2-methylisoborneol and 2-4-6-trichloroanisole

The concentrations of earthy and musty odor compounds (2-methylisoborneol (2-MIB), geosmin and 2,4,6-trichloroanisole (TCA)) in treated wastewater were measured. Concentrations of 2,4,6-TCA (4.3-37.7 ng/L) and geosmin (3.7-42.2 ng/L) higher than their odor thresholds were detected for effluents from large-scale treatment plants. The effluent from a small-scale wastewater plant treating toilet and kitchen wastewater contained the target earthy and musty odor compounds below the odor thresholds. The ozonation applied as an advanced wastewater treatment process was considerably more effective for the removal of 2,4,6-TCA than for the removal of 2-MIB and geosmin. The measured concentrations of 2,4,6-TCA in river environments without the influence of large-scale wastewater effluents were less than the odor threshold.

Topics: Anisoles; Camphanes; Chromatography, Gas; Naphthols; Odorants; Rivers; Tokyo; Waste Disposal, Fluid; Wastewater; Water Pollutants, Chemical

An automated technique based on purge-and-trap coupled to gas chromatography with mass spectrometric detection has been developed and optimized for the trace determination of five of the most important water odorants; 2-isopropyl-3-methoxypyrazine, 2-isobutyl-3-methoxypyrazine, 2-methylisoborneol, 2,4,6-trichloroanisole and geosmin. The extraction method was absolutely solvent-free. Analytes were purged from 20 ml of water sample containing sodium chloride at room temperature by a flow of He and trapped on a Tenax sorbent. The desorption step was performed with helium and temperature programming and desorbed analytes were directly transferred to a gas chromatograph coupled to a mass spectrometer for separation and determination. The method was reproducible (RSD<8%) and linear over the calibration range (10-200 ngl(-1)). The relative recoveries of the analytes from ground water sample were calculated and were between 80 and 103% and limits of detection (LOD) below odor thresholds were achieved for most of the compounds.

Topics: Anisoles; Automation; Camphanes; Gas Chromatography-Mass Spectrometry; Naphthols; Odorants; Online Systems; Pyrazines; Sensitivity and Specificity; Water

The removal of four earthy-musty compounds, 2-methylisoborneol (MIB), 2,4,6-trichloroanisole (TCA), 2-isopropyl-3-methoxy-pyrazine (IPMP), and 2-isobutyl-3-methoxy-pyrazine (IBMP), by powdered activated carbon (PAC) were investigated under the simulative condition of Xicun water plant, Guangzhou. The adsorption kinetics of odor compounds by two PACs show that main removal of odor compounds occurs within contact time of 1 h. Compared with the wood-based PAC, the coat-based PAC evidently improves the removal efficiency of poorly adsorbed compounds like MIB. The effects on removal efficiency such as optimum PAC dosage, initial concentration of the organics, chlorine residual, background organics, and changes of water quality were investigated. The percent removal of trace odorants at any given time for a particular carbon dosage is irrelative to the initial concentration of the odor compounds. Adsorptive capacity of PAC for target compounds is reduced by chlorine residual and background organics. Characteristics of raw water have vast influence on the removal of target compounds by PAC.

Topics: Adsorption; Anisoles; Camphanes; Carbon; China; Chlorine; Odorants; Pyrazines; Rivers; Water Pollutants, Chemical; Water Purification

"Earthy-musty" off-flavor problem in water samples are due to organic compounds present at the sub-part-per-trillion level. Most of the developments in the analysis of tastes and odorous compounds focus on the extraction pre-concentration technique, with detection at picogram per liter level of the earthy-musty off-flavor compounds difficult to be achieved. In this study, a simple, efficient and sensitive method for the analysis of odorous compounds has been developed by the application of solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) with initial cool programmable temperature vaporizer (PTV) inlet for the first time. Compared with initial hot PTV inlet, the initial cool inlet could greatly improve the system sensitivity, especially for the compounds with good volatility, e.g. 2-methylisoborneol (MIB). StableFlex divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was found to possess the best extraction efficiency towards these odorous compounds in water. Various SPME and PTV conditions have been studied and optimized in detail. The optimized method has been validated with good linearity, precision and accuracy. The method detection limits (MDL) of the targeted odorous compounds were found to be 0.32ng/L for 2,4,6-trichloroanisole (2,4,6-TCA), 0.14ng/L for 2,3,6-trichloroanisole (2,3,6-TCA), 0.16ng/L for 2,3,4-trichloroanisole (2,3,4-TCA), 0.38ng/L for 2,4,6-tribromoanisole (2,4,6-TBA), 0.16ng/L for gesomin and 0.15ng/L for MIB. To the best of our knowledge, this represents the best sensitivity achieved for analysis of gesomin and MIB in water via the simple and efficient SPME method. The current method has been successfully applied in the analyses of different water samples.

Topics: Anisoles; Camphanes; Dimethylpolysiloxanes; Flavoring Agents; Food Analysis; Gas Chromatography-Mass Spectrometry; Microchemistry; Nebulizers and Vaporizers; Odorants; Sensitivity and Specificity; Silicones; Styrene; Temperature; Volatilization; Water

The off-flavor compounds 2-methylisoborneol (MIB), geosmin, 2,4,6-trichloroanisole, 2,3,6-trichloroanisole, 2,3,4-trichloroanisole, and 2,4,6-tribromoanisole were analyzed in water samples by stir bar sorptive extraction (SBSE) followed by on-line thermal desorption (TD) capillary GC/MS. Quantification was performed using the MS in the single-ion-monitoring mode (SIM) with 2,4,6-trichloroanisole-D(5 )as internal standard. Quantification limits are 0.1-0.2 ng L(-1) for the haloanisoles, 0.5 ng L(-1) for geosmin, and 1 ng L(-1) for MIB. The relative standard deviations at the quantification limit ranged from 7 to 14.6%. SBSE recovery was evaluated by spiking real water samples and varied from 87 to 117%. More than twenty samples per day can be analyzed by SBSE-TD-capillary GC-MS. The same technique in combination with olfactometry was used to elucidate unknown odorous compounds in water samples.

Topics: Anisoles; Calibration; Camphanes; Gas Chromatography-Mass Spectrometry; Naphthols; Odorants; Reproducibility of Results; Sensitivity and Specificity; Taste; Water Pollutants, Chemical; Water Supply