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Refined Tunable Methodology for Characterization of Contaminant–Particle Relationships in Surface Water

Christopher H. Marvina,*, Gary G. Lepparda,b, M. Marcia Westb,c, Gary A. Sternd, Adrienne R. Bodene and Brian E. McCarryf

a National Water Research Institute, Environment Canada, 867 Lakeshore Road, Burlington, ON, Canada L7R 4A6
b Department of Biology, McMaster University, Hamilton, ON, Canada L8S 4K1
c Electron Microscopy Facility, Faculty of Health Sciences, McMaster University, Hamilton, ON, Canada L8N 3Z5
d Freshwater Institute, Department of Fisheries and Oceans, 501 University Crescent, Winnipeg, MB, Canada R3T 2N6
e Ontario Ministry of the Environment, 125 Resources Road, Toronto, ON, Canada M9P 3V6
f Department of Chemistry, McMaster University, Hamilton, ON, Canada L8S 3Z5



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Fig. 1. Protocol for the sequential sedimentation and centrifugation scheme used to fractionate surface water. EM, electron microscopy; ESEM, environmental scanning electron microscopy; TEM, transmission electron microscopy.

 


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Fig. 2. Relative percentages of selected polycyclic aromatic compounds in particle size diameter subfractions in a surface water sample from Hamilton Harbor processed using the described fractionation methodology. The sixth size range denotes particle-free fractions prepared using ultracentrifugation. PCBs, polychlorinated biphenyls.

 


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Fig. 3. Mean relative percentage contributions of polychlorinated biphenyl (PCB) homologs in >10- and <10-µm particles prepared from Hamilton Harbor surface water. Mean percentages for >10-µm particles were calculated from values for the two particle fractions isolated by centrifugation, while mean percentages for <10-µm particles were calculated using values from the four fractions isolated by sedimentation.

 


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Fig. 4. Electron-optical views (a–c) of entire aquatic particles (whole mounts) in surface water collected from Hamilton Harbor and separated into size fractions. (a) An environmental scanning electron microscopy (ESEM) image, which indicates the size and morphology of a typical aggregated particle (a multicomponent floc) from Fraction 3 (F3 of Fig. 1) in topographical view. (b) An ESEM image of a smaller floc from Fraction 4. (c) A high-resolution transmission electron microscopy (TEM) image of a small heterogeneous aggregated particle captured, from raw water, on top of a Formvar film (mounted on a TEM grid). Electron-optical images of ultrathin sections of aggregated particles collected from Hamilton Harbor water fractions (d–f). (d) A TEM image showing individual colloids within a porous large aggregate collected from raw water. (e) A TEM image showing individual colloids in an aggregate collected from Fraction 4 (10- to 20-µm range). (f) A TEM image showing individual colloids in an aggregate collected from Fraction 5 (2- to 10-µm range). The colloidal particles shown in all TEM images (of ultrathin sections above) represent the dominant particles by number. Note that for all three images, the protocol used for fixation and subsequent TEM preparation was the proxy protocol beginning with the step "glutaraldehyde + RR."

 





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