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Headley J.V.,Environment Canada | Peru K.M.,Environment Canada | Mohamed M.H.,Environment Canada | Frank R.A.,Environment Canada | And 41 more authors.
Journal of Environmental Science and Health - Part A Toxic/Hazardous Substances and Environmental Engineering | Year: 2013

This article provides a review of the routine methods currently utilized for total naphthenic acid analyses. There is a growing need to develop chemical methods that can selectively distinguish compounds found within industrially derived oil sands process affected waters (OSPW) from those derived from the natural weathering of oil sands deposits. Attention is thus given to the characterization of other OSPW components such as oil sands polar organic compounds, PAHs, and heavy metals along with characterization of chemical additives such as polyacrylamide polymers and trace levels of boron species. Environmental samples discussed cover the following matrices: OSPW containments, on-lease interceptor well systems, on-and off-lease groundwater, and river and lake surface waters. There are diverse ranges of methods available for analyses of total naphthenic acids. However, there is a need for inter-laboratory studies to compare their accuracy and precision for routine analyses. Recent advances in high-and medium-resolution mass spectrometry, concomitant with comprehensive mass spectrometry techniques following multi-dimensional chromatography or ion-mobility separations, have allowed for the speciation of monocarboxylic naphthenic acids along with a wide range of other species including humics. The distributions of oil sands polar organic compounds, particularly the sulphur containing species (i.e., OxS and OxS2) may allow for distinguishing sources of OSPW. The ratios of oxygen-(i.e., Ox) and nitrogen-containing species (i.e., NOx, and N2Ox) are useful for differentiating organic components derived from OSPW from natural components found within receiving waters. Synchronous fluorescence spectroscopy also provides a powerful screening technique capable of quickly detecting the presence of aromatic organic acids contained within oil sands naphthenic acid mixtures. Synchronous fluorescence spectroscopy provides diagnostic profiles for OSPW and potentially impacted groundwater that can be compared against reference groundwater and surface water samples. Novel applications of X-ray absorption near edge spectroscopy (XANES) are emerging for speciation of sulphur-containing species (both organic and inorganic components) as well as industrially derived boron-containing species. There is strong potential for an environmental forensics application of XANES for chemical fingerprinting of weathered sulphur-containing species and industrial additives in OSPW. © 2013 Taylor & Francis Group, LLC. Source

Brunswick P.,Environment Canada | Shang D.,Environment Canada | van Aggelen G.,Environment Canada | Hindle R.,Vogon Laboratory Services Ltd. | And 4 more authors.
Journal of Chromatography A | Year: 2015

A rapid and sensitive liquid chromatography quadrupole time of flight method has been established for the determination of total naphthenic acid concentrations in aqueous samples. This is the first methodology that has been adopted for routine, high resolution, high throughput analysis of total naphthenic acids at trace levels in unprocessed samples. A calibration range from 0.02 to 1.0μgmL-1 total Merichem naphthenic acids was validated and demonstrated excellent accuracy (97-111% recovery) and precision (1.9% RSD at 0.02μgmL-1). Quantitative validation was also demonstrated in a non-commercial oil sands process water (OSPW) acid extractable organics (AEOs) fraction containing a higher percentage of polycarboxylic acid isomers than the Merichem technical mix. The chromatographic method showed good calibration linearity of ≥0.999 RSQ to 0.005μgmL-1 total naphthenic acids with a precision <3.1% RSD and a calculated detection limit of 0.0004μgmL-1 employing Merichem technical mix reference material. The method is well suited to monitoring naturally occurring and industrially derived naphthenic acids (and other AEOs) present in surface and ground waters in the vicinity of mining developments. The advantage of the current method is its direct application to unprocessed environmental samples and to examine natural naphthenic acid isomer profiles. It is noted that where the isomer profile of samples differs from that of the reference material, results should be considered semi-quantitative due to the lack of matching isomer content. The fingerprint profile of naphthenic acids is known to be transitory during aging and the present method has the ability to adapt to monitoring of these changes in naphthenic acid content. The method's total ion scan approach allows for data previously collected to be examined retrospectively for specific analyte mass ions of interest. A list of potential naphthenic acid isomers that decrease in response with aging is proposed and a quantitative assay of an adamantane carboxylic acid is reported. © 2015. Source

Hindle R.,Vogon Laboratory Services Ltd. | Noestheden M.,Vogon Laboratory Services Ltd. | Peru K.,Environment Canada | Headley J.,Environment Canada
Journal of Chromatography A | Year: 2013

This study details the development of a routine method for quantitative analysis of oil sands naphthenic acids, which are a complex class of compounds found naturally and as contaminants in oil sands process waters from Alberta's Athabasca region. Expanding beyond classical naphthenic acids (CnH2n-zO2), those compounds conforming to the formula CnH2n-zOx (where 2≥x≤4) were examined in commercial naphthenic acid and environmental water samples. HPLC facilitated a five-fold reduction in ion suppression when compared to the more commonly used flow injection analysis. A comparison of 39 model naphthenic acids revealed significant variability in response factors, demonstrating the necessity of using naphthenic acid mixtures for quantitation, rather than model compounds. It was also demonstrated that naphthenic acidic heterogeneity (commercial and environmental) necessitates establishing a single NA mix as the standard against which all quantitation is performed. The authors present the first ISO17025 accredited method for the analysis of naphthenic acids in water using HPLC high resolution accurate mass time-of-flight mass spectrometry. The method detection limit was 1mg/L total oxy-naphthenic acids (Sigma technical mix). © 2013 Elsevier B.V. Source

Noestheden M.,Vogon Laboratory Services Ltd. | Noot D.,Vogon Laboratory Services Ltd. | Hindle R.,Vogon Laboratory Services Ltd.
Journal of Chromatography A | Year: 2012

A fast and sensitive analytical method was developed for the chlorinated phenols included in the Canadian Drinking Water Guidelines without the need for costly, time-consuming sample extraction and concentration. Sensitivity and specificity were achieved by derivatization with dansyl chloride and detection via liquid chromatography-tandem mass spectrometry. The dansyl-modified analytes displayed method detection limits in the range of 0.01-1.0 μg/L, enabling the direct determination of chlorophenols from well water without sample enrichment. Recoveries (n=4 days) ranged from 91 to 101% and accuracies were between 79 and 116% (n=4). This method significantly increases sample throughput compared to the current EPA method for phenols in finished drinking water. © 2012 Elsevier B.V. Source

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