CEN/TR 15522-2:2006

Oil spill identification - Waterborne petroleum and petroleum products - Part 2: Analytical methodology and interpretation of results

This Technical Report (TR) describes a methodology to identify waterborne oils spilled in marine, estuarine and aquatic environments by comparing samples from spills with those of suspected sources . It provides detailed analytical and processing specifications for identifying waterborne oil spills and their correlation to suspected sources. When suspected sources are not available, the methodology may be used to characterise the spill as far as possible with respect to the oil type.
This methodology is restricted to petroleum and petroleum products containing a significant proportion of
HC-components with a boiling point above 200 °C. Examples are: Crude oils, condensates, light fuel oils, diesel oils, residual bunker oils, lubricants, and mixtures of bilge and sludge samples. Still, the general concepts described in this methodology have a limited applicability for some kerosenes and some condensates, but may not be applicable for gasoline
NOTE   This method is not intended for oil spills to groundwater and soil. The chromatograms of oil extracted from soil and found in ground water may contain reduced and/or additional peaks compared to the source sample. Including such samples in this method makes it necessary to add extraction methods and to describe which compounds are possibly reduced and/or which additional peaks can be expected to change the final conclusion from a probable match into a match. This is beyond the scope of this guideline, however,  when case samples completely match according to this method, the method is valid for those samples.

Identifizierung von Ölverschmutzungen - Rohöl und Mineralölerzeugnisse aus dem Wasser - Teil 2: Analytische Methodik und Interpretation der Ergebnisse

Identification des pollutions pétrolières - Pétrole et produits pétroliers dans l'eau - Partie 2 : Méthodologie analytique et interprétation des résultats

Prepoznavanje razlitij olj - Nafta in naftni proizvodi v vodi - 2. del: Analitske metode in podajanje rezultatov

General Information

• Status: Withdrawn
• Publication Date: 31-Oct-2006
• Withdrawal Date: 02-Oct-2012
• ICS: 75.080 - Petroleum products in general
• Technical Committee: CEN/SS S27 - Waste - Characterization, treatment and streams
• Drafting Committee: CEN/SS S27 - Waste - Characterization, treatment and streams
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Start Date: 03-Oct-2012
• Completion Date: 03-Oct-2012
• Ref Project: SIST-TP CEN/TR 15522-2:2008 - Oil spill identification - Waterborne petroleum and petroleum products - Part 2: Analytical methodology and interpretation of results

Relations

• Replaced By: CEN/TR 15522-2:2012 - Oil spill identification - Waterborne petroleum and petroleum products - Part 2: Analytical methodology and interpretation of results based on GC-FID and GC-MS low resolution analyses
• Effective Date: 08-Oct-2012

Standards Content (Sample)

SLOVENSKI STANDARD
01-julij-2008
Prepoznavanje razlitij olj - Nafta in naftni proizvodi v vodi - 2. del: Analitske
metode in podajanje rezultatov
Oil spill identification - Waterborne petroleum and petroleum products - Part 2: Analytical
methodology and interpretation of results
Identifizierung von Ölverschmutzungen - Rohöl und Mineralölerzeugnisse aus dem
Wasser - Teil 2: Analytische Methodik und Interpretation der Ergebnisse
Identification des pollutions pétrolieres - Pétrole et produits pétroliers dans l'eau - Partie
2 : Méthodologie analytique et interprétation des résultats
Ta slovenski standard je istoveten z: CEN/TR 15522-2:2006
ICS:
13.020.40 Onesnaževanje, nadzor nad Pollution, pollution control
onesnaževanjem in and conservation
ohranjanje
13.060.99 Drugi standardi v zvezi s Other standards related to
kakovostjo vode water quality
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL REPORT
CEN/TR 15522-2
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
November 2006
ICS 75.080
English Version
Oil spill identification - Waterborne petroleum and petroleum
products - Part 2: Analytical methodology and interpretation of
results
Identification des pollutions pétrolières - Pétrole et produits Identifizierung von Ölverschmutzungen - Rohöl und
pétroliers dans l'eau - Partie 2 : Méthodologie analytique et Mineralölerzeugnisse aus dem Wasser - Teil 2: Analytische
interprétation des résultats Methodik und Interpretation der Ergebnisse

This Technical Report was approved by CEN on 25 September 2006. It has been drawn up by the Technical Committee CEN/BT/TF 120.

CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 15522-2:2006: E
worldwide for CEN national Members.

Contents Page
Foreword.4
Introduction .5
1 Scope .7
2 Normative references .7
3 Terms and definitions .7
4 Strategy for identification of oil spills .9
4.1 General.9
4.2 Procedure .10
4.3 Decision chart of analytical and data treatment levels.10
5 Sample preparation .12
5.1 General.12
5.2 Visual examination of samples .13
5.3 Preparation .13
5.4 Recommended sample clean up methodology .14
5.5 Recommended injection concentration .15
6 Characterization and evaluation of analytical data.15
6.1 General.15
6.2 Characterization by GC/FID – level 1 .15
6.3 Characterisation by GC/MS – level 2 .17
6.4 Treatment of the results – level 3.27
6.5 Conclusions .33
7 Reporting .33
8 Quality assurance.34
Annex A (informative) Analytical standards .35
A.1 General.35
A.2 Recommended standards and concentrations .35
A.3 Analytical standards for PAH homologues.36
A.4 Calibration- GC/MS .37
Annex B (informative) Suggested instrument conditions.39
B.1 GC/FID conditions.39
B.2 GC/MS conditions.41
B.3 Sample analysis.42
B.4 Calculations.44
B.5 SIM-sections .45
Annex C (informative) List of PAHs and biomarkers analysed by GC/MS-SIM.46
Annex D (informative) Alkyl homologues patterns of PAHs.49
Annex E (informative) Boiling points of n-alkanes .58
Annex F (informative) General composition of oils – chemical groups .59
F.1 Introduction.59
F.2 Hydrocarbons.59
F.3 Paraffins.59
F.4 Naphthenes .60
F.5 Aromatics .60
F.6 Heteroatomic organic compounds .60
F.7 Resins.60
F.8 Asphaltenes .60
Annex G (informative) Weathering of oils spilled at sea.61
G.1 Introduction.61
G.2 Evaporation.62
G.3 Dissolution .64
G.4 Re-distribution of chemical composition.65
G.5 Biodegradation .66
G.6 Contamination / in-homogeneity .67
G.7 Evaluation of weathering.67
G.8 Optional - Semi-quantitative distribution of PAH homologues - weathering check.69
Annex H (informative) Characteristic Features of Different Oil Types in Oil Spill Identification .70
H.1 Introduction.70
H.2 Light fuel oil (gas oil, diesel, fuel No 2).70
H.3 Lubricating oil.75
H.4 Heavy fuel oil (HFO, Bunker C, Fuel No 6).79
H.5 Waste oil (bilge oil, sludge, slops).87
H.6 Crude oil .93
H.7 Conclusion .98
Annex I (informative) Example of the evaluation of an oil case .100
I.1 Introduction.100
I.2 GC/FID results.100
I.3 GC/MS results .102
I.4 Conclusion .106
Bibliography.107

Foreword
This document (CEN/TR 15522-2:2006) has been prepared by CEN/BT/TF 120 “Oil spill identification”, the
secretariat of which is held by SN.
Introduction
This Technical Report gives a recommendation on a forensic methodology for identifying waterborne oils. The
methodology may be a support to the legal process as evidence for prosecuting offenders ("potential
responsible party" – PRP). This methodology is a technical revision of the Nordtest Method NT CHEM 001
(1991) "Oil spill identification".
This methodology is described by the following CEN documents:
Part 1 – Sampling: describes sampling techniques and the handling of oil samples prior to their arrival at the
forensic laboratory;
Part 2 – Methodology: covers the general concepts and laboratory procedures of oil spill identification
methodology, analytical techniques, data processing, data treatment, and interpretation/evaluation of results.
Oil spill identification and oil comparison is a complex methodology due to the large variation in samples and
oil spill situations, which can be encountered. Part 1 is a compilation of instructions and experiences from
experts all over the world and will guide the user in sampling, storing and delivering oil samples. Part 2 will
guide the reader through the process by dividing the methodology into 3 tiered levels. It prescribes how to
prepare and analyse oil samples with GC/FID and, if necessary, with GC-low-resolution mass spectrometry.
Differences found between samples are only relevant if a difference is larger than the analytical variance of
the method. Therefore good analytical performance and strict quality assurance are essential. In the annexes
...