Determination of three alkylphenol isomers in various water samples using a new HPLC method based on a duet stationary phase

The level of three alkylphenols (APs) 4-nonylphenol, 4-octylphenol and 4-tert-octylphenol was monitored in various water samples using a new developed and validated HPLC method. The HPLC method employed a column with a mixed-mode stationary phase (C18/SCX) using a mobile phase of water to methanol?=?15:85 (v/v) delivered at a flow rate of 1 mL/min at room temperature. Both diode array, DAD and fluorescence, FLD detectors were employed. The method is linear when APs concentration ranged from 0.025 to 0.5 μg/mL with a DAD detection at 279 nm and between 0.0008 and 0.1 μg/mL when the detection was made by FLD (excitation at 220 nm, emission at 315 nm). The limit of detection and limit of quantitation for alkylphenols were found to be 5 and 15 ng/mL, respectively (detection by DAD). The method was employed with good results for the determination of APs in the presence of polycyclic aromatic hydrocarbons in various water samples.     

高效液相色谱三元梯度分离法测定大气中11种醛酮类化合物分析方法的研究

研究建立了高效液相色谱三元梯度分离法测定11种醛酮类化合物的最佳色谱分离条件,醛酮类化合物的最小检测量从0.45到2.04ng,各化合物保留时间的相对标准偏差RSD≤0.38%,在所测定的含量范围内具有很好的线性关系,每种化合物的相关系数均大于0.999;并研究了涂敷2,4-二硝基苯肼硅胶吸附采样夹的制作方法,且应用于大气环境中醛酮类化合物的分析,方法简单、快速,11种醛酮类化合物的平均解吸效率在98.3%～105%之间,结果令人满意.     

evaluation of a measurement method for forest vegetation in a large-scale ecological survey

We evaluate a field method for determining species richness andcanopy cover of vascular plants for the Forest Health MonitoringProgram (FHM), an ecological survey of U.S. forests. Measurementsare taken within 12 1-m² quadrats on 1/15 ha plots in FHM.Species richness and cover are determined for four height classes(strata) within each quadrat and aggregated by stratum over the entireplot. We estimated (1) the agreement between experienced trainers andinexperienced technicians who collected the data on this survey(accuracy) and (2) the agreement among the technicians (precision) forresults on species richness and cover from 3 test plots at 3 timeintervals. The methods appear to be highly precise, although somediscrepancies with the values obtained by the trainers were found.Trainers found significantly more species in the ground stratum (0–0.6 m) and measured significantly more cover in the uppermost stratum(>4.9 m). The proportion of variation due to measurement error andtemporal variability was less than 13% for species richness (all strata)and cover (all but one stratum). This indicates that the method issuitable for monitoring changes in species richness and canopy coverfor a large-scale synoptic monitoring project such as FHM.     

Multi-residue determination of pharmaceuticals in sludge and sludge enriched soils using pressurized liquid extraction, solid phase extraction and liquid chromatography with tandem mass spectrometry

An analytical method to determine a selection of 27 frequently prescribed and consumed pharmaceuticals in biosolid enriched soils and digested sludges is presented. Using a combination of pressurized liquid extraction, solid phase extraction and liquid chromatography with tandem mass spectrometry, it was possible to detect all analytes in each sample type at the low-sub ng g(-1) level. Solid phase extraction efficiencies were compared for 6 different sorbent types and it was found that Waters Oasis HLB cartridges offered enhanced selectivities with 20 analytes showing final method recoveries > or =60% in both soils and digested sludges. The method was validated for linearity, range, precision and limits of detection in both sample matrices. All analytes were then determined in sludge enriched soils as well as the precursor thermally dried sludge fertilizer produced from a primary wastewater treatment plant. Levels of the antibacterial agent triclosan were found to exceed 20 microg g(-1) in digested sludge and 5 microg g(-1) in thermally dried sludge cake. Significant traces of carbamazepine and warfarin were also detected in the above samples.     

Monitoring and measurement of microalgae using the first derivative of absorbance and comparison with chlorophyll extraction method

Monitoring of microalgae in water supplies and industrial applications are becoming increasingly important, yet there are few options available that are simple and accurate, and can provide real-time information. The present work illustrates a new method to determine the concentration of microalgae in water and wastewater using spectrophotometry and the first derivative of absorbance. Chlorella vulgaris was used as an indicator microalga, spiked in water samples representing a range of water qualities (distilled water, surface water, and wastewater), and correlations among C. vulgaris concentrations, absorbance, and the first derivative of absorbance measurements were investigated. In addition, detection limits were established and sensitivity analyses were carried out to determine the lowest C. vulgaris concentrations that can be confidently measured in different water matrices. Finally, the study compared the performance and detection limits of the spectrophotometry-based methods with the well-accepted chlorophyll extraction method. A strong linear relationship (R²?>?0.97) was found between C. vulgaris concentration and absorbance at 695 nm. Using the first derivative of absorbance improved C. vulgaris detection limits by reducing the effects of the background noise and interferences from other substances. The detection limits established using the first derivative method were 0.47, 0.56, and 1.96 mg TVS/L in distilled water, surface water, and wastewater, respectively. In comparison, the detection limits of the chlorophyll extraction method were found to be 19.6, 38.6, and 48.3 mg TVS/L in the same water matrices. These results indicate that first derivative of absorbance can be successfully used for monitoring of microalgae in surface waters and environmental samples as well as in bioreactors used for microalgae cultivation in industrial applications.     

新型侧链聚硅氧烷液晶高分子用作毛细柱气相色谱固定液的研究

以合成的新型胆甾酯类侧链聚硅氧烷液晶高分子作固定液 ,涂渍在弹性石英毛细管柱上 ,具有较高的柱效和选择性 ,热稳定性好 ,适于分离多种异构体混合物。     

Landslide susceptibility mapping in an area of underground mining using the multicriteria decision analysis method

Landslides are geomorphological phenomena that affect anthropogenic and natural features on the Earth’s surface. Many previous studies have identified several factors that have contributed to landslides. Among these factors are physical characteristics, such as slope, aspect, and land cover, of Earth’s surface. Moreover, landslides can be triggered by human activities such as underground mining. This study aims to identify landslide susceptibility areas by analyzing landslide-related factors, including land subsidence triggered by underground mining. The area of interest was Kozlu, Turkey, where underground mining has been in progress for the past 100 years. Thus, to identify landslide risk zones, the multicriteria decision analysis method, together with the analytical hierarchy method, was used. The datasets included were topography, land cover, geological settings, and mining-induced land subsidence. The spatial extent of land subsidence was estimated using a previously published model. A landslide susceptibility map (LSM) was developed using a purposely developed GIS-based software. The results were compared with a terrain deformation map, which was developed in a separate study using the differential synthetic aperture radar interferometry (DInSAR) technique. The results showed a substantial correlation between the LSM and DInSAR map. Furthermore, it was found that ~?88% of the very high and high landslide risk areas coincided with location of the past landslide events. These facts suggest that the algorithm and data sources used were sufficient to produce a sufficiently accurate LSM, which may be used for various purposes such as urban planning.     

Preliminary evaluation of evaluation of the efficiency of aircraft liquid waste treatment using resolvable sanitizing liquid: a case study in Changchun

The physical, chemical, and biological indices of aircraft liquid wastes collected from multiple airplanes at Longjia Airport, Changchun, China were measured according to "Integrated Wastewater Discharge Standard," evaluating treatment efficiency of resolvable sanitizing liquid. The results indicate that, after being treated by the resolvable sanitizing liquid, the indices of all first-class pollutants met the requirements of the standard, while among the second-class pollutants, the suspension content, biochemical oxygen demand after 5 days, and chemical oxygen demand as well as the contents of amino nitrogen, total phosphorus, anionic surfactants, total copper, absorbable organic halogen, and phenolic compounds did not reach the discharge standard. Particularly, the level of fecal coliform bacteria in the aircraft liquid wastes can meet the standard specification by adding more than 1 mL/L resolvable sanitizing liquid. The aircraft wastewater treated by resolvable sanitizing liquid cannot be directly discharged back into the environment as well as urban drainage systems.     

Development, validation, and uncertainty measurement of multi-residue analysis of organochlorine and organophosphorus pesticides using pressurized liquid extraction and dispersive-SPE techniques

Increased water use associated with rapid growth in the Las Vegas Valley has inadvertently led to the creation of unique wetland systems in Southern Nevada with an abundance of biological diversity. Constructed and naturally created wetlands in the Las Vegas Valley watershed were studied to characterize and understand their potential role for improving ecosystem services (i.e., water purification). Nutrient and metal removal was assessed at four sites including a natural urban runoff wetland, a constructed urban runoff wetland, a constructed wastewater wetland, and a natural urban runoff/wastewater wetland. Plant nutrient uptake was dependent on ambient nutrient concentrations in water and sediments of specific wetlands, irrespective of the type of plants present. Phosphorus was mostly concentrated in below-ground plant parts whereas nitrogen was concentrated in above-ground parts. As for metalloids, bulrushes were more efficient than cattails at taking up arsenic and selenium. Averaging all the wetland sites and plant species, total nitrogen, phosphorus, arsenic and selenium removal was 924.2, 61.5, 0.30, and 0.38 kg/ha/year, respectively. Our findings suggest that natural and created wetland systems can improve water quality in the Las Vegas Valley watershed for some common pollutants, however, other measures are still needed to improve water quality below regulatory thresholds.     

Monitoring of aminophenol isomers in surface water samples using a new HPLC method

A new HPLC method was developed for the simultaneous determination of aminophenol isomers by means of a mixed-mode stationary phase containing both SCX and C18 moieties. All factors influencing the separation were discussed and optimized. The chromatographic conditions for the separation of aminophenols are the stationary phase duet SCX/C18, the mobile phase of aqueous phosphate buffer (pH 4.85):methanol?=?85:15 (v/v) delivered with a flow rate of 1 mL/min and a detection at 285 nm. The method proposed was validated in terms of linearity, limits of detection and quantification, accuracy and precision. The HPLC method elaborated here was applied with good results on river water samples. In order to survey the quality of surface rivers entered in treatment plants which deliver water for Bucharest, two major rivers were included in a monitoring program which last more than 1 year.     

Real-time discharge measurement in tidal streams by an index velocity

Discharge measurement in a tidal stream is always a difficult task. Owing to the complex flow conditions, discharge measurement in tidal streams has to be finished quickly, and must be highly efficient in order to yield an accurate measurement of real-time discharge. Measuring the discharge of tidal streams is done in three steps: (1) establishing the stage and cross-sectional area relation, (2) estimating the index velocity by using a velocity distribution equation based on the probability concept, (3) establishing the relationship between the index and mean velocities. Then the cross-sectional area and mean velocity can be estimated by the gage height and index velocity, respectively. The discharge of tidal streams is computed as the product of the cross-sectional area and mean velocity. The velocity distribution of the Taipei Bridge and Guan-du Bridge in the Tanshui River were established and analyzed to demonstrate the use of discharge measurement by index velocity for estimating the discharge of this tidal stream. The results reveal no large difference between the discharges measured by the conventional methods and the index velocity. This pilot study proposed a cost-effectiveness and efficient method. It is an easy, quick, and accurate model for measuring the real-time discharge of a tidal stream. It makes automatic, real-time, and continuous monitoring of the discharge in a tidal stream become possible.     

Evaluation of ogawa passive sampling devices as an alternative measurement method for the nitrogen dioxide annual standard in El Paso, Texas

Nitrogen Dioxide (NO₂) is a common urban air pollutant that results from the combustion of fossil fuels. It causes serious human health effects, is a precursor to the formation of ground level ozone, another serious air pollutant, and is one of the six criteria air pollutants established by the United States (U.S.) Clean Air Act (CAA). Ogawa Passive Sampling Devices (PSDs) for NO₂ were collocated and operated at six NO₂ Federal Reference Method (FRM) monitor locations in the El Paso, Texas area for the 2004 calendar year. Passive samples were taken at 2-week, 3-week, and 4-week intervals and compared against the continuously operating FRM monitors. Results showed that the collective NO₂ annual arithmetic mean for all passive monitors was identical to the NO₂ mean for all FRM monitors. Of the individual locations, three passive annual NO₂ means were identical to their corresponding FRM means, and three passive annual NO₂ means differed from their corresponding FRM means by only one part per billion (ppb). Linear correlation analysis between all readings of the individual NO₂ PSDs and FRM values showed an average absolute difference of 1.2 ppb with an r ² of 0.95. Paired comparison between high and low concentration annual NO₂ sites, seasonal considerations, and interlab quality control comparisons all showed excellent results. The ease of deployment, reliability, and the cost-savings that can be realized with NO₂ PSDs could make them an attractive alternative to FRM monitors for screening purposes, and even possibly an equivalent method for annual NO₂ monitoring. More tests of the Ogawa NO₂ PSD are recommended for different ecosystem and climate regimes.     

Nitrosamine occurrence at Korean surface water using an analytical method based on GC/LRMS

The survey of nitrosamine occurrence at Korean surface water of Nakdong river is conducted in this study. For this purpose, the nitrosamine analytical method based on more affordable GC/LRMS (low resolution mass spectrometry) has been developed. According to the study results, six nitrosamine compounds (NDEA as N-nitrosomethylethylamine, NDPA as N-nitrosodi-n-propylamine, NDMA as N-nitrosodimethylamine, NMEA as N-nitrosomethylethylamine, NDBA as N-nitrosodi-n-butylamine, and NDPHA as N-nitrosodiphenylamine) were detected at the Nakdong river. Among these, NDEA and NDPA are the most important compounds in terms of the nitrosamine contamination of the Nakdong river. The detected concentration of NDEA exceeded the CDHCS (California Department of Health Care Services) response level of 100 ng/L at several sites. The detected concentration of NDPA approached the response level (500 ng/L) at a few sites. When all nitrosamine concentrations were summed up, the maximum concentration of 735.7 ng/L was detected at the Nakdong river. An equation describing a decrease in total nitrosamine concentration along downstream sampling sites was proposed in this study. The equation can be used to predict the downstream nitrosamine contamination at the Nakdong river. Among various water quality parameters, T-N showed a good correlation with total nitrosamine concentration.     

Comparison of a matrix solid phase dispersion and a classical extraction method for the determination of chlorinated pesticides in fish muscle

A new multiresidue extraction technique was used to determine incurred chlorinated hydrocarbon pesticide residues in various fish species sampled at 2 locations along the Tensas River in Louisiana. Residue levels of total DDT (combined DDT, DDE, and DDD levels) in fish muscle fillets from paired samples ranged from 0.2 to 3.9 ppm on a wet weight basis. These findings were compared to those of another laboratory that used a different protocol to isolate the residues from the fish muscle fillets. This latter protocol typifies the more complicated, time-consuming protocols used by governmental agencies for screening purposes. Results demonstrated that the new extraction technique reduced analysis time, solvent waste, and cost per sample without affecting the quality of residue detection and measurement.     

Atmospheric vapour phase and particulate phase mercury in a coastal desert climate

Vapour (T-Hg(v)) and particulate (T-Hg(p)) mercury were measured in the lower atmosphere at a ground station in Kuwait Bay. The concentration of T-Hg(v) varied from 0-86 ng m(-3) with a mean of 3.8 +/- 5.5 ng m(-3)(n= 13 326). About 40% of the measured T-Hg(v) values over Kuwait Bay are higher than the global range (1-3 ng m(-3)). Car exhausts contributed to the increase of T-Hg(v) during the rush hours. However the contribution of T-Hg(v) from air crossing Kuwait Bay exceeds that T-Hg(v) produced by traffic probably because of the effects of the substantial load of industrially-derived mercury in the sediments of this shallow region. Thermal inversions have a major impact on the levels during the evening hours. The concentration of T-Hg(p) varied from 0.00-0.22 ng m(-3) with a mean of 0.03 +/- 0.03 ng m(-3)(n= 175). The T-Hg(p)/T-Hg(v)% ratio varied from 0-11.1 (n= 171) with a mean of 1.0 +/- 1.5%. Meteorological parameters influence the T-Hg(v) and T-Hg(p) concentrations with dust storms having a major impact on T-Hg(p) concentrations.     

Development of a solid phase microextraction (SPME) method for the sampling of VOC traces in indoor air

Solid-phase microextraction (SPME) was studied for the measurement of volatile organic compounds (VOCs) in indoor air. An adsorptive PDMS/Carboxen fibre was used and an analytical methodology was developed in order to overcome competitive adsorption. Kinetics and adsorption isotherms were investigated for different sample volumes and model compounds. In order to evaluate competitive adsorption on the fibre, these compounds were studied alone and in mixture. From the results obtained, the operating conditions allowing co-adsorption of the target compounds were determined: the air sample is enclosed in a 250 mL glass bulb where the SPME fibre is exposed until adsorption equilibrium. This procedure was combined with GC/MS analysis for the identification and quantification of VOCs in indoor air. The performances were determined by using a standard gas containing 10 VOCs representative of indoor environments (acetaldehyde, acetone, BTX, alpha-pinene, trichloroethylene, alkanes). The detection limits were determined in single ion monitoring mode and for a signal to noise ratio of 3. Except acetaldehyde (6 microg m(-3)), they are all below 0.5 microg m(-3). Calibration curves are linear up to 10 micromol m(-3) for all the compounds with good correlation coefficients (above 0.99). The reproducibility ranges from 6 to 12% according to the compound. The methodology was then applied to the comparison of the VOCs content in classrooms of two different schools.     

Long-term measurement of volatile organic compounds in ambient air by canister-based one-week sampling method

A canister-based 1 week sampling method using a mechanical flow controller and a 6 L fused-silica-lined canister was evaluated for the long-term measurement of 47 VOCs in ambient air at pptv (volume/volume) to ppbv levels by use of a three-stage preconcentation method followed by GC-MS analysis. The GC conditions were initially optimized for complete separations of several pptv-level VOCs (e.g. vinyl chloride, 1,3-butadiene, acrylonitrile, 1,2-dichloroethane and chloroform) in ambient air because the selected ions are easily interfered with by coexisting C4-, C5-hydrocarbons and analytes presented at ppbv levels. Thirty-four VOCs determined by the 1 week and 24 h sampling method in December 16-22 (2002) had concentrations of 6.0-15000 pptv per compound. Concentrations of 28 VOCs (including polar VOCs (e.g. methyl isobutyl ketone and butyl acetate)) obtained by the method were approximately equal to the mean values calculated from 24 h sampling (< +/- 10% deviation). Six VOCs that had low concentrations of 6.0-43 pptv showed more than +/- 10% deviation. Thirteen VOCs were not detected during the entire sampling period. The effect of relative humidity or ozone for the specific VOCs (e.g. MIBK, butyl acetate, vinyl chloride, 1,3-butadiene and styrene) was negligible.     

自制固相微萃取涂层用于自来水中五氯酚的测定

采用石英毛细管作为模具,甲基丙烯酸和乙二醇二甲基丙烯酸酯在石英纤维表面原位聚合得到聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)作为固相微萃取涂层,并以五氯酚为研究对象,采用顶空SPME-GC-ECD法对该涂层的萃取性能进行评价。使用正交试验优化萃取温度、萃取时间、盐浓度、pH和搅拌速度。在最优条件下,建立了水样中五氯酚的分析方法,方法检出限为1ng/L,线性范围为2～5000ng/L,线性相关系数为0.9999,相对标准偏差(RSD,n=5)为8.9%,加标回收率为110.8%。