SPE-UPLC-MS/MS法测定地下水中多种农药残留

采用固相萃取超高效液相色谱串联质谱法(SPE-UPLC-MS/MS)同时测定地下水中涕灭威、克百威、2,4滴和五氯酚等4种农药残留,通过优化试验条件,使方法在10.0μg/L～200μg/L范围内线性良好,检出限为0.003μg/L～0.006μg/L.标准溶液低、中2个质量浓度水平的加标回收率为84.1％ ～98.8...     

超高效液相色谱—串联质谱快速测定水中的溴氰菊酯

建立了超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS)快速测定地表水及饮用水中溴氰菊酯的方法,并应用于实际水样的检测分析。结果表明:水样经0.22μm滤膜过滤后可直接采用超高效液相色谱-三重四级杆串联质谱仪多重反应监测(MRM)模式定量检测水中溴氰菊酯;最优分析条件下,溴氰菊酯的检出限为0.30μg/L,其线性检测范围为0.30~20.0μg/L,相关系数为0.999 7;采用该方法检测水中的溴氰菊酯,不同水平(2.00、5.00μg/L和20.0μg/L)样品加标回收率为95.5%~98.5%,相对标准偏差为1.37%~3.59%。方法快速简便、灵敏度高、定性定量准确,适合日常批量水样的快速分析。     

顶空-便携式气相色谱法测定土壤中的苯系物

建立了顶空-便携式气相色谱快速测定土壤中苯、甲苯、乙苯、间对二甲苯、邻二甲苯的方法,并讨论了无机盐及振荡时间等因素对顶空分析灵敏度的影响。结果表明,方法回收率为87.2%~105.1%,相对标准偏差(RSD)5.3%~7.8%,最低检出限为0.1~0.8μg/kg;苯、甲苯、乙苯、间对二甲苯、邻二甲苯的线性范围分别为0.8~160μg/kg、1.6~320μg/kg、2.0~400μg/kg、2.0~400μg/kg和3.2~800μg/kg。方法回收率、RSD与标准方法相比没有显著性差异,较之标准方法其更能满足现场快速监测的需要。     

土壤中挥发性有机物的快速测定方法

本文建立了用便携式气相色谱-质谱仪快速测定土壤中VOCs的方法。该方法能够快速对土壤样品中VOCs进行定性分析和定量测定。当采样量达到5 g时,方法检出限0.02~2.11μg/L,相对标准偏差2.0%~13.5%;加标20μg/L时,回收率63%~123%。采用该方法测定北京地区5个土壤样品,总体质量浓度为0~873μg/kg。     

顶空/气相色谱-质谱法测定固废浸出液中苯系物

本方法以实验用水和醋酸缓冲溶液作为浸提剂,利用零顶空萃取法提取固废浸出液,并应用顶空-气相色谱质谱法测定,内标法定量分析,对其检出浓度,加标回收率和精密度进行了研究,结果显示:每个化合物RF的相对标准偏差均小于20%,测定得到最低检出浓度分别为0.1~0.3μg/L和0.1~0.4μg/L;加标回收率范围分别在95.7%~108%和101%~105%之内;RSD分别为1.7%~9.8%和4.4%~7.6%。     

电导和直流安培双检测器离子色谱法测定清洁水样中的碘化物

选用配备了2种不同检测器(电导检测器和直流安培检测器)的离子色谱仪对稀释后过0.22μm滤膜的水样进行分析。配备有直流安培检测器的离子色谱仪测定水中碘化物的方法在0.100~20.0μg/L范围内线性关系良好,相关系数(r)=0.9999,方法检出限为0.030μg/L,测定下限为0.120μg/L,样品加标回收率为95.0%~104%,相对标准偏差为1.06%~1.64%;配备有电导检测器的离子色谱仪测定水中碘化物的方法在20.0~2.00×105μg/L范围内线性关系良好,相关系数(r)=0.9995,方法检出限为2.00μg/L,测定下限为8.00μg/L,样品加标回收率为99.0%~110%,相对标准偏差为0.71%~3.12%。离子色谱-直流安培检测器法测定水中碘化物的方法准确度高、灵敏度高、精密度好,检出限相对较低,适用于测定ρ(碘化物)≤20.0μg/L的清洁水样;离子色谱-电导检测器法主要适用于测定ρ(碘化物)≥20.0μg/L的水样。     

地表水中四乙基铅吹扫捕集-气相色谱/质谱分析方法研究及其应用

系统研究了地表水中四乙基铅的吹扫捕集-气相色谱/质谱分析方法,水样的加标回收率为82%～105%,最低检测限(3σ)及最低定量限(10σ)分别为0.015μg/L和0.05μg/L,0.1μg/L的水样重复进样(n=7)的相对标准偏差为5.4%。利用该方法对浙江省主要城市饮用水源地地表水中四乙基铅进行分析,检测结果均低于检出限。     

DPX快速萃取程序升温大体积进样GC/MS法测定水中19种多溴联苯化合物

建立DPX快速吸附萃取、程序升温(PTV)大体积进样与气相色谱/质谱(GC/MS)联用,SIM模式同时测定水中19种多溴联苯(PBBs)单体的方法。该方法在PBBs质量浓度1~50μg/L范围内线性良好,19种PBBs单体检出限为0.147~0.230μg/L,相对标准偏差为6.61%~10.5%,加标回收率为61.5%~82.6%。     

自动固相微萃取-气相色谱-三重四极杆质谱法直接测定水体中的多环芳烃

建立了固相微萃取(SPME)与气相色谱-三重四极杆质谱法(GC-MS/MS)联用直接测定水体中16种多环芳烃的快速分析方法。通过实验,对固相微萃取纤维涂层的选择、萃取时间、萃取温度等萃取条件以及碰撞电压等参数进行了优化。实验结果表明,采用涂层厚度为100μm的聚二甲基硅氧烷(PDMS)萃取头,以350转/分钟(r/min)40℃下搅拌萃取40min,在GC进样口经280℃热解析6min后,以气相色谱-三重四极杆质谱的多反应监测(MRM)模式检测。在0.2~4.0μg/L的线性范围内,该方法对水中16种PAHs所得的回归方程均具有较好的线性关系,相关系数r值为0.9953~0.9995,检出限为0.001~0.02μg/L。16种PAHs的0.4μg/L加标水样的回收率平均值范围在71%~115%之间,6次平行测定的RSD范围在3.3%~15.6%之间。     

UPLC-MS/MS法同时测定地表水中多种有机污染物

采用超高效液相色谱-串联质谱法直接进样测定地表水中26种有机污染物,通过优化试验条件,使各目标化合物在1.00μg/L^100μg/L范围内线性良好,相关系数(r 2)>0.995,方法检出限为0.003μg/L^1.0μg/L。将该方法用于地表水样的测定,加标回收率为79.0%~120%,6次测定结果的RSD均<15%。     

Topsoil and Housedust Metal Concentrations in the Vicinity of a Lead Battery Manufacturing Plant

The aim of the study was to determine the extent of heavy metal pollution in the vicinity of a lead battery manufacturing plant in the Czech Republic, both in the general environment and within homes. Topsoils (0–5 cm) were sampled from 100 sites along 4 transects which crossed the battery factory, the town centre and outlying rural areas. Housedust samples were collected from 15 plant-workers' homes and 15 non plant-workers' homes located at various distances from the factory. Samples were analysed for levels of Pb, Zn, Cd, Cu, As and Sb, using ICP-AES. Soil concentrations of Pb, Cd, As and Sb peaked at the perimeter fence of the battery factory with Pb levels of up to 12 650 g g> ^-1. Concentrations of these metals decreased exponentially within 500 m of the plant. Whilst the battery factory does appear to be a source of all the metals with the exception of Zn, emissions do not appear to be transported to any great extent over distances of more than 0.5 km. Topsoil and housedust concentrations of Pb, Zn, Cd, Cu, As and Sb in the general Mlada Boleslav area do not appear to be significantly different from those recorded in a large scale survey of urban soils in the United Kingdom. A comparison of housedust Pb concentrations in homes of plant workers and non-plant workers suggests that there may be a small input of Pb into the home environment by battery plant employees.     

微波消解-原子吸收光度法测定土壤中铜锌铅镉镍铬

用微波消解－原子吸收光度法测定土壤中铜，锌，铅，镉，镍和铬。通过硝酸－氢氟酸－过氧化氢体系消解液对土壤样品消解，选择出微波最佳消解条件。对硝酸－盐酸－过氧化氢体系消解液和硝酸－氢氟酸－过氧化氢体系消解液进行消解对比试验，发现前者不能将土壤样品完全消解，后者能将样品消解完全，但需将消解液中剩余的酸赶尽，否则测定结果将明显偏低。微波消解土壤与传统电热消解相比，操作简便快速，可提高工作效率。     

An Overview of Contaminant-Related Issues Identified by Monitoring in San Francisco Bay

The San Francisco Estuary Regional Monitoring Program for Trace Substances (RMP) began in 1993 and is sponsored by 74 local, state, and federal agencies and companies through their discharge or Bay use permits. The RMP monitors water, sediment, toxicity, and bivalve bioaccumulation at 25 sites in the Bay that are considered to represent "background" conditions. Several major environmental issues have been identified by the RMP. Polychlorinated biphenyls and mercury were often above water quality guidelines, and often occurred in fish tissues above U.S. Environmental Protection Agency (U.S. EPA) screening values. Concentrations do not appear to be decreasing, suggesting continuing inputs. Episodes of aquatic toxicity often occurred following runoff events that transport contaminants into the Bay from urbanized and agricultural portions of the watershed. Sediment toxicity occurred throughout the Bay, and has been correlated with concentrations of specific contaminants (chlordanes, polynuclear aromatic hydrocarbons) at some locations; mixtures of contaminants were probably also important. Since the RMP does not monitor all ecosystem components, assessments of the overall condition of the Bay cannot be made. However, in terms of contamination, the RMP samples suggest that the South Bay, and North Bay sites are moderately contaminated.     

Biomagnification factors (fish to Osprey eggs from Willamette River,Oregon, U.S.A.) for PCDDs,PCDFs, PCBs and OC pesticides

A migratory population of 78 pairs of Osprey (Pandion haliaetus) nesting along the Willamette River in westernOregon was studied in 1993. The study was designed to determinecontaminant concentrations in eggs, contaminant concentrationsin fish species predominant in the Ospreys diet, andBiomagnification Factors (BMFs) of contaminants from fish specieseaten to Osprey eggs. Ten Osprey eggs and 25 composite samplesof fish (3 species) were used to evaluate organochlorine (OC)pesticides, polychlorinated biphenyls (PCBs), polychlorinateddibenzo-p-dioxins (PCDDs), and polychlorinated dibenzofurans(PCDFs). Mercury was also analyzed in fish. Geometric meanresidues in Osprey eggs were judged low, e.g., DDE 2.3 g g^-1 wet weight (ww), PCBs 0.69 g g^-1, 2,3,7,8-TCDD 2.3 ng kg^-1, and generally well below known threshold values for adverse effects on productivity, and the population was increasing. Osprey egg residue data presentedby River Mile (RM) are discussed, e.g., higher PCDDs were generally found immediately downstream of paper mills and eggsfrom the Willamette River had significantly elevated PCBs and PCDDs compared to reference eggs collected nearby in the CascadeMountains. Prey remains at nest sites indicated that the Largescale Sucker (Catostomus macrocheilus) and NorthernPikeminnow (Ptychocheilus oregonensis) accounted for an estimated 90.1% of the biomass in the Osprey diet, and composite samples of these two species were collected from different sampling sites throughout the study area for contaminant analyses. With the large percentage of the fishbiomass in the Osprey diet sampled for contaminants (and fisheaten by Ospreys similar in size to those chemically analyzed),and fish contaminant concentrations weighted by biomass intake, a mean BMF was estimated from fish to Osprey eggs for the largeseries of contaminants. BMFs ranged from no biomagnification(0.42) for 2,3,7,8-TCDF to 174 for OCDD. Our findings for themigratory Osprey were compared to BMFs for the resident HerringGull (Larus argentatus), and differences are discussed. Webelieve a BMF approach provides some basic understanding ofrelationships between contaminant burdens in prey species offish-eating birds and contaminants incorporated into their eggs,and may prove useful in understanding sources of contaminants inmigratory species although additional studies are needed.     

The Draft of the New German Guideline VDI 3782/8 to Model Automobile Exhaust Dispersion

The draft of the German guideline to calculate automobile exhaust dispersion is explained. It contains a two-stage-system: For first quick estimates the guideline contains the simple models MLuS and STREET. In case these models are not applicable or their results shows concentration levels close to the air quality standards, the more complex models PROKAS_V and MISKAM are recommended. PROKAS_V is a Gaussian plume model, MISKAM is a 3-dimensional microscale non hydrostatic flow model for built-up areas with an Eulerian dispersion model. The guideline comprises cases in rural areas without or with few adjacent buildings as well as urban areas with buildings near the roads. The contribution gives information about the models, typical results and some of the problems showing up presently.     

Hydrocarbon Utilization in Yeast Isolates Found to Grow in Association with Petroleum in a Polluted Ultisol of Midwestern Nigeria

The population counts of hydrocarbon-utilising yeasts weremonitored at six sampling stations in the Benin City municipalarea over a four-week period. Although the population countswere relatively constant in each locality, the highest countsoccurred in areas heavily polluted by domestic and industrialeffluents. A total of thirty-five hydrocarbon-degrading yeastswere isolated from soil at the sampling stations usingn-hexadecane as sole carbon source. The isolates were identifiedas belonging to the genera Candida (27 strains), Endomycopsis (4 strains). All the organisms grew on long-chainn-alkane, kerosene, diesel oil and crude oil but failed to growon short-chain n-alkane, aromatic and alicyclic hydrocarbons.Measurement of growth attributes of the isolates usingn-hexadecane, diesel oil and crude oil as substrates showed thatthe Candida species were better utilizers of hydrocarbonsubstrates relative to Endomycopsis and Schizosaccharomyces species.     

Hydrologic–Economic Model for Managing Irrigation Intensity in Irrigation Areas under Watertable and Soil Salinity Targets

This paper gives mathematical details and sample applications of SWAGMAN Farm (SWAGMAN, Salt Water and Groundwater Management), a farm-scale hydrologic economic model that integrates agronomic, climatic, irrigation, hydrogeological and economic aspects of irrigated agriculture. The model is capable of determining optimum mix of land use to keep watertable and soil salinity within acceptable limits while maximising the economic returns. Alternatively, the model can simulate water and salt balance and economics of a given cropping preference. Web-based and Geographic Information Systems versions of the model are available for integration with the environmental reporting systems of the irrigation areas.     

火焰原子吸收光谱法测定苏州开发区26种蔬菜中铜锌铁锰镍

用火焰原子吸收光谱法测定了苏州开发区26种蔬菜中的铜、锌、铁、锰和镍的含量。蔬菜样品用硝酸高氯酸混合酸进行消解。4次测定值的相对标准差<5%,加标回收率在92%～107%之间。26种蔬菜中铜、锌、铁、锰、镍的含量基本均在世贸组织规定的范围内。     

Cyanobacterial Flora from Polluted Marine Shores

Citation of cyanobacterial cultures from the shores of south west coast of Gujarat, India and their relationship with sea water quality, influenced by extensive pollutant runoff is reported in this study. Intensity of pollution was evaluated by physico-chemical analysis of water. Higher load of suspended solids (60–1000 mg l⁻¹) and nutrients (PO₄ ⁻P: 1.3–4 μmole l⁻¹ and NO₃ ⁻N: 12.5–17.8 μmole l⁻¹) were persistent throughout the analysis. Community structure is seen to be influenced by such persistent pollution. Twenty nine cyanobacterial species were isolated belonging to 9 genera of 4 families, with an elevated occurrence of Oscillatoria and Lyngbya species. No heterocystous cyanobacteria were isolated throughout the study.     

Using Multiple Taxonomic Groups to Index the Ecological Condition of Lakes

Biological indicators of communitiestypically reflect a common environmental signalreflecting the general condition of the ecosystem, as well asindividual signals by indicators differentiallysensitive to particular environmental conditions. Wedescribe here a method of integrating and interpretingsuch indicators from 19 New England lakes for fivetaxonomic groups (diatoms, benthos, zooplankton, fish,and birds). Our approach provides a systematicstandardized way to integrate multiple metrics fromdifferent taxonomic groups by addressing four elementscrucial to analyzing data from multiple indicators: covariate control, re-scaling of data, standardizing the sign of responses, and dimensional reduction. We evaluated the biologicalmetrics against individual environmental stressors andagainst multivariate physicochemical metricscharacterizing general anthropogenic stress among thelakes. The method detected a response to variationin the gross environmental condition of the lakes thatwas correlated across taxa and metrics. In addition,a differential response to near shore conditions wasdemonstrated for fish. The success of the approach inthis study lends support to its general application toecological monitoring involving complex data sets.