-226) using the MicroMist microconcentric nebulizer with a
shielded torch. The detection limits were in the sub-pg
l(-1) range and the precision ranged from 1 to $2\%$ RSD
(n=5) for the 1 ng l(-1) concentration level (0.4 pg sample
size). A further increase in sensitivity for long-lived
radionuclides of nearly one order of magnitude in comparison
with the MicroMist microconcentric nebulizer was observed
using ultrasonic nebulization, but the amount of analyte
required was significantly higher (by a factor of 25). In
contrast, the direct injection high-efficiency nebulizer
(DIHEN) in double-focusing sector field ICP-MS (DF-ICP-MS)
with a shielded torch resulted in a decrease in sensitivity
in comparison with the unshielded torch because of a higher
water load due to the direct injection of aqueous solution
into the plasma. At low solution uptake rates (down to
several mu l min(-1)), the uranium solutions were analyzed
by DIHEN-ICP-MS using a double-focusing sector field
instrument with higher sensitivity than quadrupole-based
ICP-MS. Flow injection was used for sample introduction to
measure small sample volumes of radioactive waste solutions
(20 mu l). The determination of Np-237 at a concentration of
10 ng l(-1) by flow injection DF-ICP-MS was possible with a
precision of $2.0\%$ (RSD, n=5). In order to avoid mass
spectral interferences and matrix effects long-lived
radionuclides (e.g., of U, Th and Tc-99) were separated from
the radioactive waste matrix by liquid-liquid extraction or
ion exchange. The methods developed for the precise
determination of the concentration and isotopic ratios of
long-lived radionuclides were applied to aqueous standard
solutions and radioactive wastes by double-focusing sector
field ICP-MS. The precision of Pu isotopic analysis by
double-focusing ICP-MS with a shielded torch was 0.2, 2 and
$14\%$ for 1000, 100 and 10 pg l(-1) (amount of analyte:
500, 50 and 5 fg), respectively.},
keywords = {J (WoSType)},
cin = {ZCH},
ddc = {540},
cid = {I:(DE-Juel1)ZCH-20090406},
pnm = {Entwicklung analytischer Verfahren},
pid = {G:(DE-Juel1)FUEK118},
shelfmark = {Chemistry, Analytical / Spectroscopy},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000083077900031},
doi = {10.1039/a901762c},
url = {https://juser.fz-juelich.de/record/39797},
}