An international round robin test on the analysis of carbonaceous aerosols
on quartz fiber filters sampled at an urban site was organized by the Vienn
a University of Technology. Seventeen laboratories participated using: nine
different thermal and optical methods. For the analysis of total carbon (T
C), a good agreement of the values obtained by all laboratories was found (
7 and 9% r.s.d.) with only two outliers in the complete data set. In contra
st the results of the determination of elemental carbon (EC) in two not pre
-extracted samples were highly variable ranging over more than one order of
magnitude and the relative standard deviations (r.s.d.) of the means were
36.6 and 4.5%. The laboratories that obtained similar results by using meth
ods which reduce the charring artifact were put together to a new data set
in order to approach a "real EC" value. The new data set consisting of the
results of 10 laboratories using seven different methods showed 16 and 24%
lower averages and r.s.d. of 14 and 24% for the two not pre-extracted sampl
es. Taking the current filters as "equivalents" for urban aerosol samples w
e conclude that the following methods can be used for the analysis of EC in
carbonaceous aerosols: thermal methods with an optical feature to correct
for. charring during pyrolysis, two-step thermal procedures reducing charri
ng during pyrolysis, VDI 2465/1 method (removal of OC by solvent extraction
and thermodesorption in nitrogen) and the VDI 24652 method (combustion of
OC and EC at different temperatures) with an additional pre-extraction with
a dimethyl foramide (DMF)/toluene mixture. Only thermal methods without an
y correction for charring during pyrolysis and the VDI 2465/2 method were o
utside the range of twice the standard deviation of the new data set. For a
filter sample pre-extracted with the DMF/toluene mixture the average and r
.s.d. from all laboratories (20.7 mu gC; 24.4% r.s.d.) was very similar as
for the laboratory set reduced to 10 laboratories (20.6 mu gC; 19% r.s.d.).
Thus DMF pre-extraction appears to improve the performance of the thermal
methods without charring during pyrolysis control, e.g. the VDI 2465/2 meth
ods. (C) 2001 Elsevier Science Ltd. All rights reserved.