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BS EN 15522-2:2023 Oil spill identification. Petroleum and petroleum related products - Analytical method and interpretation of results based on GC-FID and GC-low resolution-MS analyses, 2023
- undefined
- 1 Scope
- 2 Normative references
- 3 Terms and definitions [Go to Page]
- 3.1 General
- 3.2 Sample comparison
- 3.3 Abbreviations
- 4 Strategy for the identification of oil spill sources [Go to Page]
- 4.1 General
- 4.2 Basis for reliable conclusions – Numerical comparisons
- 5 General lab instructions [Go to Page]
- 5.1 Sampling and sample preparation
- 5.2 GC-FID and GC-MS analysis
- 5.3 Conclusions and reporting
- 6 Sample preparation [Go to Page]
- 6.1 General
- 6.2 Visual examination and description of samples
- 6.3 Preparation [Go to Page]
- 6.3.1 Sample storage
- 6.3.2 Water samples
- 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
- 6.3.6 Samples from oiled birds, fish and other animals and vegetation
- 6.3.7 Sediment
- 6.4 Sample clean-up [Go to Page]
- 6.4.1 General
- 6.4.2 Particle removal
- 6.4.3 Asphaltenes precipitation
- 6.4.4 Alumina column clean-up of biogenic materials
- 6.4.5 Silica or Florisil® column clean-up
- 6.5 Recommended injection concentration
- 7 Characterization and evaluation of analytical data [Go to Page]
- 7.1 General
- 7.2 Characterization by GC-FID – Level 1 [Go to Page]
- 7.2.1 General
- 7.2.2 Evaluation of the influence of weathering on sample comparison [Go to Page]
- 7.2.2.1 General
- 7.2.2.2 Chromatogram overlay – Level 1.1
- 7.2.2.3 Bar chart (histogram) – Level 1.2
- 7.2.2.4 GC-PW-plot – Level 1.2
- 7.2.3 Acyclic isoprenoids ratios – Level 1.2
- 7.2.4 Level 1 criteria
- 7.2.5 Level 1 conclusions
- 7.3 Characterization by GC-MS – Level 2 [Go to Page]
- 7.3.1 General
- 7.3.2 Visual inspection and overall characterization - Level 2.1
- 7.3.3 Treatment of the GC-MS results – Level 2.2
- 7.4 Treatment of the results using the MS-PW-plot– Level 2.2 [Go to Page]
- 7.4.1 General
- 7.4.2 PW-plot calculations
- 7.4.3 Evaluation of the variability of the analysis and peak integration
- 7.4.4 Evaluation of weathering
- 7.5 Treatment of the results using diagnostic ratios – Level 2.2 [Go to Page]
- 7.5.1 General
- 7.5.2 Diagnostic ratios calculation
- 7.5.3 Normative diagnostic ratios
- 7.5.4 Analytical error
- 7.5.5 Match-criterion for ratios
- 7.5.6 Criteria for selecting, eliminating and evaluating diagnostic ratios [Go to Page]
- 7.5.6.1 General
- 7.5.6.2 Elimination by means of a signal to noise (S/N) test
- 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
- 7.6 Conclusions
- 8 Reporting [Go to Page]
- 8.1 General
- 8.2 Internal documentation – technical report
- 8.3 Identification report – summary report
- 9 Quality assurance
- Annex A (normative)GC-FID analysis [Go to Page]
- A.1 General
- A.2 Analytical standards for GC-FID analyses [Go to Page]
- A.2.1 N-alkanes
- A.2.2 Injection concentration of the standard GC-FID
- A.2.3 Storage of frequently used standard solutions
- A.3 Suggested instrumental conditions
- A.4 Measures to improve and verify the accuracy of the method – GC-FID [Go to Page]
- A.4.1 Mass discrimination
- A.4.2 Column resolution
- A.4.3 Linearity
- A.4.4 Mid-level concentration
- A.4.5 Variance
- A.4.6 GC-FID sequence
- Annex B (normative)GC-MS analysis [Go to Page]
- B.1 General
- B.2 Analytical standards for GC-MS analyses [Go to Page]
- B.2.1 General
- B.2.2 Crude oil to be used around each sequence
- B.2.3 Oil mixture
- B.2.4 Analytical standards for PAH homologues
- B.2.5 FAMEs
- B.2.6 Storage of frequently used standard solutions
- B.3 Suggested instrumental conditions [Go to Page]
- B.3.1 GC conditions for the exchange of analytical results
- B.3.2 GC-MS conditions for full-scan analysis
- B.3.3 MS preparation for selected ion monitoring (SIM) analysis
- B.4 Measures to improve and verify the accuracy of the GC-MS method [Go to Page]
- B.4.1 Relative retention time
- B.4.2 Mass discrimination
- B.4.3 Peak symmetry and column resolution
- B.4.4 Patterns
- B.4.5 Linearity
- B.4.6 Mid-level concentration
- B.4.7 Variance
- B.4.8 Sample analysis with GC-MS
- Annex C (informative)Precision statement [Go to Page]
- C.1 General
- C.2 Precision of the MS-PW-plot
- C.3 Precision of the ratio comparison
- C.4 Reproducibility
- C.5 The effect of the ratio type on the RSD
- C.6 Example of a paired ratio calculation in Excel®
- C.7 Calculation of the evaporation line for the MS-PW-plot in Excel®
- Annex D (normative)Evaluative reporting using match definitions or likelihood ratios [Go to Page]
- D.1 General
- D.2 Match definitions
- D.3 Likelihood ratios (LR)
- Annex E (normative)List of compounds and compound groups analysed by GC-MS-SIM [Go to Page]
- E.1 General
- E.2 Compounds [Go to Page]
- E.2.1 General
- E.2.2 Compound type
- E.3 Normative ratios and informative ratios.
- Annex F (informative)Chromatograms and ratios of compounds and compound groups analysed by GC-MS-SIM [Go to Page]
- F.1 General
- F.2 Alkanes
- F.3 Cyclohexanes and polycyclic alkanes
- F.4 Mono-aromatic and poly-aromatic compounds [Go to Page]
- F.4.2 PAHs, alkyl-PAHs and S-PAHs
- F.4.3 Tri-aromatic steranes
- F.5 FAMEs
- Annex G (informative)General composition of oils – chemical groups [Go to Page]
- G.1 General
- G.2 Hydrocarbons
- G.3 Aliphatic compounds [Go to Page]
- G.3.1 General
- G.3.2 Paraffins
- G.3.3 Naphthenes
- G.4 Aromatic compounds
- G.5 Heteroatomic organic compounds [Go to Page]
- G.5.1 General
- G.5.2 Resins
- G.5.3 Asphaltenes
- Annex H (informative)Weathering of oils spilled on water and land [Go to Page]
- H.1 General
- H.2 Weathering processes [Go to Page]
- H.2.1 Weathering of oils spilled on water
- H.2.2 Weathering of waterborne oils stranded on land or land based oil spills
- H.2.3 Mixing and contamination
- H.2.5 In-situ burning
- H.3 Evaluation of weathering processes [Go to Page]
- H.3.1 Evaporation
- H.3.2 Dissolution
- H.3.3 Photo-oxidation
- H.3.4 Biodegradation
- H.3.5 Wax redistribution
- H.3.6 Mixing [Go to Page]
- H.3.6.1 General
- H.3.6.2 MS-PW-plot
- H.3.6.3 Mixing tool
- H.3.7 Contamination
- H.3.8 In-situ burning [Go to Page]
- H.3.8.1 Background
- H.3.8.2 Evaporation
- H.3.8.3 Pyrogenic PAHs
- Annex I (informative)Characteristic features of different oil types in oil spill identification [Go to Page]
- I.1 General
- I.2 Crude oil [Go to Page]
- I.2.2 Analysis [Go to Page]
- I.2.2.1 Basics
- I.2.2.2 GC screening
- I.2.2.3 GC-MS analysis
- I.2.2.4 Sulfur content of crude oils and oil products
- I.3 Light fuel oil (gas oil, diesel, fuel No 2, biofuels, GTL) [Go to Page]
- I.3.1 General
- I.3.2 Analysis, GC screening
- I.3.3 GC-MS analysis
- I.3.4 Biofuels
- I.3.5 Gas to liquid products
- I.4 Lubricating oil [Go to Page]
- I.4.1 General
- I.4.2 Analysis [Go to Page]
- I.4.2.1 GC screening
- I.4.2.2 GC-MS analysis
- I.5 Heavy fuel oil (HFO, Bunker C, Fuel No 6) and low sulfur fuel oil [Go to Page]
- I.5.1 General
- I.5.2 Analysis [Go to Page]
- I.5.2.1 Basics
- I.5.2.2 Screening
- I.5.2.3 GC-MS analysis
- I.6 Waste oil (bilge oil, sludge, slops) [Go to Page]
- I.6.1 General
- I.6.2 Analysis [Go to Page]
- I.6.2.1 GC screening
- I.6.2.2 GC-MS analysis
- I.7 Conclusion
- Annex J (informative)Example of external documentation – identification report of an oil spill case [Go to Page]
- J.1 General
- J.2 Sample information
- J.3 Analytical procedure [Go to Page]
- J.3.1 Method
- J.3.2 Dilution/extraction
- J.3.3 Analyses
- J.4 Results
- J.5 Interpretation [Go to Page]
- J.5.1 General
- J.5.2 Positive match
- J.5.3 Probable match
- J.5.4 Inconclusive
- J.5.5 Non-match
- J.6 Conclusions
- Annex K (informative)Example of internal documentation – technical report of an oil spill case [Go to Page]
- K.1 General
- K.2 Sample information [Go to Page]
- K.2.1 Samples
- K.2.2 Contact information
- K.2.3 Request
- K.2.4 Photo(s) of the samples
- K.3 Sample preparation and analyses
- K.4 Quality assurance
- K.5 GC-FID results – Level 1 [Go to Page]
- K.5.1 GC-FID chromatograms – Level 1.1
- K.5.2 GC-FID numerical comparisons – Level 1.2 [Go to Page]
- K.5.2.1 Duplicate comparisons
- K.5.2.2 Bilge and water samples comparison
- K.5.2.3 Comparison of the water samples relative to sample Bilge main
- K.5.2.4 Comparison of the water samples relative to sample Bilge front
- K.5.3 GC-FID conclusions
- K.6 GC-MS results – Level 2 [Go to Page]
- K.6.1 General
- K.6.2 GC-MS chromatograms – Level 2.1
- K.6.3 GC-MS numerical comparisons – Level 2.2 [Go to Page]
- K.6.3.1 Integration
- K.6.3.2 Duplicate comparison
- K.6.3.3 Bilge front compared with Water 1 and Water 2
- K.6.3.4 Bilge main compared with Water 1 and Water 2
- K.6.4 Visual inspection
- K.6.5 Overall conclusions [Go to Page]
- 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 [Go to Page]
