Numerous unidentified white blobs were discovered along Ship Cove Beach, Newfoundland, Canada, in September 2024. Fueled by national and international media coverage and public speculation, this incident raised concerns about potential health, safety, and environmental impacts. A comprehensive forensic analysis was conducted using physicochemical characterization, spectroscopy, mass spectrometry, and elemental analysis to determine the composition, nature, and possible origin of the material. The chemical fingerprinting results indicate the following: (1) the sample is unlikely to be petroleum-derived or contaminated by petroleum products; (2) biodiesel is improbable due to the absence of significant fatty acid methyl esters; (3) the material does not appear to be silicone-based or chlorinated (e.g., silicone sealants or chlorinated vinyl compounds); (4) the presence of aldehydes, fatty acids, and plant-derived sterols-coupled with the absence of cholesterol-suggests a plant oil-based origin; (5) high molecular weight compounds and thermal transformation behavior point to the presence of polymeric materials; and (6) the substance is neither flammable, combustible, corrosive, oxidizing, nor radioactive. These findings contribute to understanding the nature of the spill and highlight the utility of multidisciplinary forensic approaches in environmental incident response.

This study investigates the 2020 oil spill near Postville, Labrador, using forensic chemical fingerprinting to identify the source of contamination. Petroleum hydrocarbons and biomarker profiling were applied to characterize hydrocarbon signatures in environmental samples and compare them with potential sources. Hydrocarbon group analysis excluded gasoline and lubricating oil, while n-alkane distributions and diagnostic ratios indicated a strong correlation with kerosene. Low levels of terpanes, and hopanes, and polycyclic aromatic hydrocarbons (PAHs) most abundant with low molecular weight congeners were found in most environment samples, consistent with light fuel oils, like kerosene and marine diesel. Diamantane and bicyclic sesquiterpene ratios aligned with both kerosene and marine diesel. Bilge water contained hetero-sulfur alkylated PAHs and aromatic steranes, differing from kerosene and marine diesel. Multivariate analyses, including principal component and hierarchical clustering, confirmed the strongest link to light fuel oils, kerosene and marine diesel, both are the possible sources for most environmental samples. These findings demonstrate the effectiveness of oil forensic techniques in source attribution and environmental management.

Total petroleum hydrocarbons (TPH), n-alkanes, petroleum biomarkers, and polycyclic aromatic hydrocarbons (PAHs) were analyzed in 63 intertidal zone sediments from the southeast shoreline of Vancouver Island and the nearby Southern Gulf Islands, British Columbia (BC), Canada, using gas chromatography coupled with a flame ionization detector and mass spectrometry. All sites had TPH levels much lower than the Canadian Council of Ministers of the Environment thresholds for fine- and coarse-grained soils in agricultural and natural areas. Terrestrial plants were the main source of n-alkanes, though petrogenic n-alkanes were found in 13 % of 63 samples, as indicated by the carbon preference index (CPI) and related characteristics. PAHs primarily originated from pyrogenic input, with some locations showing mixed petrogenic and pyrogenic inputs based on analyzing diagnostic ratios, like pyrogenic index and certain isomer ratios. Petroleum contamination was evident at sites with intensive human activities or oil spill history, such as Cowichan Bay, Octopus Point, Medicine Beach, Fulford Harbor, East Portland, Separation Point, Maple Bay, and Aldridge Point, marked by significant levels of petroleum biomarkers, petrogenic n-alkanes, and PAHs. While all PAHs pose minimal risk to benthic organisms, compounds like naphthalene, 2-methyl naphthalene, and certain 3-6 ring PAHs could potentially affect them at certain sites from Cowichan Bay, East Portland, Separation Point, Medicine Beach, and Maple Bay.

The forensic investigation of hazardous noxious substances (HNS) is paramount for an effective response to chemical spill emergencies and other accidents. Analyzing unknown emergency samples poses a challenge due to the limited availability of background information, making the selection of appropriate sample preparation and analytical methodologies difficult. The utilization of high-resolution mass spectrometers (HRMS) in screening both target and non-target substances proves instrumental in revealing hazardous substances that may be overlooked alongside the intended analytes. In this study, a gas chromatography-quadruple time-of-flight mass spectrometer (GC-QTOF-MS) was employed to identify numerous organic compounds in an indoor dust sample. The compounds detected encompassed normal alkanes, fatty acids (saturated and unsaturated), alcohols, phenols, sterols, drugs, polycyclic aromatic hydrocarbons (PAHs), pesticides, flame retardants (such as polybrominated biphenyl ethers, PBDEs), plasticizers (such as phthalates and phosphates), among others. Notably, concentrations of n-alkanes, fatty acids, and phthalates were relatively high, while PAHs and pesticides were present at trace levels. The application of GC-QTOF-MS provides a swift and confirmative approach for analyzing target, suspect, and non-target compounds in both routine and emergency scenarios. This methodology proves invaluable in enhancing our capability to comprehensively assess and address chemical incidents, ensuring a more thorough and accurate response.

The physicochemical properties of a renewable diesel (RD) and several petroleum diesel (PD)-dominant diesels were examined to assess the feasibility of identifying and quantifying the presence of RD and biodiesel from PD and their blends. Relative to all PD-dominant diesels, the RD exhibited a lower density, a higher flash point, reduced evaporation loss and a comparable viscosity and water content. The studied RD contained a limited amount of aromatics, with aliphatic hydrocarbons predominantly within the C-15 to C(18 )range. Most individual petroleum hydrocarbons were detected in the PD-dominant diesels, whereas the most abundant hydrocarbons for the RD were alkanes in the <n-C-19 carbon range. The typical chemical signature of RD includes clustered peaks within the C-15 to C-18 range on GC/FID chromatograms coupled with a sharp decline in the abundance of n-al-kanes from -n-C-19 and heavier. These properties are robust indicators of RD, even in RD/PD blends. However, quantifying the RD/PD blending ratios is challenging because of their overlapping chemical compositions. The quantified blending ratios for the blended biodiesel/PD are close to theoretical biodiesel ratios. Our analyses provide valuable insights into the forensic identification of RD, biodiesel, PD and their blends

With the implementation of stringent environmental regulations, high sulfur fuel oils (HSFO) are shifted to very low (VLSFOs) and ultralow sulfur fuel oils (ULSFOs). The current understanding of these fuels is far from suf-ficient. The chemical fingerprints of these oils are significantly altered by desulfurization processes, and sulfur-containing compounds present in these oils are in low or extremely low concentrations. These changes pose challenges for petroleum analysis. The ULSFOs studied were limited to distillates. Like conventional fuel oils, ULSFOs are diverse. ULSFOs do not just include distillates but can be a mixture of multiple oil products. The present work measured and compared the physical and chemical properties of ULSFOs with conventional fuels. Gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS) was applied to characterize the chemical fingerprints of ULSFOs. Polycyclic aromatic sulfur heterocycles (PASHs) and their alkylated ho-mologues were determined in considerable abundance in the oils with <= 1,000 ppm and <= 500 ppm of total sulfur. The chromatographic profiles of ULSFOs were obviously different from that of crude oil and high sulfur fuel oil. Most of PASHs are barely detectable in <= 10 ppm S ultralow sulfur diesel fuels (ULSDs), which were subject to deep desulfurization. Some dibenzothiophene isomers such as 4-methyldibenzothiophene,4,6-dime-thyldibenzothiophene and 2,4,6-trimethyldibenzothiophene naturally occur in relatively high abundance and are the most refractory to the refinery process due to the methyl steric hindrance. These refractory species were clearly detected in <= 10 ppm S ULSDs while other PASHs are barely detectable. Certain compounds with special chemical fingerprints in ULSFOs and ULSDs have potential suitability as diagnostic molecular markers for associated oil spill characterization and identification.

In many jurisdictions, dispersants are included in contingency plans as a viable countermeasure that can help reduce the overall environmental impact of marine oil spills. When used, it is imperative to monitor the progression of dispersant and oil to assess their environmental fate and behaviour. Amphiphilic salt dioctyl sodium sulfosuccinate (DOSS) is the major effective component of the most commonly available dispersants, such as Corexit® EC9500A. Without proper sample preparation, dispersed oil in water samples could interfere with the accurate analysis of DOSS and easily contaminate the LC-MS system. In this work, solid phase extraction (SPE) weak anion exchange (WAX) cartridges were used to separate oil and DOSS in aqueous samples. DOSS was accurately determined by liquid chromatography coupled with a high resolution Orbitrap mass spectrometer (LC-HRMS). Oil fingerprinting analysis was conducted and total petroleum hydrocarbons (TPHs), polycyclic aromatic hydrocarbons (PAHs), and petroleum biomarkers were determined by gas chromatography-flame ionization detection (GC-FID) and mass spectrometry (GC-MS). This SPE-LC/GC-MS method was used for the analysis of oil-dispersant water samples containing a mixture of Corexit® EC9500A and a selection of crude oils and refined petroleum products. Nearly a 100% DOSS recovery was obtained for various oil-surfactant conditions. Parallel quantitation of oils with dispersants was achieved using this method. A portion of the TPH loss was possibly attributed to oil retained by the SPE column. Chemical fingerprints and diagnostic ratios of target compounds in recovered dispersed oil overall remain unchanged compared with those of all studied oils.

Steam assisted gravity drainage (SAGD) is an energy and water intensive oil recovery technology for in-situ extraction of oil sands bitumen. It is essential to recycle the SAGD produced water (PW) to reduce water consumption and improve the energy efficiency of the process. This work investigated the removal of residual organic matter (ROM) in the SAGD-PW by the ceramic nanofiltration (NF) membrane process. The overall removal efficiency of ROM in the SAGD-PW was influenced by their polarities, membrane pore size, and membrane material. Non-polar oil components including saturated and aromatic hydrocarbons were completely removed; meanwhile, approximately 80% of polar components were removed by the membrane nanofiltration. Membrane nanofiltration significantly altered the chemical composition of the SAGD-PW by removing 95.0–98.3% of total solvent extracted material (TSEM). The chemical fingerprints of the solvent extracted materials in the feed and permeate samples were characterized. The profile of polar components such as naphthenic acids (NAs) in the permeate samples is significantly different from that in the feed samples.

Total petroleum hydrocarbons (TPH), n-alkanes, petroleum biomarkers, and polycyclic aromatic hydrocarbons (PAHs) were analyzed in the sediments collected from the shorelines and bottom of St. Clair River, Ontario, Canada. Most of the sampling sites had low TPH (< 20 μg/g). River bottom sediment usually had higher level of TPHs, total alkanes, total biomarkers, and total PAHs than most of the shoreline ones. Mixed biogenic and petrogenic n-alkanes were present in all the sites. Most sites had trace amounts of petroleum biomarkers. Mixed pyrogenic and petrogenic inputs with the predominant petroleum, have contributed to the detected PAHs at all sampling sites. PAHs detected would not show potential toxicity to benthic organisms in all shoreline sampling sites; however, some light molecular weight PAHs (e.g., phenanthrene, 2-methyl naphthalene, and acenaphthylene) are anticipated to have possible adverse impacts to sediment-dwelling organisms in part of the river bottom sediment.

ABSTRACT Environment and Climate Change Canada (ECCC) has developed a series of field guides to provide technical support tools for decisions regarding the evaluation of freshwater and marine shorelines and treatment options during an oil spill response. The new Freshwater Shoreline Response Guide is aligned with and complements the most recent editions of the ECCC Shoreline Cleanup Assessment Technique (SCAT) Manual (ECCC, 2018) and the ECCC Field Guide to Oil Spill Response on Marine Shorelines (ECCC, 2016). ECCC is engaged to provide science-based information to the spill response community and develop an expertise in spill response. The purpose of the Freshwater Shoreline Response Field Guide is to provide advice and guidance on the protection and treatment of freshwater shorelines threatened or affected by an oil spill. This Field Guide focuses on conventional tactics normally available to responders and appropriate for freshwater shoreline environments. The content of the Field Guide is organized to describe key elements of: Health and safety for field teamsNet Environmental Benefit Analysis (NEBA) / Spill Impact Mitigation Assessment (SIMA)Freshwater environmentsOil fate and behaviour in freshwater environmentsResponse – planning, treatment, special topics, and completion and monitoring

The characterization, occurrence, fate and behaviour of spilled oil in the affected boreal freshwater ecosystem were investigated in this study following a spill in March 2015, in Gogama, Ontario, Canada. A physicochemical property analysis of the source oil showed that the spilled oil was consistent with a conventional light oil. Oil samples collected immediately following the spill had lost their relatively light molecular alkanes and polycyclic aromatic hydrocarbons (PAHs) due to evaporation or dissolution. Twenty months post-spill, oil contamination levels decreased at sites located furthest from the accident site. Most of the sampling sites close to the incident site contained lightly weathered source oil, while some sediment contained heavily weathered source oil. Biogenic and pyrogenic inputs were also present in all the oil-contaminated sediments, where light molecular weight hydrocarbons had higher loss rates than heavy ones. Branched alkanes were more resistant to loss than corresponding straight isomers. Water samples usually had a lower loss of both alkylated PAHs and alkanes than in the underlying sediments. This difference can be ascribed to the fractionation of petroleum hydrocarbons between being deposited in sediment, and being released into water phases, especially when oils were freshly released into the water phase by disturbing bottom sediment. Aside from the rapid loss through evaporation and dissolution, microbial degradation was the major weathering process causing the loss of hydrocarbons 20 months after the spill.

Purpose This study aimed to investigate the occurrence, fate, and behaviour of oil components 46 years post-spill by analysing polar naphthenic acid fraction components (NAFCs). Methods Oil residues and sediment samples were collected from the shoreline of Chedabucto Bay, Nova Scotia, Canada, at sites affected by the 1970 Arrow oil spill, in June 2016. Sediments were extracted with Soxhlet extraction; NAFCs were separated through a silica gel column firstly, then analysed by high-performance liquid chromatography–high-resolution mass spectrometry (HPLC-HRMS). Results and discussion In all samples, the most abundant NAFC species were those having only oxygen as the heteroatom ( O o species, o indicating the number of oxygen atoms, from 1 to 8) and a high degree of saturation. O 2 species accounted for 50–70% of all O o species. NAFCs with sulphur heteroatoms were the second abundant species, then by those containing both nitrogen and oxygen heteroatoms. NAFCs in most Arrow oil residues had higher levels of oxygen species, especially for heavier molecular weight congeners, than the oil remaining stored in the sunken tanker. Environmental sediment samples, collected from near a marina away from the spill site, mainly contained a biological contribution with obviously recent petroleum oil input, whereas all Arrow oil residues were composed mainly of NAFCs that are characteristic of petroleum, and varied abundance between sites. Conclusions Characteristics of NAFCs from different sources varied from each other. Site-specific environmental conditions played a major role in controlling the fate and behaviour of oil components, including NAFCs.

In June 2016, oil residues and sediment samples were collected from the shoreline of Chedabucto Bay, Nova Scotia, Canada, at sites affected by the 1970 Arrow oil spill. This study aimed to investigate the occurrence, fate, and behaviour of oil components 45 years post-spill by analysing polar naphthenic acid fraction components (NAFCs) through high-performance liquid chromatography–high-resolution mass spectrometry (HPLC–HRMS). In all samples, the most abundant NAFC species were those having only oxygen as the heteroatom ( O o species, o indicating the number of oxygen atoms, from 1 to 8) and a high degree of saturation. NAFC species only containing two oxygen atoms (O 2 ) accounted for 50–70% of all O o species. The abundance of all remaining species was negligible compared with O o species. NAFCs in most Arrow oil residues had higher levels of oxygen species than the oil remaining stored in the sunken tanker. Environmental sediment samples collected from near a marina away from the spill site contained a dominant biological, whereas all Arrow oil residues were mainly composed of NAFCs that are characteristic of petroleum. The abundance of NAFCs in the Arrow oil residues varied between sites, confirming that site-specific environmental conditions play a major role in controlling the fate and behaviour of oil components, including NAFCs.

The Fraser River Delta is a unique and dynamic region supporting the diverse ecosystems and habitats in the Canadian West Coast. Total petroleum hydrocarbons (TPH), n-alkanes, petroleum biomarkers, and polycyclic aromatic hydrocarbons (PAHs) were analyzed for the intertidal sediments taken from the shorelines of the Delta area, British Columbia, Canada, to establish the baseline background data. Most of the sampling sites had low TPH (< 40 μg/g); only two samples had TPH from 100 to 150 μg/g. Mainly biogenic n-alkanes were present in all sites. Non-detectable to trace amounts of petroleum biomarkers were found at most sites. Mixed pyrogenic and petrogenic inputs contributed to the presence of PAHs at most sites. PAHs are not present in amounts anticipated negative effects to benthic organisms in all sampling sites, except that benzo (a) pyrene (BaP) from the upper intertidal zone (UIZ) of Burnaby Fraser Foreshore Park may have possible adverse biological effects.

The 1970 SS Arrow incident in Chedabucto Bay, Nova Scotia (NS) was a milestone event in Canada's oil spill response history and has been used by Environment and Climate Change Canada (ECCC) for ongoing research for almost 50 years. In August of 2015, the remaining sunken section of the SS ARROW released Bunker C oil from its tanks and some sections of shorelines impacted in 1970 were affected once again. The Canadian Coast Guard led the 2015 response effort, which included Shoreline Clean-Up and Assessment Technique (SCAT) surveys, to evaluate the contamination on the shorelines of Chedabucto Bay. This poster presents an overview of the 1970 event as well as the shoreline contamination resulting from the 2015 release from the SS Arrow. It summarizes the SCAT survey results and the operational response of the ECCC's National Environmental Emergencies Centre (NEEC) in support of the incident.

In 1985, the MV Manolis L ran aground and sank on Blow Hard Rock near the Change Islands in Notre Dame Bay, Newfoundland and Labrador. From 2013 to 2016, the Canadian Coast Guard (CCG) conducted several operations to trap and recover oil leaking from the sunken tanker. Seventeen samples were collected between 2013 and 2016 from the sunken vessel to identify the oil source and evaluate the evolution of the physicochemical properties of the oil trapped in the sunken vessel. Most of the oils collected in 2016 and all the oils collected from 2013 to 2015 were heavy fuel oils that had not undergone significant weathering (Group 1). Two oils collected in 2016 were identified as diesel oil in terms of their hydrocarbon composition (Group 2). Other two oils collected in 2016 (Group 3) had similar hydrocarbon properties as Group 1 heavy fuel oils; however, they had greater quantities of biomarkers and GC-detectable total petroleum hydrocarbons (TPH) in the > n-C-34 fraction and a lower quantity of resolved components, such as n-alkanes and PAHs. Detailed chemical fingerprinting pointed to these samples as being heavy fractions of Group 1 oils that had settled into a residual layer or had weathered through evaporation loss. Neither the heavy fuel oil nor diesel oil experienced significant loss through photo-oxidation and biodegradation, even 31 years post-sinking. Physical deposition, evaporation, and/or dissolution, especially deposition, were the main factors altering the physicochemical properties of the heavy fuel oil trapped in the sunken vessel.

Polycyclic aromatic sulfur heterocycles (PASHs), as a group of major sulfur-containing compounds, widely occur in crude oil and its refined products. Accurate analyses of these petrochemical components play an important role in monitoring oil quality, forensic source identification, and assessment of environmental impact of an oil spill. PASHs occur at relatively lower abundances in most crude oils and refined petroleum products than their corresponding aromatic hydrocarbons and are co-eluted together with some petroleum hydrocarbons in chromatographic analysis, resulting in high uncertainty for their quantitation. Capillary gas chromatography coupled with a quadrupole time-of-flight mass spectrometry (GC-QTOF-MS) provides high resolution and high mass accuracy, which facilitates discrimination of the delicate mass defects of isobaric compounds with the same nominal mass and external matrix material. In this work, GC-QTOF-MS was applied to analyze bicyclic to pentacyclic PASHs including benzothiophenes, dibenzothiophenes, benzonaphthothiophenes, dinaphthothiophenes and their C1- to C4- alkylated homologues in a number of crude oils, refined petroleum products, and environmental samples. GC-QTOF-MS analysis substantially improved the identification confidence and reduced quantitation uncertainty of PASHs and polycyclic aromatic hydrocarbons (PAHs) by eliminating the interferences presented in nominal mass chromatograms.

Total petroleum hydrocarbons (TPH), n-alkanes, petroleum biomarkers, and polycyclic aromatic hydrocarbons (PAHs) were analyzed in the intertidal sediments of Burrard Inlet, Vancouver, British Columbia, Canada. Most of the sampling sites had low TPH (<40 μg/g). Only 10% of sampling sites, located nearby a harbour and densely populated areas, had relatively high TPH (<260 μg/g). Main biogenic n-alkanes were present in all the sites, except for the main petrogenic input in the sample from the upper intertidal zone (UIZ) of the Maplewood Mudflats. Most sites had trace amounts of petroleum biomarkers. Mixed pyrogenic and petrogenic inputs contributed to PAHs at most sites. PAHs did not show potential toxicity to benthic organisms at most sites; however, possible negative effects from some of the detected PAHs were found for the samples from the UIZs of the Maplewood Mudflats and Labour View Park, and from the lower intertidal zone (LIZ) of Gates Park.

Naphthenic acids (NAs) or naphthenic acid fraction compounds (NAFCs) are generally recognized as a family of cycloaliphatic carboxylic acids naturally occurring in petroleum. These acid extractable organics (AEOs) from petroleum industry activities including oil sands produced waters (OSPW) have led to increasing environmental concern in recent years due to their potential release into the environment. This study presents a characterization of naphthenic acids in a number of crude oils and refined petroleum products from various sources. NAs with unsaturated degree of z - 2 to z - 24 and carbon number ranging from 6 to 60 were determined by liquid chromatography-high resolution Orbitrap mass spectrometry (LC-HRMS). NA profiles generally vary from oil to oil. Conventional light crude oils generally contain low concentrations of NAs, while heavier crudes and oil sands bitumen contain significant levels of NAs. NAs in Federated and Alaska North Slope crude oils are relatively low with O-2-NA concentrations of 139 mu g/g and 419 mu g/g, respectively, while their abundances are as high as 7994 mu g/g in Venezuelan Orinoco bitumen. The ratio of even to odd (E/O) carbon number NAs in all petroleum oils studied is close to 1.0 for z - 2 to z - 24 NAs. NA series z 0 to z - 12 in bitumen account for about 90% of the total determined NAs, and z - 14 to z - 24 NAs make up the remaining similar to 10%. Moreover, z - 2 similar to - 6 (1- to 3-ring) NAs are the most predominant in all oil samples. In terms of distribution according to carbon number, C-6 to C-21 NAs (alpha-group) make up about 44.2% of the total NAs in an Alberta oil sands bitumen. Caustic extraction of oil sands bitumen mostly transports the more toxic low-molecular weight portion of NAs into OSPW, in which alpha-group NAs constitute about 90% of the total NAs. Evaporation (up to 23.6% by weight) weathering slightly enriched the NAs but likely did not affect the distribution profile of NAs in a diluted bitumen (dilbit).