19
Oil Spill identification - Round Robin 20045
Cedre remarks that the biomarkers have a low abundance and a high
variance. This is shown on page 12 of their report between Source I
and Extract I for e.g. %32abS and %30g.
Several other participants use the same instrument (see 6.2) and were
able to analyze the biomarkers with a good sensitivity and a low
variance. In the report of Cedre no information about the injection
concentration could be found.
The method applied is quite normal although the injection temperature
is lower than most participants use.
RIZA has tested the injection temperature for the GC-FID analysis with
a split/splitless injector at 300°C, 325°C and 350°C and found a better
performance and a lower variance of the alkanes in the range of C30-
C44. Using the split/splitless injector in a series at a temperature of
350°C however resulted in a fast decrease of the performance of the
rubber sealing around the liner, although a high temperature ring was
used.
Based on that a temperature of 325°C is used for the split/splitless
injector (GC-FID) and 350°C for the PTV injector (GC-MS).
2.3 LASEM
Contact: Pauline Pierre
LASEM is a laboratory of the ministry of Defense and is located in Brest.
The samples have been analyzed with GC-MS in the full scan mode
(m/z 50 - 300) with an ion trap as detector.
=> In first approximation, the chromatogram of the four samples have the
same shape: mixture of light and heavier oils.
The comparison between the n-alkanes repartition of the four samples shows
differences in low boiling rang, but it could come from volatility of these
compounds: it does not allow to differentiate them.
The usually used biomarkers do not permit to conclude, because of their too
low abundance. Diagnostic ratios coming from the PAH’s, present more or
less significant differences, depending on the considered ratio.
As a conclusion,
Oil spills at day 1 seem to be different from source I and II,
Oil spills at day 2 seem to be different from source I and II,
Source I and source II are different,
Oil spill at day 1 seems to have the same source as the day 2’s.
Notes/remarks:
LASEM reports:
The usually used biomarkers do not permit to conclude, because of their too
low abundance.
RIZA has diluted the extract 8 times and diluted 3 ul of the source
samples in 1 ml DCM. Injections of 1 ul resulted in a good sensitivity
with about the same peak height for all samples (see fig 11 of the RIZA
report)