固相萃取-高效液相色谱法测定生活污水中壬基酚聚氧乙烯醚及其降解产物

比较了液-液萃取和固相萃取浓缩富集水体中壬基酚聚氧乙烯醚(NPnEO,n为聚合度)及其小分子代谢产物的效率,建立了复杂基体水样中壬基酚聚氧乙烯醚及其小分子代谢产物多成分同时测定的高分辨高灵敏的固相萃取(SPE)-正相高效液相色谱(NP-HPLC)-荧光检测(FL)方法。优化了影响SPE回收率的条件,洗脱溶剂和样品过柱的速度。SPE对NPnEO的回收率大于82%;使用1L水样,方法的检测限对壬基酚(NP)、NP1EO为0.01μgL,NP2EO、NP3EO为0.02μgL,NP4EO～NP12EO为0.05μgL。应用本方法测定了生活污水水样,检测到了NPnEO(n=1～12)及其小分子降解产物NP、NP1EO、NP2EO。     

加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法测定沉积物中5种微囊藻毒素

建立了加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法同时测定沉积物中5种微囊藻毒素(MC-LR、MC-RR、MC-LW、MC-LF、MC-YR)的方法。选择甲醇-水(1∶4,V/V)为ASE萃取溶剂,萃取温度和萃取压力分别为80℃和13.1 MPa,固相萃取过程以HLB小柱为萃取柱,采用液相色谱-串联质谱分析。方法在5种微囊藻毒素质量浓度5~100μg/L内线性良好(r0.995),回收率为76.0%~118%,相对标准偏差为1.9%~12.0%,检出限为2~3μg/kg,定量下限为8~12μg/kg。该方法已用于西太湖沉积物的检测,具有较好的方法适用性。     

固相微萃取与气相色谱-质谱联用测定饮用水中甲基叔丁基醚

采用固相微萃取与气相色谱-质谱联用测定饮用水中甲基叔丁基醚(MTBE),研究了萃取头涂层材料、萃取温度、盐浓度、萃取时间和溶液的pH值等操作条件对分析方法的影响.该方法分析MTBE的线性范围0.01-10μg/L,检出限0.66ng/L.0.01μg/L的MTBE水样五组平行测定实验中,相对标准偏差为4.8%.用所建立的方法测得大兴某地下水中MTBE的含量0.8μg/L,加标回收率达到90%.     

固相微萃取-气相色谱法测定水中痕量甲萘威

建立了固相微萃取-气相色谱法测定水中痕量甲萘威的方法,并对固相微萃取条件进行了优化。结果显示,固相萃取的最佳条件为:水样pH值≤3,不添加无机盐,聚二甲基硅氧烷(PDMS,100μm)作为萃取纤维,萃取温度为80℃,萃取时间为30 min,解吸时间为90 s。优化后的方法,在甲萘威质量浓度0.01~1.0 mg/L范围内线性良好,相关系数为0.999 5,方法的精密度为1.9%,检出限为0.3μg/L,加标回收率为85.6%~92.4%,可满足地表水中甲萘威的测定要求。     

顶空固相微萃取-气相色谱-串联质谱法测定水中2,4,6-三氯酚

建立了顶空固相微萃取-气相色谱-串联质谱法(HS-SPME-GC-MS-MS)测定水中2,4,6-三氯酚的方法。优化条件下,在1. 00～50. 0μg/L质量浓度范围内线性响应良好(r~2=0. 999 1);检出限0. 224μg/L,测定下限0. 896μg/L;加标样相对标准偏差(RSD)为4. 15%～6. 24%;加标回收率为81. 0%～115%;单个样品检测总时间40 min。该方法萃取与气相色谱-串联质谱分析在线一步完成,操作简便、灵敏度高、抗干扰性强,适用于地表水、生活饮用水、工业废水等水体中2,4,6-三氯酚的检测。     

2-(2-吡啶偶氮)-间苯二酚固相萃取光度法测定镉的研究

研究了用2-(2-吡啶偶氮)-间苯二酚(PAR)固相萃取光度法测定镉,在pH=8 0的硼酸-氢氧化钠缓冲介质中,TritonX-100存在下,QAMDHB与镉反应生成2∶1稳定络合物,体系最大吸收波长为520nm,摩尔吸光系数 =5 18×104L·mol-1·cm-1。样品中的镉用强阴离子交换固相萃取柱固相萃取预分离和富集后,用该方法测定,结果令人满意。     

固相萃取-高效液相色谱-质谱联用法测痕量双酚A的方法优化

通过优化固相萃取和液相色谱条件,建立了固相萃取-高效液相色谱-质谱法测定水中双酚A的检测方法.水样经C18固相萃取柱净化并富集双酚A后,采用C18反相色谱柱XR-ODS(2.0 mm×100 mm,2.2μm)分离,MRM负离子模式测定.结果表明:BPA浓度为5～200 ng/L范围内线性关系良好(相关系数为0.999...     

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。     

2-(2-吡啶偶氮)-5-二甲氨基酚固相萃取光度法测定环境样品中钴(Ⅱ)的研究

根据新试剂2-(2-吡啶偶氮)-5-二甲氨基酚(PADMAP)与钴的显色反应及C18固相萃取小柱对显色络合物的固相萃取,建立了一种测定环境样品中痕量钴的新方法,在pH4 0的HAc—NaAc缓冲介质中,溴化十六烷基三甲基铵(CTMAB)存在下,PADMAP与钴反应生成2∶1稳定络合物,该络合物可用C18固相萃取小柱富集,小柱上富集的络合物用乙醇(内含2%乙酸)洗脱后用光度法测定。络合物最大吸收波长为585nm,摩尔吸光系数为1 05×105L·mol-1·cm-1,钴含量在0—1 0mg/L内符合比耳定律。方法用于几种环境样品中钴的分析,结果令人满意。     

北京公园水体中邻苯二甲酸酯类物质的测定及其分布特征

为了正确评估北京市公园水体受PAEs污染的程度,采集了北京11个公园湖水的水样,采用固相萃取-气相色谱联用技术检测了其中六种邻苯二甲酸酯类物质(PAEs)的含量,该方法加标回收率在73%～89.3%,RSD为5.9%～18.1%,检出限在0.40～4.58mg/L。实验结果为北京公园水体中总PAEs浓度在6.4～138.1μg/L,平均值为27.9μg/L,证明北京公园水体受到不同程度的PAEs污染,主要的污染物为邻苯二甲酸二丁酯(DBP)和邻苯二甲酸双(2-乙基己基)酯(DEHP),其中东南部以及西北部的公园污染较严重。分析了PAEs在公园湖水底泥中和水体中的分布特征,结果显示,PAEs在湖水底泥中的含量明显大于在水体中的含量。     

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。     

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.     

Concentrations of Cadmium, Mercury and Selenium in Blood, Liver and Kidney of Common Eider Ducks from the Canadian Arctic

We determined concentrations of selected trace elements inlivers, kidneys and blood samples from common eiders (Somateria mollissima borealis) from the eastern Canadianarctic during 1997 and 1998. Concentrations of totalmercury and organic mercury were generally low in the liversof these birds (less than 6 and 4 g g^–1 dry wt,respectively). Selenium ranged between 11–47 g g^–1 inlivers. Renal cadmium concentrations were among the highestever published for this species (range: 47–281 g g^–1). The regressions of log-transformed concentrations ofthese trace elements in blood samples on those in liver orkidney were significant (all P-values < 0.05) andpositive. However, except for organic mercury (RM ² = 0.83), the co-efficients of determination were low tomoderate (range of R ²: 0.26–0.52), suggesting poorto moderate predictive capability. Furthermore, therelationships between total mercury in blood and liverchanged between 1997 and 1998, suggesting that it would notbe possible to predict consistently, concentrations ofmercury in blood from those in liver based on samples takenin one year. Blood samples can be used to determineconcentrations of these trace elements in common eiders (andprobably other sea duck species as well). The use of bloodsamples is especially warranted when it is undesirable tokill the animal such as when working with rare or endangeredsea duck species or when the objective is to relate traceelement exposure to annual survival rates. However, thepredictive equations developed here should not be used topredict expected concentrations in one type of tissue fromthose in the other.