24 Oil Spill identification - Round Robin 20045
Oil spill identification samples from inland waters and the North Sea are
analyzed according the concept guideline Part 2 of CEN BT/TF 120.
In general: Samples are analyzed in duplicate with GC-FID. After
assessment of the results the (probably) matching samples are also
analyzed with GC-MS in SIM mode.
After a visual assessment of the chromatograms (probably) matching
samples are integrated for a large range of compounds (depending on
the type of oil and compounds available). Ratios between spill and
source samples are compared by using the repeatability limit (ISO
5725) as a match criterion.
=>
Extract I
match
non-match
Extract II
match
non-match
Source I
Source II
Notes/remarks:
RIZA has diluted the Sintef mixture for peak recognition a factor of 3
with DCM and has analyzed the diluted mixture 8 times in order to
calculate the RSD for the mixture at the given concentration.
The results can be found on the CD in file St Sintef ratio validation.xls.
In the guideline it is stated that the RSD should be equal or lower than
5% during validation of the method. This is valid for all ratios with the
ratio DR-30d/30ab at limit.
2.10 Sintef
Contacts: K.R. Sorheim, L-G. Faksness and P.S. Daling.
Sintef http://www.sintef.no/ is a large Norwegian engineering institute
and is among others active in the petroleum industry and petroleum
research. Sintef analyzes all oil spill samples for the Norwegian
government.
As a basis for this oil spill fingerprinting case, SINTEF has used the
presently draft version, August 2005, of the "CEN/BT/TaskForce 120
Oil Spill Identification": Part 2 Analytical methodology and
interpretation of results"
Sintef analyzed the RR-samples with GC-FID and with GC-MS in SIM
mode on PAH's and biomarkers. The resulting chromatograms are first
evaluated visually and when a possible match is assumed a series of
ratios are statistically compared.
=> Extract I and II: Positive match between the spill samples.
The spill samples are from the same source
Source I: Positive match to the spills (Extract I and Extract II)
Source II: Non-match to the spills (Extract I and Extract II)