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On Jan. 9, 2014, a spill of "crude" 4-methylcyclohexanemethanol (MCHM) into the Elk River in West Virginia contaminated the water supply for 300,000 people. The crude MCHM caused an intense licorice odor in the drinking water that supplied the area in and around Charleston, W.Va. A sensitive analytical method developed by a commercial laboratory was used to verify the concentrations of crude MCHM presented to a consumer panel selected using specific criteria. The method used for the panel studies was ASTM E679-04, which has been used to determine other odor thresholds in water. The odor threshold and odor recognition concentrations for crude MCHM in water were estimated by the consumer panel to be 0.55 and 7.4 μg/L, respectively. Two estimates of the odor objection concentration were 7.7 and 8.8 μg/L. [ABSTRACT FROM AUTHOR]

Government agencies responsible for ensuring healthful water and/or air quality are often faced with resolving public complaints of nuisance odors. Understanding variations in odor intensity may ultimately lead to the establishment and application by such agencies of quantitative limits for effective odorant control. An odor panel was trained in suprathreshold odor intensity evaluation using both the ASTM Method E544 (Butanol Method) and the APHA Method 2170 (Flavor Profile Analysis (FPA) Method). A linear mixed model was fitted to the panel data, taking into account the fixed effects of concentration levels and the random effects of panelists and sessions. The FPA method proved easier to administer and revealed less inter-session variance than the ASTM Method, suggesting its greater utility in applications involving odor panels. For both methods, there was a high standard deviation, relative to the mean. This finding indicates that the intensity scales may be useful for understanding relative odor intensities, but should not be used as a precise measure, or as a basis for establishing regulatory limits. [ABSTRACT FROM AUTHOR]

Varieties of gas chromatography (GC) combined with chemical detection (CD) and sensory analysis at the odour detection port (ODP) for the evaluation of environmental odorants has steadily increased in application and sophistication; this has given rise to a plethora of techniques that cater to specific tasks. With this diversity of approaches in mind, there is a need to assess the critical points at which these approaches differ, as well as likely risks and factors that may affect them. These critical points explained within this review include sample preparation, GC separation techniques (with associated co-elution risks), how the elute is separated between CD and sensory analysis, the type of CD, the type of sensory analysis (with particular attention paid to its factors and guidelines), integrative data techniques, as well as how that data may be used. Additionally, this review provides commentary on the current state of the research space and makes recommendations based on how these analyses should be reported, the standardisation of nomenclature, as well as the impediments to the future goals of this research area. By careful consideration of the critical points of varying analytical processes and how best to communicate these findings, the quality of output within this area will improve. This review provides a benchmark for how GC-CD/sensory analysis should be undertaken and reported., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Author(s). Published by Elsevier Ltd.. All rights reserved.)

Certain nitrosamines in water are disinfection byproducts that are probable human carcinogens. Nitrosamines have diverse and complex precursors that include effluent organic matter, some anthropogenic chemicals, and natural (likely non-humic) substances. An easy and selective tool was first developed to characterize nitrosamine precursors in treated wastewaters, including different process effluents. This tool takes advantages of the polarity rapid assessment method (PRAM) and ultrafiltration (UF) (molecular weight distribution) to locate the fractions with the strongest contributions to the nitrosamine precursor pool in the effluent organic matter. Strong cation exchange (SCX) and C18 solid-phase extraction cartridges were used for their high selectivity for nitrosamine precursors. The details of PRAM operation, such as cartridge clean-up, capacity, pH influence, and quality control were included in this paper, as well as the main parameters of UF operation. Preliminary testing of the PRAM/UF method with effluents from one wastewater treatment plant gave very informative results. SCX retained 45-90% of the N-nitrosodimethylamine (NDMA) formation potential (FP)-a measure of the precursors-in secondary and tertiary wastewater effluents. These results are consistent with NDMA precursors likely having a positively charged amine group. C18 adsorbed 30-45% of the NDMAFP, which indicates that a substantial portion of these precursors were non-polar. The small molecular weight (MW) (<1 kDa) and large MW (>10 kDa) fractions obtained from UF were the primary contributors to NDMAFP. The combination of PRAM and UF brings important information on the characteristics of nitrosamine precursors in water with easy operation., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Second-order rate constants of the direct ozone reactions [formula: see text] and the indirect OH radical reactions [formula: see text] for nine chemicals on the US EPA's Drinking Water Contaminant Candidate List (CCL) were studied during the ozonation and ozone/hydrogen peroxide advanced oxidation process (O(3)/H(2)O(2) AOP) using batch reactors. Except for the thiocarbamate herbicides (molinate and EPTC), all other CCL chemicals (linuron, diuron, prometon, RDX, 2,4-dinitrotoluene, 2,6-dinitrotoluene and nitrobenzene) show low reactivity toward ozone. The general magnitude of ozone reactivity of the CCL chemicals can be explained by their structures and the electrophilic nature of ozone reactions. The CCL chemicals (except RDX) are highly reactive toward OH radicals as demonstrated by their high [formula: see text] values. Ozonation at low pH, which involves mainly the direct ozone reaction, is only efficient for the removal of the thiocarbamates. Ozonation at high pH and O(3)/H(2)O(2) AOP will be highly efficient for the treatment of all chemicals in this study except RDX, which shows the lowest OH radical reactivity. Removal of a contaminant does not mean complete mineralization and reaction byproducts may be a problem if they are recalcitrant and are likely to cause health concerns.

Two nitrogen-specific detection methods, nitrogen-phosphorus detection (NPD) and nitrogen chemiluminescence detection (NCD), were investigated as low cost alternatives to mass spectrometry (MS) with chemical ionization (CI) for analysis of nitrosamines in aqueous samples. NCD showed greater sensitivity to N-nitrosodimethylamine (NDMA) and seven other volatile nitrosamines than did NPD. Instrument detection levels for NDMA were established at 2.6 microg/L and 4.0 microg/L in solvent with 3 microL splitless gas chromatograph (GC) injection for NCD and NPD, respectively. Using a dual-column confirmation method, both NCD and NPD compared favorably with CI-MS results for NDMA analysis in a variety of water sample types. For seven other nitrosamines, both detectors showed excellent accuracy in analyzing high concentrations (greater than 300 ng/L) in complex wastewater matrices, while the accuracy of spike recoveries of very low levels (less than 15 ng/L) in clean matrices varied for each nitrosamine and detection method.