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BS EN 15522-2:2023

BS EN 15522-2:2023

$215.11

Oil spill identification. Petroleum and petroleum related products – Analytical method and interpretation of results based on GC-FID and GC-low resolution-MS analyses

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BSI 2023 222
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This document specifies a method to identify and compare the compositional characteristics of oil samples. Specifically, it describes the detailed analytical and data processing methods for identifying the characteristics of spill samples and establishing their correlation to suspected source oils. Even when samples or data from suspected sources are not available for comparison, establishing the specific nature (e.g. refined petroleum, crude oil, waste oil, etc.) of the spilled oil still helps to constrain the possible source(s). This methodology is restricted to petroleum related products containing a significant proportion of hydrocarbon-components with a boiling point above 150 Ā°C. Examples are: crude oils, higher boiling condensates, diesel oils, residual bunker or heavy fuel oils, lubricants, and mixtures of bilge and sludge samples, as well as distillate fuels and blends. While the specific analytical methods are perhaps not appropriate for lower boiling oils (e.g. kerosene, jet fuel, or gasoline), the general concepts described in this methodology, i.e. statistical comparison of weathering-resistant diagnostic ratios, are applicable in spills involving these kinds of oils. Paraffin based products (e.g. waxes, etc.) are outside the scope of this method because too many compounds are removed during the production process [37]. However, the method can be used to identify the type of product involved. Although not directly intended for identifying oil recovered from groundwater, vegetation, wildlife/tissues, soil, or sediment matrices, they are not precluded. However, caution is needed as extractable compounds can be present in these matrices that alter and/or contribute additional compounds compared to the source sample. If unrecognized, the contribution from the matrix can lead to false ā€œnon-matchesā€. It is therefore advisable to analyse background sample(s) of the matrix that appear unoiled. When analysing ā€œnon-oilā€ matrices additional sample preparation (e.g. clean-up) is often required prior to analysis and the extent to which the matrix affects the correlation achieved is to be considered. Whether the method is applicable for a specific matrix depends upon the oil concentration compared to the ā€œmatrix concentrationā€. In matrices containing high concentrations of oil, a positive match can still be concluded. In matrices containing lower concentrations of oil, a false ā€œnon-matchā€ or an ā€œinconclusive matchā€ can result from matrix effects. Evaluation of possible matrix effects is beyond the scope of this document.

PDF Catalog

PDF Pages PDF Title
2 undefined
14 1 Scope
2 Normative references
15 3 Terms and definitions
3.1 General
17 3.2 Sample comparison
3.3 Abbreviations
18 4 Strategy for the identification of oil spill sources
4.1 General
19 4.2 Basis for reliable conclusions ā€“ Numerical comparisons
20 5 General lab instructions
5.1 Sampling and sample preparation
5.2 GC-FID and GC-MS analysis
22 5.3 Conclusions and reporting
6 Sample preparation
6.1 General
6.2 Visual examination and description of samples
23 6.3 Preparation
6.3.1 Sample storage
6.3.2 Water samples
24 6.3.3 Oil samples from an Ethylene-tetrafluorethylene (ETFE) net
6.3.4 Thick oil and emulsified oil samples
6.3.5 Tar balls and emulsified lumps
25 6.3.6 Samples from oiled birds, fish and other animals and vegetation
6.3.7 Sediment
6.4 Sample clean-up
6.4.1 General
6.4.2 Particle removal
26 6.4.3 Asphaltenes precipitation
6.4.4 Alumina column clean-up of biogenic materials
27 6.4.5 Silica or FlorisilĀ® column clean-up
28 6.5 Recommended injection concentration
29 7 Characterization and evaluation of analytical data
7.1 General
30 7.2 Characterization by GC-FID ā€“ Level 1
7.2.1 General
7.2.2 Evaluation of the influence of weathering on sample comparison
7.2.2.1 General
7.2.2.2 Chromatogram overlay ā€“ Level 1.1
31 7.2.2.3 Bar chart (histogram) ā€“ Level 1.2
33 7.2.2.4 GC-PW-plot ā€“ Level 1.2
7.2.3 Acyclic isoprenoids ratios ā€“ Level 1.2
34 7.2.4 Level 1 criteria
7.2.5 Level 1 conclusions
7.3 Characterization by GC-MS ā€“ Level 2
7.3.1 General
7.3.2 Visual inspection and overall characterization – Level 2.1
35 7.3.3 Treatment of the GC-MS results ā€“ Level 2.2
7.4 Treatment of the results using the MS-PW-plotā€“ Level 2.2
7.4.1 General
36 7.4.2 PW-plot calculations
7.4.3 Evaluation of the variability of the analysis and peak integration
38 7.4.4 Evaluation of weathering
39 7.5 Treatment of the results using diagnostic ratios ā€“ Level 2.2
7.5.1 General
40 7.5.2 Diagnostic ratios calculation
7.5.3 Normative diagnostic ratios
44 7.5.4 Analytical error
45 7.5.5 Match-criterion for ratios
46 7.5.6 Criteria for selecting, eliminating and evaluating diagnostic ratios
7.5.6.1 General
48 7.5.6.2 Elimination by means of a signal to noise (S/N) test
49 7.5.6.3 Elimination by means of the comparison of the duplicate analyses of extracts
7.5.6.4 Optional: Evaluation of diagnostic ratios using conventional or multivariate statistics
50 7.6 Conclusions
51 8 Reporting
8.1 General
52 8.2 Internal documentation ā€“ technical report
53 8.3 Identification report ā€“ summary report
9 Quality assurance
55 Annex A (normative)GC-FID analysis
A.1 General
A.2 Analytical standards for GC-FID analyses
A.2.1 N-alkanes
56 A.2.2 Injection concentration of the standard GC-FID
A.2.3 Storage of frequently used standard solutions
A.3 Suggested instrumental conditions
57 A.4 Measures to improve and verify the accuracy of the method ā€“ GC-FID
A.4.1 Mass discrimination
58 A.4.2 Column resolution
60 A.4.3 Linearity
A.4.4 Mid-level concentration
61 A.4.5 Variance
A.4.6 GC-FID sequence
62 Annex B (normative)GC-MS analysis
B.1 General
B.2 Analytical standards for GC-MS analyses
B.2.1 General
63 B.2.2 Crude oil to be used around each sequence
B.2.3 Oil mixture
B.2.4 Analytical standards for PAH homologues
64 B.2.5 FAMEs
B.2.6 Storage of frequently used standard solutions
B.3 Suggested instrumental conditions
B.3.1 GC conditions for the exchange of analytical results
66 B.3.2 GC-MS conditions for full-scan analysis
67 B.3.3 MS preparation for selected ion monitoring (SIM) analysis
68 B.4 Measures to improve and verify the accuracy of the GC-MS method
B.4.1 Relative retention time
B.4.2 Mass discrimination
B.4.3 Peak symmetry and column resolution
69 B.4.4 Patterns
B.4.5 Linearity
B.4.6 Mid-level concentration
70 B.4.7 Variance
B.4.8 Sample analysis with GC-MS
71 Annex C (informative)Precision statement
C.1 General
C.2 Precision of the MS-PW-plot
72 C.3 Precision of the ratio comparison
73 C.4 Reproducibility
74 C.5 The effect of the ratio type on the RSD
75 C.6 Example of a paired ratio calculation in ExcelĀ®
76 C.7 Calculation of the evaporation line for the MS-PW-plot in ExcelĀ®
79 Annex D (normative)Evaluative reporting using match definitions or likelihood ratios
D.1 General
D.2 Match definitions
80 D.3 Likelihood ratios (LR)
82 Annex E (normative)List of compounds and compound groups analysed by GC-MS-SIM
E.1 General
83 E.2 Compounds
E.2.1 General
88 E.2.2 Compound type
89 E.3 Normative ratios and informative ratios.
93 Annex F (informative)Chromatograms and ratios of compounds and compound groups analysed by GC-MS-SIM
F.1 General
F.2 Alkanes
94 F.3 Cyclohexanes and polycyclic alkanes
100 F.4 Mono-aromatic and poly-aromatic compounds
F.4.2 PAHs, alkyl-PAHs and S-PAHs
111 F.4.3 Tri-aromatic steranes
112 F.5 FAMEs
116 Annex G (informative)General composition of oils ā€“ chemical groups
G.1 General
117 G.2 Hydrocarbons
G.3 Aliphatic compounds
G.3.1 General
G.3.2 Paraffins
G.3.3 Naphthenes
118 G.4 Aromatic compounds
G.5 Heteroatomic organic compounds
G.5.1 General
G.5.2 Resins
G.5.3 Asphaltenes
120 Annex H (informative)Weathering of oils spilled on water and land
H.1 General
H.2 Weathering processes
H.2.1 Weathering of oils spilled on water
122 H.2.2 Weathering of waterborne oils stranded on land or land based oil spills
H.2.3 Mixing and contamination
125 H.2.5 In-situ burning
126 H.3 Evaluation of weathering processes
H.3.1 Evaporation
129 H.3.2 Dissolution
131 H.3.3 Photo-oxidation
137 H.3.4 Biodegradation
140 H.3.5 Wax redistribution
146 H.3.6 Mixing
H.3.6.1 General
H.3.6.2 MS-PW-plot
148 H.3.6.3 Mixing tool
H.3.7 Contamination
H.3.8 In-situ burning
H.3.8.1 Background
H.3.8.2 Evaporation
149 H.3.8.3 Pyrogenic PAHs
151 Annex I (informative)Characteristic features of different oil types in oil spill identification
I.1 General
I.2 Crude oil
152 I.2.2 Analysis
I.2.2.1 Basics
I.2.2.2 GC screening
154 I.2.2.3 GC-MS analysis
157 I.2.2.4 Sulfur content of crude oils and oil products
158 I.3 Light fuel oil (gas oil, diesel, fuel No 2, biofuels, GTL)
I.3.1 General
159 I.3.2 Analysis, GC screening
161 I.3.3 GC-MS analysis
164 I.3.4 Biofuels
165 I.3.5 Gas to liquid products
166 I.4 Lubricating oil
I.4.1 General
168 I.4.2 Analysis
I.4.2.1 GC screening
169 I.4.2.2 GC-MS analysis
172 I.5 Heavy fuel oil (HFO, Bunker C, Fuel No 6) and low sulfur fuel oil
I.5.1 General
173 I.5.2 Analysis
I.5.2.1 Basics
174 I.5.2.2 Screening
176 I.5.2.3 GC-MS analysis
181 I.6 Waste oil (bilge oil, sludge, slops)
I.6.1 General
182 I.6.2 Analysis
I.6.2.1 GC screening
183 I.6.2.2 GC-MS analysis
186 I.7 Conclusion
188 Annex J (informative)Example of external documentation ā€“ identification report of an oil spill case
J.1 General
J.2 Sample information
J.3 Analytical procedure
J.3.1 Method
J.3.2 Dilution/extraction
J.3.3 Analyses
J.4 Results
J.5 Interpretation
J.5.1 General
189 J.5.2 Positive match
J.5.3 Probable match
J.5.4 Inconclusive
J.5.5 Non-match
J.6 Conclusions
191 Annex K (informative)Example of internal documentation ā€“ technical report of an oil spill case
K.1 General
K.2 Sample information
K.2.1 Samples
K.2.2 Contact information
K.2.3 Request
192 K.2.4 Photo(s) of the samples
K.3 Sample preparation and analyses
194 K.4 Quality assurance
196 K.5 GC-FID results ā€“ Level 1
K.5.1 GC-FID chromatograms ā€“ Level 1.1
198 K.5.2 GC-FID numerical comparisons ā€“ Level 1.2
K.5.2.1 Duplicate comparisons
200 K.5.2.2 Bilge and water samples comparison
201 K.5.2.3 Comparison of the water samples relative to sample Bilge main
202 K.5.2.4 Comparison of the water samples relative to sample Bilge front
203 K.5.3 GC-FID conclusions
204 K.6 GC-MS results ā€“ Level 2
K.6.1 General
K.6.2 GC-MS chromatograms ā€“ Level 2.1
205 K.6.3 GC-MS numerical comparisons ā€“ Level 2.2
K.6.3.1 Integration
206 K.6.3.2 Duplicate comparison
208 K.6.3.3 Bilge front compared with Water 1 and Water 2
209 K.6.3.4 Bilge main compared with Water 1 and Water 2
213 K.6.4 Visual inspection
214 K.6.5 Overall conclusions
K.6.5.1 Bilge front compared with Water 1 and Water 2
K.6.5.2 Bilge main compared with Water 1 and Water 2

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BS EN 15522-2:2023
$215.11