水质丁基黄原酸测定难点探讨

丁基黄原酸是水质监测的重要项目之一。水中丁基黄原酸的测定,在样品采集保存、前处理及仪器分析各阶段都存在一定的技术难点。实际分析时很容易出现测定结果不理想,甚至定性定量错误等问题。结合实验对丁基黄原酸测定中容易出现的问题及注意事项进行探讨,正确区分丁基黄原酸及其盐,有效保存样品,采用低损失的前处理方法以及选择性好的分析仪器,有利于提高丁基黄原酸测定的准确性。众多丁基黄原酸测定方法中,液相色谱质谱法、离子色谱法以及液相色谱法在选择性和灵敏度方面更具优势,也可用于其他方法检出丁基黄原酸时对测定进行确认。     

顶空-气相色谱-质谱法测定水中痕量丁基黄原酸

建立了顶空-气相色谱-质谱联用测定水中丁基黄原酸的方法。丁基黄原酸在酸性条件下分解成易挥发的二硫化碳,可用顶空-气相色谱分离、质谱定量测定。与传统的分光光度法相比,该法简便、快捷,在0.010～1.00 mg/L范围内线性良好,准确度高,加标回收率为95.1%～100.6%,精密度好,相对标准偏差为3.1%～6.5%,方法检出限为0.002 mg/L,适用于水中丁基黄原酸的监测。     

吹扫捕集-气相色谱-质谱法测定水中痕量丁基黄原酸

建立了吹扫捕集-气相色谱-质谱联用测定水中丁基黄原酸的方法.丁基黄原酸在酸性条件下分解成易挥发的二硫化碳,经吹扫捕集富集后用气相色谱分离质谱定量测定.与传统的分光光度法相比,更简便快捷,在0.25～10.0μg/L范围内线性良好,准确度高,添加回收率为98.3％～105％,精密度好,相对标准偏差为5.92％ ～ 10.7％,方法检出限为0.07μg/L.与顶空法相比,灵敏度更高.     

地表水中丁基黄原酸的保存条件研究

通过对不同基质地表水样中丁基黄原酸在p H值、温度、光照、保存时间等条件下进行保存研究,确定对其保存效果的影响为:保存时间保存温度样品中丁基黄原酸浓度光照强度p H值。建议地表水样品使用棕色玻璃瓶盛装,于4℃下避光保存原水。高浓度样品,保存时间不超过5 d;低浓度样品,保存时间不超过1 d,最好采样后立即分析。     

离子色谱—三重四极杆质谱测定环境水样中有机磷

建立了一种非衍生—离子色谱—三重四极杆质谱法测定环境水样中有机磷（草甘膦、氨甲基膦酸、草铵膦、杀木膦和乙烯利）的方法。环境水样经RP-C18固相萃取柱和Ba柱除去杂质后,滤液无须衍生化,可直接进行定量分析。有机磷通过AS 19阴离子色谱柱分离,在负离子模式下以多反应监测方式（MRM）进行检测。结果表明,草甘膦、氨甲基膦酸和草铵膦在0.10～10.0 μg/L范围内的线性相关系数（r）均＞0.999,检出限分别为0.02,0.03和0.03 μg/L,相对标准偏差（RSD）分别为2.8%～4.7%,5.4%～11.7%和5.1%～7.4%。杀木膦和乙烯利在0.02～2.00 μg/L范围内的 r 值均＞0.999,检出限分别为0.007和0.004 μg/L,RSD分别为3.7%～5.8%和2.1%～13.2%。对实际水样进行测定,各目标物的加标回收率为70.0%～120%。该方法操作简便,精密度好,准确度高,适用于环境水样中5种极性有机磷的测定。     

超高效液相色谱法快速检测地表水中丁基黄原酸

建立了直接进样-超高效液相色谱分离-紫外吸收测定地表水中丁基黄原酸的分析方法。通过对流动相的优化,确定最佳分析条件:0.050 mol/L超纯水乙酸铵溶液(pH约为9.5):乙腈=80:20等度洗脱,Waters ACQUITY UPLC BEH C₁₈色谱柱(50 mm×2.1 mm,1.7 μm)分离,流速0.30 mL/min,进样体积10.0 μL,302 nm紫外吸收。结果显示,0.5～20.0 μg/L范围线性良好,R=0.9998; 2.0、10.0、20.0 μg/L重复测定,变异系数小于5%,精密度良好;实际水样加标回收率为95.5%～101.6%;以3倍信噪比计算得出检出限为0.80 μg/L。该方法分析速度快,2 min内可完成,满足环境质量监测要求。     

水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究

建立柱前衍生-液相色谱-荧光检测法同时测定水中草甘膦和氨甲基膦酸的方法。水样经芴甲氧羰酰氯衍生化后取上清液进样,采用ODS C18柱,以水(5 mmol/L乙酸铵)-乙腈作为流动相进行梯度洗脱,采用荧光检测器进行检测。实验通过加入柠檬酸三钠,解决了实际水样中金属阳离子的干扰问题。草甘膦和氨甲基膦酸在一定范围内线性良好(r=0.997 3~0.999 0),回收率为92.2%~102%,相对标准偏差为4.3%~8.5%,方法检出限为1.29μg/L和1.84μg/L。     

高效液相色谱法测定柑橘及橘园土壤中乙撑硫脲残留

建立了高效液相色谱测定柑橘及橘园土壤中乙撑硫脲残留的方法,优化了试验条件.方法在0 mg/L～5.35 mg/L范围内线性良好,橘园土壤、橘皮、橘肉样品的检出限(以鲜重计)分别为0.006 mg/kg、0.008 mg/kg、0.006 mg/kg,样品测定的RSD≤5.1%,加标回收率为82.9%～92.8%.     

铜试剂亚铜分光光度法测定水中丁基黄原酸

在盐酸羟胺还原体系中萃取，用铜试剂将丁基黄原酸亚铜转化成铜试剂亚铜，进而分光测定丁基黄原酸的新方法，大大提高了比色法的灵敏度，其浓度在０￣８０μｇ／Ｌ符合比耳定律，相对误差小于１．５％，平均回收率达９２％￣１０５％，适用于水中丁基黄原酸的测定。     

加速溶剂萃取-气相色谱质谱法同时测定土壤及沉积物中34种有机氯农药及18种多氯联苯类化合物

建立了加速溶剂萃取-气相色谱质谱法同时测定34种有机氯农药(OCPs)和18种多氯联苯类化合物(PCBs)的方法。当取样量为10. 0 g时,52种有机化合物的检出限为0. 03～0. 29μg/kg,以空白样品为基体进行加标回收试验,平均回收率为44. 7%～123. 0%,相对标准偏差(RSD,n=7)为1. 8%～21. 5%。该方法灵敏度高,实现了低浓度有机化合物的定量分析,分析结果准确可靠,满足土壤和沉积物中34种有机氯农药和18种多氯联苯类化合物分析的要求。     

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.