Wm. Kwiatek et al., Trace element analysis by means of synchrotron radiation, XRF, and PIXE: selection of sample preparation procedure, J ALLOY COM, 328(1-2), 2001, pp. 283-288
When it comes to biological samples, trace element (TE) determination has t
o cope with very low concentrations, sometimes even below the minimum detec
table limit (MDL). This is why special sample preparation procedures have t
o be employed so that the TE concentration in the specimen is effectively e
nhanced in a known way. The aim of this study was the selection of a proper
sample preparation procedure by determination of selected element concentr
ations in different types of biological samples. In this work several sampl
e preparation procedures were applied in order to choose the best one for s
pecific experimental needs. The methods included: (a) tissue sectioning met
hod (if appropriate); (b) dry method without chemical treatment - the sampl
es were dried, homogenized and pressed into pellet; (c) wet method with che
mical treatment - the samples were mineralized. The analyses were performed
with different analytical methods in order to confirm the results obtained
and in order to determine the influence of target preparation procedure on
the level of elemental concentrations determination. The measurements were
done by means of SRIXE (synchrotron radiation induced X-ray emission), EDX
RF (energy dispersive X-ray fluorescence), TR-XRF (total reflection X-ray f
luorescence), and PIXE (proton-induced X-ray emission). The above methods a
re described and the analytical results discussed. The results of the eleme
ntal analyses per-formed with different techniques show a good agreement on
ly for some elements. The mineralization process increases the sensitivity
of elemental determination only for selected elements. In other cases one c
ould observe decreasing of elemental concentration in respect to non minera
lized samples. Selection of sample preparation procedure depends on analyti
cal requirements. (C) 2001 Elsevier Science BY All rights reserved.