How Analytical Techniques are Helping Solve a Newfoundland Mystery

by , | Dec 11, 2024

Discover how analytical chemistry is unraveling the mystery of white blobs on the beach

In September 2024, white blobs, ranging in size up to around 15 centimeters in diameter, began washing ashore along Newfoundland’s beaches, prompting curiosity among locals and the broader community. To solve this mystery, Dr. Chris Kozak, a chemistry professor at Memorial University, Newfoundland, applied a suite of analytical techniques to study the chemical composition of the material in an attempt to identify its origin.

Initial Steps and Sample Preparation Challenges

The investigation began with basic sensory analysis—Kozak notes that the material had a distinct volatile hydrocarbon aroma, and the samples felt wet and tacky. From there, the team conducted solubility tests. “It’s important to determine the material’s solubility as this has a major influence on subsequent analysis,” says Kozak. “If it’s not soluble in common organic solvents, that would rule out liquid chromatography and even gas chromatography.”

Kozak describes attempts to dissolve the material in a range of organic solvents, including acetone, toluene, and dichloromethane. “It was very poorly soluble in almost every solvent we tried,” he reports. “Even in dimethyl sulfoxide, which most synthetic polymers will dissolve in, this material just swelled.” Eventually, the team resorted to using chloroform in an ultrasonic bath which broke down the material into small fragments suitable for analysis.

Determining the Chemical Composition

The first significant breakthrough came with the utilization of infrared spectroscopy (IR). “The IR results showed carbonyl groups, which pointed us toward a polyester or a polyurethane,” Kozak explains. He notes they also observed hydroxyl groups which was not surprising, considering the samples looked and felt as though they had a high moisture content.

The next experiment involved combustion elemental analysis. This confirmed the absence of nitrogen and sulfur, ruling out polyurethane or biological origins, and indicated the material contained 68% carbon, 10% hydrogen, and 22% oxygen.

In combustibility testing, the material melted but did not burn. “We attributed this to the high moisture content, confirmed by thermogravimetric analysis,” says Kozak. “With 18% moisture by mass, the material appeared to cure in the aqueous environment, trapping ocean water.” Heating above 100°C released the moisture, and decomposition occurred at around 300°C, leaving a 10% residue.

Next, a differential scanning calorimeter revealed that the material froze between 0 and -50°C. “There was a shift from a crystalline to glassy substance (as it warmed up from -50°C), so we did see a glass transition temperature,” advises Kozak. “So we had a very strong idea that it was going to be some sort of ester-containing polymer.”

To confirm these findings, the team used nuclear magnetic resonance (NMR) and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). “NMR showed no aromatic groups but revealed aliphatic protons and unsaturated alkenes,” says Kozak. “The MALDI-TOF results indicated the presence of vinyl acetate and fragments of synthetic rubber, such as isoprene and butadiene.” 

This data led the team to believe that the blobs were likely a mix of polyvinyl acetate and synthetic rubber—materials often used in industrial adhesives.

Environmental and Industrial Clues and Concerns

Kozak’s observations of embedded materials such as seaweed and pebbles led him to believe that the substance entered the ocean as a liquid and cured upon exposure to water. “The material wasn’t spongy (it lacked pores or open cells); it formed a solid monolith, trapping water at the molecular level,” he notes, speculating that the source may have been an industrial adhesive spill.

The mystery of how this material ended up on Newfoundland’s shores remains unsolved, but the investigation has revealed critical insights. The identification of the material as an adhesive suggests this is a case of plastic pollution. This is particularly important as some early theories about the origin of the blobs assumed they came from a natural source. Reports of similar blobs continuing to wash ashore indicate an ongoing environmental challenge requiring further attention.

This investigation highlights the power of analytical methods in addressing environmental concerns. By employing techniques such as IR spectroscopy, NMR, and MALDI-TOF MS, Kozak and his team were able to piece together a major part of the puzzle.

Meet the Expert

Chris Kozak

Dr. Christopher Kozak is a professor of chemistry at Memorial University of Newfoundland in St. John’s, Canada. He obtained his B.Sc. in Biological Chemistry from McMaster University in Hamilton, Ontario in 1997. He then moved to The University of British Columbia in Vancouver to obtain his PhD. In 2002 he moved to the UK to perform postdoctoral research at the University of York, followed by a Natural Sciences and Engineering Research Council (NSERC) postdoctoral fellowship at The University of Oxford. In 2004, he moved back to Canada and took up a position as an Assistant Professor at Concordia University in Montreal, Quebec. In 2005 he moved to his current position at Memorial University. His research focuses on earth-abundant transition metal-catalyzed polymerization of renewable feedstocks including CO2, cyclic esters, anhydrides and epoxides. In 2020 he and a team of colleagues received funding from the Canada Foundation for Innovation and the provinces of Newfoundland and Labrador and Nova Scotia to create the Atlantic Canada Environmental and Sustainable Chemistry and Engineering Centre. This funding allowed for a massive investment in the core research instrumentation in the region, transforming the analytical capabilities at Memorial University.

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