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@ARTICLE{Krachler:62615,
author = {Krachler, M. and Mohl, C. and Emons, H. and Shotyk, W.},
title = {{I}nfluence of digestion procedures on the determination of
rare earth elements in peat and plant samples by
{USN}-{ICP}-{MS}},
journal = {Journal of analytical atomic spectrometry},
volume = {17},
issn = {0267-9477},
address = {Cambridge},
publisher = {ChemSoc},
reportid = {PreJuSER-62615},
pages = {844 - 851},
year = {2002},
note = {Record converted from VDB: 12.11.2012},
abstract = {Analytical procedures for the determination of rare earth
elements (REE) in 250 mg aliquots of difficult-to-digest
peat and plant matrices by ICP-MS were developed. Three
different pressurised digestion approaches were tested for
this purpose, namely (i) closed vessel acid digestion on a
hot-plate at 180 degreesC, (ii) digestion in a microwave
high pressure autoclave at a temperature of 240 degreesC and
(iii) high pressure ashing (HPA) at a temperature of 320
degreesC. Acid mixtures for digestion contained concentrated
nitric acid (3-5 ml) alone or additions of hydrofluoric acid
(HF) or tetrafluoroboric acid (HBF4) at volumes of 0.05-1.0
ml. The selection of appropriate volumes of HF or HBF4 was
identified as a critical step in obtaining accurate results.
For several reasons, HBF4 is preferred in comparison with
the normally used addition of HF for the destruction of
siliceous matter in the samples investigated. The optimum
acid mixture consisted of 3 ml of HNO3 and 0.1 ml of HBF4.
High sample throughput (40 samples simultaneously in about 2
h) favours the microwave autoclave over the other two
digestion systems. An ultrasonic nebuliser (USN) with
membrane desolvation used for sample introduction reduced
the spectral interferences originating from oxide formation
of lighter REE and Ba to a negligible extent. Internal
standardisation with Rh and Re proved to be essential for
obtaining correct results. In this way, all REE could be
reliably quantified by USN-ICP-MS without applying any
mathematical correction equations. The accuracy of the
optimised procedures was assessed by the determination of
REE in digests of the certified reference material GBW 07602
Bush Branches and Leaves and of the candidate reference
material CRM 670 Aquatic Plant. The developed analytical
procedures were applied to the determination of REE in two
different peat matrices. Results for these peat samples
obtained by USN-ICP-MS showed good agreement with INAA
values. Strong fractionation of REE caused by the addition
of HF or HBF4 in excess, known as lanthanide contraction,
could be experimentally established, except for europium,
which revealed a different behaviour.},
keywords = {J (WoSType)},
cin = {ICG-III},
ddc = {540},
cid = {I:(DE-Juel1)VDB49},
pnm = {Chemie und Dynamik der Geo-Biosphäre},
pid = {G:(DE-Juel1)FUEK257},
shelfmark = {Chemistry, Analytical / Spectroscopy},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000177254600015},
doi = {10.1039/b200780k},
url = {https://juser.fz-juelich.de/record/62615},
}