{"id":430869,"date":"2024-10-20T07:25:09","date_gmt":"2024-10-20T07:25:09","guid":{"rendered":"https:\/\/pdfstandards.shop\/product\/uncategorized\/bs-en-15522-22023\/"},"modified":"2024-10-26T14:05:54","modified_gmt":"2024-10-26T14:05:54","slug":"bs-en-15522-22023","status":"publish","type":"product","link":"https:\/\/pdfstandards.shop\/product\/publishers\/bsi\/bs-en-15522-22023\/","title":{"rendered":"BS EN 15522-2:2023"},"content":{"rendered":"
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 \u00b0C. 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 \u201cnon-matches\u201d. It is therefore advisable to analyse background sample(s) of the matrix that appear unoiled. When analysing \u201cnon-oil\u201d 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 \u201cmatrix concentration\u201d. In matrices containing high concentrations of oil, a positive match can still be concluded. In matrices containing lower concentrations of oil, a false \u201cnon-match\u201d or an \u201cinconclusive match\u201d can result from matrix effects. Evaluation of possible matrix effects is beyond the scope of this document.<\/p>\n
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2<\/td>\n | undefined <\/td>\n<\/tr>\n | ||||||
14<\/td>\n | 1 Scope 2 Normative references <\/td>\n<\/tr>\n | ||||||
15<\/td>\n | 3 Terms and definitions 3.1 General <\/td>\n<\/tr>\n | ||||||
17<\/td>\n | 3.2 Sample comparison 3.3 Abbreviations <\/td>\n<\/tr>\n | ||||||
18<\/td>\n | 4 Strategy for the identification of oil spill sources 4.1 General <\/td>\n<\/tr>\n | ||||||
19<\/td>\n | 4.2 Basis for reliable conclusions \u2013 Numerical comparisons <\/td>\n<\/tr>\n | ||||||
20<\/td>\n | 5 General lab instructions 5.1 Sampling and sample preparation 5.2 GC-FID and GC-MS analysis <\/td>\n<\/tr>\n | ||||||
22<\/td>\n | 5.3 Conclusions and reporting 6 Sample preparation 6.1 General 6.2 Visual examination and description of samples <\/td>\n<\/tr>\n | ||||||
23<\/td>\n | 6.3 Preparation 6.3.1 Sample storage 6.3.2 Water samples <\/td>\n<\/tr>\n | ||||||
24<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
25<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
26<\/td>\n | 6.4.3 Asphaltenes precipitation 6.4.4 Alumina column clean-up of biogenic materials <\/td>\n<\/tr>\n | ||||||
27<\/td>\n | 6.4.5 Silica or Florisil\u00ae column clean-up <\/td>\n<\/tr>\n | ||||||
28<\/td>\n | 6.5 Recommended injection concentration <\/td>\n<\/tr>\n | ||||||
29<\/td>\n | 7 Characterization and evaluation of analytical data 7.1 General <\/td>\n<\/tr>\n | ||||||
30<\/td>\n | 7.2 Characterization by GC-FID \u2013 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 \u2013 Level 1.1 <\/td>\n<\/tr>\n | ||||||
31<\/td>\n | 7.2.2.3 Bar chart (histogram) \u2013 Level 1.2 <\/td>\n<\/tr>\n | ||||||
33<\/td>\n | 7.2.2.4 GC-PW-plot \u2013 Level 1.2 7.2.3 Acyclic isoprenoids ratios \u2013 Level 1.2 <\/td>\n<\/tr>\n | ||||||
34<\/td>\n | 7.2.4 Level 1 criteria 7.2.5 Level 1 conclusions 7.3 Characterization by GC-MS \u2013 Level 2 7.3.1 General 7.3.2 Visual inspection and overall characterization – Level 2.1 <\/td>\n<\/tr>\n | ||||||
35<\/td>\n | 7.3.3 Treatment of the GC-MS results \u2013 Level 2.2 7.4 Treatment of the results using the MS-PW-plot\u2013 Level 2.2 7.4.1 General <\/td>\n<\/tr>\n | ||||||
36<\/td>\n | 7.4.2 PW-plot calculations 7.4.3 Evaluation of the variability of the analysis and peak integration <\/td>\n<\/tr>\n | ||||||
38<\/td>\n | 7.4.4 Evaluation of weathering <\/td>\n<\/tr>\n | ||||||
39<\/td>\n | 7.5 Treatment of the results using diagnostic ratios \u2013 Level 2.2 7.5.1 General <\/td>\n<\/tr>\n | ||||||
40<\/td>\n | 7.5.2 Diagnostic ratios calculation 7.5.3 Normative diagnostic ratios <\/td>\n<\/tr>\n | ||||||
44<\/td>\n | 7.5.4 Analytical error <\/td>\n<\/tr>\n | ||||||
45<\/td>\n | 7.5.5 Match-criterion for ratios <\/td>\n<\/tr>\n | ||||||
46<\/td>\n | 7.5.6 Criteria for selecting, eliminating and evaluating diagnostic ratios 7.5.6.1 General <\/td>\n<\/tr>\n | ||||||
48<\/td>\n | 7.5.6.2 Elimination by means of a signal to noise (S\/N) test <\/td>\n<\/tr>\n | ||||||
49<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
50<\/td>\n | 7.6 Conclusions <\/td>\n<\/tr>\n | ||||||
51<\/td>\n | 8 Reporting 8.1 General <\/td>\n<\/tr>\n | ||||||
52<\/td>\n | 8.2 Internal documentation \u2013 technical report <\/td>\n<\/tr>\n | ||||||
53<\/td>\n | 8.3 Identification report \u2013 summary report 9 Quality assurance <\/td>\n<\/tr>\n | ||||||
55<\/td>\n | Annex A (normative)GC-FID analysis A.1 General A.2 Analytical standards for GC-FID analyses A.2.1 N-alkanes <\/td>\n<\/tr>\n | ||||||
56<\/td>\n | A.2.2 Injection concentration of the standard GC-FID A.2.3 Storage of frequently used standard solutions A.3 Suggested instrumental conditions <\/td>\n<\/tr>\n | ||||||
57<\/td>\n | A.4 Measures to improve and verify the accuracy of the method \u2013 GC-FID A.4.1 Mass discrimination <\/td>\n<\/tr>\n | ||||||
58<\/td>\n | A.4.2 Column resolution <\/td>\n<\/tr>\n | ||||||
60<\/td>\n | A.4.3 Linearity A.4.4 Mid-level concentration <\/td>\n<\/tr>\n | ||||||
61<\/td>\n | A.4.5 Variance A.4.6 GC-FID sequence <\/td>\n<\/tr>\n | ||||||
62<\/td>\n | Annex B (normative)GC-MS analysis B.1 General B.2 Analytical standards for GC-MS analyses B.2.1 General <\/td>\n<\/tr>\n | ||||||
63<\/td>\n | B.2.2 Crude oil to be used around each sequence B.2.3 Oil mixture B.2.4 Analytical standards for PAH homologues <\/td>\n<\/tr>\n | ||||||
64<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
66<\/td>\n | B.3.2 GC-MS conditions for full-scan analysis <\/td>\n<\/tr>\n | ||||||
67<\/td>\n | B.3.3 MS preparation for selected ion monitoring (SIM) analysis <\/td>\n<\/tr>\n | ||||||
68<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
69<\/td>\n | B.4.4 Patterns B.4.5 Linearity B.4.6 Mid-level concentration <\/td>\n<\/tr>\n | ||||||
70<\/td>\n | B.4.7 Variance B.4.8 Sample analysis with GC-MS <\/td>\n<\/tr>\n | ||||||
71<\/td>\n | Annex C (informative)Precision statement C.1 General C.2 Precision of the MS-PW-plot <\/td>\n<\/tr>\n | ||||||
72<\/td>\n | C.3 Precision of the ratio comparison <\/td>\n<\/tr>\n | ||||||
73<\/td>\n | C.4 Reproducibility <\/td>\n<\/tr>\n | ||||||
74<\/td>\n | C.5 The effect of the ratio type on the RSD <\/td>\n<\/tr>\n | ||||||
75<\/td>\n | C.6 Example of a paired ratio calculation in Excel\u00ae <\/td>\n<\/tr>\n | ||||||
76<\/td>\n | C.7 Calculation of the evaporation line for the MS-PW-plot in Excel\u00ae <\/td>\n<\/tr>\n | ||||||
79<\/td>\n | Annex D (normative)Evaluative reporting using match definitions or likelihood ratios D.1 General D.2 Match definitions <\/td>\n<\/tr>\n | ||||||
80<\/td>\n | D.3 Likelihood ratios (LR) <\/td>\n<\/tr>\n | ||||||
82<\/td>\n | Annex E (normative)List of compounds and compound groups analysed by GC-MS-SIM E.1 General <\/td>\n<\/tr>\n | ||||||
83<\/td>\n | E.2 Compounds E.2.1 General <\/td>\n<\/tr>\n | ||||||
88<\/td>\n | E.2.2 Compound type <\/td>\n<\/tr>\n | ||||||
89<\/td>\n | E.3 Normative ratios and informative ratios. <\/td>\n<\/tr>\n | ||||||
93<\/td>\n | Annex F (informative)Chromatograms and ratios of compounds and compound groups analysed by GC-MS-SIM F.1 General F.2 Alkanes <\/td>\n<\/tr>\n | ||||||
94<\/td>\n | F.3 Cyclohexanes and polycyclic alkanes <\/td>\n<\/tr>\n | ||||||
100<\/td>\n | F.4 Mono-aromatic and poly-aromatic compounds F.4.2 PAHs, alkyl-PAHs and S-PAHs <\/td>\n<\/tr>\n | ||||||
111<\/td>\n | F.4.3 Tri-aromatic steranes <\/td>\n<\/tr>\n | ||||||
112<\/td>\n | F.5 FAMEs <\/td>\n<\/tr>\n | ||||||
116<\/td>\n | Annex G (informative)General composition of oils \u2013 chemical groups G.1 General <\/td>\n<\/tr>\n | ||||||
117<\/td>\n | G.2 Hydrocarbons G.3 Aliphatic compounds G.3.1 General G.3.2 Paraffins G.3.3 Naphthenes <\/td>\n<\/tr>\n | ||||||
118<\/td>\n | G.4 Aromatic compounds G.5 Heteroatomic organic compounds G.5.1 General G.5.2 Resins G.5.3 Asphaltenes <\/td>\n<\/tr>\n | ||||||
120<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
122<\/td>\n | H.2.2 Weathering of waterborne oils stranded on land or land based oil spills H.2.3 Mixing and contamination <\/td>\n<\/tr>\n | ||||||
125<\/td>\n | H.2.5 In-situ burning <\/td>\n<\/tr>\n | ||||||
126<\/td>\n | H.3 Evaluation of weathering processes H.3.1 Evaporation <\/td>\n<\/tr>\n | ||||||
129<\/td>\n | H.3.2 Dissolution <\/td>\n<\/tr>\n | ||||||
131<\/td>\n | H.3.3 Photo-oxidation <\/td>\n<\/tr>\n | ||||||
137<\/td>\n | H.3.4 Biodegradation <\/td>\n<\/tr>\n | ||||||
140<\/td>\n | H.3.5 Wax redistribution <\/td>\n<\/tr>\n | ||||||
146<\/td>\n | H.3.6 Mixing H.3.6.1 General H.3.6.2 MS-PW-plot <\/td>\n<\/tr>\n | ||||||
148<\/td>\n | 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 <\/td>\n<\/tr>\n | ||||||
149<\/td>\n | H.3.8.3 Pyrogenic PAHs <\/td>\n<\/tr>\n | ||||||
151<\/td>\n | Annex I (informative)Characteristic features of different oil types in oil spill identification I.1 General I.2 Crude oil <\/td>\n<\/tr>\n | ||||||
152<\/td>\n | I.2.2 Analysis I.2.2.1 Basics I.2.2.2 GC screening <\/td>\n<\/tr>\n | ||||||
154<\/td>\n | I.2.2.3 GC-MS analysis <\/td>\n<\/tr>\n | ||||||
157<\/td>\n | I.2.2.4 Sulfur content of crude oils and oil products <\/td>\n<\/tr>\n | ||||||
158<\/td>\n | I.3 Light fuel oil (gas oil, diesel, fuel No 2, biofuels, GTL) I.3.1 General <\/td>\n<\/tr>\n | ||||||
159<\/td>\n | I.3.2 Analysis, GC screening <\/td>\n<\/tr>\n | ||||||
161<\/td>\n | I.3.3 GC-MS analysis <\/td>\n<\/tr>\n | ||||||
164<\/td>\n | I.3.4 Biofuels <\/td>\n<\/tr>\n | ||||||
165<\/td>\n | I.3.5 Gas to liquid products <\/td>\n<\/tr>\n | ||||||
166<\/td>\n | I.4 Lubricating oil I.4.1 General <\/td>\n<\/tr>\n | ||||||
168<\/td>\n | I.4.2 Analysis I.4.2.1 GC screening <\/td>\n<\/tr>\n | ||||||
169<\/td>\n | I.4.2.2 GC-MS analysis <\/td>\n<\/tr>\n | ||||||
172<\/td>\n | I.5 Heavy fuel oil (HFO, Bunker C, Fuel No 6) and low sulfur fuel oil I.5.1 General <\/td>\n<\/tr>\n | ||||||
173<\/td>\n | I.5.2 Analysis I.5.2.1 Basics <\/td>\n<\/tr>\n | ||||||
174<\/td>\n | I.5.2.2 Screening <\/td>\n<\/tr>\n | ||||||
176<\/td>\n | I.5.2.3 GC-MS analysis <\/td>\n<\/tr>\n | ||||||
181<\/td>\n | I.6 Waste oil (bilge oil, sludge, slops) I.6.1 General <\/td>\n<\/tr>\n | ||||||
182<\/td>\n | I.6.2 Analysis I.6.2.1 GC screening <\/td>\n<\/tr>\n | ||||||
183<\/td>\n | I.6.2.2 GC-MS analysis <\/td>\n<\/tr>\n | ||||||
186<\/td>\n | I.7 Conclusion <\/td>\n<\/tr>\n | ||||||
188<\/td>\n | Annex J (informative)Example of external documentation \u2013 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 <\/td>\n<\/tr>\n | ||||||
189<\/td>\n | J.5.2 Positive match J.5.3 Probable match J.5.4 Inconclusive J.5.5 Non-match J.6 Conclusions <\/td>\n<\/tr>\n | ||||||
191<\/td>\n | Annex K (informative)Example of internal documentation \u2013 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 <\/td>\n<\/tr>\n | ||||||
192<\/td>\n | K.2.4 Photo(s) of the samples K.3 Sample preparation and analyses <\/td>\n<\/tr>\n | ||||||
194<\/td>\n | K.4 Quality assurance <\/td>\n<\/tr>\n | ||||||
196<\/td>\n | K.5 GC-FID results \u2013 Level 1 K.5.1 GC-FID chromatograms \u2013 Level 1.1 <\/td>\n<\/tr>\n | ||||||
198<\/td>\n | K.5.2 GC-FID numerical comparisons \u2013 Level 1.2 K.5.2.1 Duplicate comparisons <\/td>\n<\/tr>\n | ||||||
200<\/td>\n | K.5.2.2 Bilge and water samples comparison <\/td>\n<\/tr>\n | ||||||
201<\/td>\n | K.5.2.3 Comparison of the water samples relative to sample Bilge main <\/td>\n<\/tr>\n | ||||||
202<\/td>\n | K.5.2.4 Comparison of the water samples relative to sample Bilge front <\/td>\n<\/tr>\n | ||||||
203<\/td>\n | K.5.3 GC-FID conclusions <\/td>\n<\/tr>\n | ||||||
204<\/td>\n | K.6 GC-MS results \u2013 Level 2 K.6.1 General K.6.2 GC-MS chromatograms \u2013 Level 2.1 <\/td>\n<\/tr>\n | ||||||
205<\/td>\n | K.6.3 GC-MS numerical comparisons \u2013 Level 2.2 K.6.3.1 Integration <\/td>\n<\/tr>\n | ||||||
206<\/td>\n | K.6.3.2 Duplicate comparison <\/td>\n<\/tr>\n | ||||||
208<\/td>\n | K.6.3.3 Bilge front compared with Water 1 and Water 2 <\/td>\n<\/tr>\n | ||||||
209<\/td>\n | K.6.3.4 Bilge main compared with Water 1 and Water 2 <\/td>\n<\/tr>\n | ||||||
213<\/td>\n | K.6.4 Visual inspection <\/td>\n<\/tr>\n | ||||||
214<\/td>\n | 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 <\/td>\n<\/tr>\n<\/table>\n","protected":false},"excerpt":{"rendered":" Oil spill identification. Petroleum and petroleum related products – Analytical method and interpretation of results based on GC-FID and GC-low resolution-MS analyses<\/b><\/p>\n |