M. Guillemin et al., INTERNATIONAL ROUND-ROBIN TESTS ON THE MEASUREMENT OF CARBON IN DIESEL EXHAUST PARTICULATES, International archives of occupational and environmental health, 70(3), 1997, pp. 161-172
Object: Diesel soot has been recognized as probably carcinogenic to hu
mans. Elemental carbon (also called black carbon) in soot is considere
d at the moment as the most significant surrogate to be measured for a
ssessing the exposure to this pollutant. Its analysis is done by combu
stion in an oven and determination of the CO2 formed, after eliminatio
n of the organic fraction of the soot by heating and/or by solvent ext
raction. The analysis allows determination of both fractions of the so
ot: ''elemental carbon'' (EC) and organic carbon (OC). The sum of EC a
nd OC is called TC (total carbon). Method: An informal European coordi
nation group organized two round robin tests on filter Samples collect
ed from diluted diesel emissions. The first round (RRT1) was performed
on 13 different samples analyzed by ten laboratories. The range of lo
ading was 2.5 to 150 mu g/cm(2) of EC. No evaluation of the precision
within laboratories could be made since each laboratory gave only one
result per sample. Therefore a second round (RRT2) was organized with
two samples and a blank filter sent in several portions to 11 laborato
ries. It should be stressed that each laboratory used its own method a
nd that no standardization was planned at this stage. Results: Results
of RRT1 showed that the coefficient of variation between laboratories
decreased with higher loading and was around 10% to 15% for EC above
about 20 mu g/cm(2). Dispersion of the results varied and it appeared
that the way OC is removed from the soot is probably the most importan
t factor of influence. The correlation between the laboratories was go
od as a whole but some systematic differences could be detected. Besid
es the different techniques to remove the organic carbon, the pretreat
ment of the filter by HCl (either as a vapor or as a solution) to remo
ve the inorganic carbonates (potential interference sources), is proba
bly also a significant factor of influence in the dispersion of the re
sults between laboratories. It is not yet clear from these results whe
ther the ''environmental'' laboratories give different results from th
e ''occupational'' laboratories, but it is clear that their objectives
differ since for the ''environmentalists'', EC is not a specific mark
er of diesel immissions, in contrast to the ''occupationalists'' Concl
usion: It can be concluded that, although significant differences exis
t between laboratories they can be attributed mainly to the narrow dis
tribution of the results within a single laboratory, and that the over
all agreement of the results for EC and TC is fairly good. These resul
ts obtained with pure diesel engine emissions, should be complemented
by field samples, but they have already achieved relevant findings in
the performance of the procedures used to assess exposure to diesel so
ot.