固相萃取-气相色谱法测定水中多种农药类内分泌干扰物

建立了水样中用固相萃取小柱提取和净化、GC-ECD检测、GC-MSD定性证实的农药类内分泌干扰物检测方法,该方法样品提取、浓缩、净化步骤简便,能实现31种目标物同时检测。方法检测限0.05~0.50μg/L。添加回收率69%~101%,相对标准偏差低于10%。选择农药包括有机氯类(如滴滴涕、六六六、三氯杀螨醇、艾氏剂、异狄氏剂、狄氏剂、七氯、硫丹、氯丹等),氨基甲酸酯类(如甲草胺、乙草胺等),除虫菊酯类(如氯氰菊酯、速灭菊酯等)及其它农药(如氟乐灵、除草醚、毒死蜱)。该方法应用到测定某水库的水样,水库中31种农药类内分泌干扰物总浓度为48.8~890 ng/L,平均浓度295 ng/L。     

气相色谱—串联质谱法检测水中苯霜灵、甲霜灵、噁霜灵残留量

建立水中甲霜灵、苯霜灵、噁霜灵农药残留量的气相色谱—串联质谱(GC-MS/MS)的检测分析方法。样品采用乙腈提取、固相萃取(SPE)柱净化。采用GC-MS/MS分析时,三种农药在15 mim内完全分离并流出。添加浓度加标回收率为80.6%~88.4%,相对标准偏差(RSD)小于5.0%。在0.01~0.20 mg/L质量浓度范围之间线性关系良好(r~20.999 0)。该方法的灵敏度、精密度和准确度均满足农药残留分析要求,适用于水中的农药残留的快速筛查与定性、定量分析。     

基于荧光素酶发光体系测试饮用水中农药的综合毒性

利用农药对荧光素酶催化的发光反应具有非常显著的抑制作用,对甲拌磷、乐果、毒死蜱、百草枯等4种农药分别进行单一毒性和等比混合法联合毒性测试,建立了一种快速检测饮用水中农药综合毒性的生物学方法。试验结果表明,单一农药乐果、甲拌磷、百草枯和毒死蜱的EC50值分别为7.56 mg/L、12.7 mg/L、19.0 mg/L和65.3 mg/L,毒性强弱顺序为乐果甲拌磷百草枯毒死蜱,相关系数≥0.995;将4种农药以等比方式配制成两两混合液后,当质量浓度为20.0 mg/L~100 mg/L时,除百草枯与毒死蜱表现为毒性协同外,其他两两混合农药的毒性以拮抗作用为主。     

酶抑制法检测蔬菜中的有机磷农药

对新型酶抑制检测蔬菜中有机磷农药残留量的方法进行了研究,介绍了胆碱酯酶的提取、纯化方法,以及用粗酶和纯酶检测蔬菜中有机磷农药残留量的测定效果,确定了最佳实验条件。对样品的预处理方法进行了改进,得出该法的检测限为1mg／L,对甲基对硫磷等几种常用农药的加标回收率为90．4％～112％,相对标准偏差为1．06％～9．83％,表明三项评价指标均符合全国农药残留科研协作组对农药残留分析方法的基本要求。     

北京工业废水和城市污水中有机氯农药残留分析

建立了基于HLB固相萃取柱和气相色谱-电子捕获(GC-ECD)测定水体中有机氯农药的方法,并对方法的回收率、灵敏度进行了评价,同时分析了北京市七类典型污染点源50个采样点位有机氯农药的浓度,检测到的有机氯农药包括γ-六六六、β-六六六、4,4’-滴滴涕、α-六六六、δ-六六六、硫丹Ⅰ、4,4’-滴滴伊、艾氏剂和异狄氏剂,它们的检出率分别为90%、60%、50%、46%、26%、8%、6%、2%和2%。主要有机氯农药污染残留为γ-六六六、β-六六六和4,4’-滴滴涕。检出有机氯农药浓度范围是0.20~76.40ng/L。方法对有机氯农药的回收率达到60.93%~141.50%,方法检测限为0.27~2.90ng/L。     

城市污水处理厂水样中菊酯类农药残留分析

建立了基于C18固相萃取柱和气相色谱/电子捕获(GC/ECD)分析水体中环境激素类物质——菊酯类农药的分析方法,并对方法的回收率、灵敏度进行了评价,同时分析了北京市高碑店、北小河两个城市污水处理厂进水与出水中菊酯类农药的浓度,研究发现在其废水中存在联苯菊酯、氯氰菊酯、氰戊菊酯和溴氰菊酯,浓度在0.013~0.920μg/L之间。结果表明,曝气活性污泥法对菊酯类农药的去除效果较好。方法对菊酯类农药的回收率达到67.7%~96.2%,方法检测限为0.010~0.015μg/L。     

江苏省主要农药产品的环境残留监测方法研究

介绍了江苏省生产的主要农药品种，综述了草甘膦、丁草胺、乙草胺、百草枯和氟乐灵等5种除草剂，代森锰锌、戊唑醇、百菌清、甲基硫菌灵和三环唑等5种杀菌剂，毒死蜱、吡虫啉、氯氰菊酯等3种杀虫剂，以及乙烯利、多效唑等2种植物生长调节剂的生产现状及危害，以及上述农药在水、土壤等环境介质中的检测方法。以期为相关农药残留的检测方法标准化、环境中控制限值的制定、农药类环境事故应急监测以及农药生产与使用的环境监管提供技术支持。     

邕江流域有机氯农药残留问题的初步研究

采用固相萃取和GC-ECD对邕江流域水体中17种痕量有机氯农药的残留状况进行分析测定,检测结果表明,邕江干流均检出硫酸硫丹,但有机氯农药浓度较低,均未超过现有相关标准。城市内河残留的有机氯农药以六六六为主,主要来自于长期的历史残留,而硫酸硫丹除朝阳溪和相思湖丰水期未检测到外,均普遍检出。方法检出限为1~5ng/L,替代物加标回收率为103.5%~112.0%。     

气相色谱法测定果蔬中有机氯农药

建立了果蔬中8种有机氯农药气相色谱—电子捕获检测器检测方法。样品用丙酮浸泡,石油醚提取,浓硫酸净化,以HP-5毛细管柱作为分离柱,经程序升温分离各组份,以峰面积外标法定量,能有效分离8种有机氯农药,并能消除基质干扰。取样量25 g时,该法在0.00320~0.126 mg/L具有良好的线性,最低检出浓度为六六六0.0025~0.0042μg/kg、DDT 0.0029~0.0069μg/kg。用此方法在全国土壤调查中对新疆区内果蔬进行检测,获得了较为满意的结果。     

超高效液相色谱 三重四极杆质谱法测定地表水和地下水中11种三嗪类农药

建立了针对地表水和地下水中11种三嗪类农药的超高效液相色谱三重四极杆质谱分析方法,并对前处理、仪器分析、方法特性指标等因素进行优化探讨。使用SB-C18色谱柱、乙腈水二元混合液流动相进行化合物分离,设置柱温为40℃、进样量为10μL,质谱采用正离子模式检测,内标法定量,采用平均相对响应因子法拟合标准曲线。结果表明,11种三嗪类农药的方法检出限为0.003~0.01μg/L,对3种质量浓度的基体加标样品分别进行6次平行分析,测定结果的相对标准偏差为2.1%~19%,平均加标回收率为80.0%~108%。采集地表水和地下水样品,经尼龙或聚四氟乙烯滤膜过滤后上机测定,在1种地表水样品中检出了阿特拉津和扑灭津,平均质量浓度分别为0.032和0.009μg/L。该方法具有准确度高、重复性好、检出限低等优点,能够满足现阶段地表水和地下水的环境管理监测要求。     

Mercury in Tree Swallow Food, Eggs, Bodies, and Feathers at Acadia National Park, Maine, and an EPA Superfund Site, Ayer, Massachusetts

We monitored nest boxes during 1997–1999 at Acadia National Park, Mt. Desert Island, ME and at an old-field site in Orono, ME to determine mercury (Hg) uptake in tree swallow (Tachycineta bicolor) eggs, tissues, and food boluses. Also, in 1998–1999 we monitored nest boxes at Grove Pond and Plow Shop Pond at a U.S. Environmental Protection Agency Superfund site in Ayer, MA. We recorded breeding success at all locations. On average among locations, total mercury (THg) biomagnified 2 to 4-fold from food to eggs and 9 to 18-fold from food to feathers. These are minimum values because the proportion of transferable methyl mercury (MeHg) of the THg in insects varies (i.e., 35%–95% of THg) in food boluses. THg was highest in food boluses at Aunt Betty Pond at Acadia, whereas THg in eggs was highest at the Superfund site. A few eggs from nests at each of these locations exceeded the threshold (i.e., 800–1,000 ng/g, wet wt.) of embryotoxicity established for Hg. Hatching success was 88.9% to 100% among locations, but five eggs failed to hatch from 4 of the 11 clutches in which an egg exceeded this threshold. MeHg in feathers was highest in tree swallows at Aunt Betty Pond and the concentration of THg in bodies was related to the concentration in feathers. Transfer of an average of 80%–92% of the Hg in bodies to feathers may have enhanced nestling survival. Residues of Hg in tissues of tree swallows in the Northeast seem higher than those of the Midwest.     

Concentration of Cd, Cu, Pb, Zn, Al, and Fe in soils of Manresa, NE Spain

The aims of this study were to determine the contents of cadmium (Cd), copper (Cu), lead (Pb), zinc (Zn), aluminium (Al), and iron (Fe) (aqua regia-extractable) in 27 soil plots (54 samples) from Manresa, NE Spain, and to establish relationships between heavy metals and some soil properties. The main soil types were surveyed and the median concentrations (mg kg(-1)) obtained were Cd 0.28, Cu 20.3, Pb 18.6, Zn 67.4, Al 22,572, and Fe 21,551. Element concentrations for these soils were lower than the published values for the Valencia region (Spain) and Torrelles and Sant Climent municipal districts (Catalonia, Spain). In terms of soil properties, the results of this study suggest that, in Manresa soils, both trace element adsorption and retention are influenced by several properties such as clay minerals, carbonates, organic matter, and pH. All element contents were positively correlated with clay content. Pb and Zn were negatively correlated with pH and CaCO(3).     

电感耦合等离子体原子发射光谱法测定水中钡、铍、硼、钒、钴、钛、钼7种微量元素

用电感耦合等离子体原子发射光谱法测定水中Ba、Be、B、V、Co、Ti、Mo 7种元素含量,具有测定方法简便、快速、准确、精密度高、数据可靠等特点。     

微波消解—原子吸收/原子荧光光度法测定活性污泥中的Cd、Pb、Ni、Cu、Zn、Cr、K、As、Hg

通过实验,建立了活性污泥中金属和重金属的测定方法。活性污泥样品经硝酸—氢氟酸或硝酸—高氯酸微波消解处理后,Pb、Ni、Cu、Zn、Cr、K选用火焰原子吸收分光光度法测定,Cd用石墨炉原子吸收分光光度法测定,As、Hg用原子荧光光度法测定。该方法操作简单,结果准确,重现性好。样品加标回收率为93%-108%,相对标准偏差〈5%。     

Determination of Cu, Pb, Zn, Ni, Co, Cd, and Mn in road dusts of Samsun City

The dust samples from 52 different locations in central roads of Samsun City were collected in a study area of 40 km long for the purpose of determining total metal concentrations of dust samples by flame atomic absorption spectrometry. The concentrations of Cu, Pb, Co, Zn, Ni, Mn, and Cd were found in the ranges of 11.92–352.43, 5.47–223.57, 4.52–41.69, 40.85–173.10, 18.71–131.29, 133.19–179.13, and 0.02–6.16 mg/kg, respectively. The results showed that metal levels were higher around the industrial area than other locations. Principal component analysis was also carried out to ascertain the possible contributing factors towards the metal concentrations. Validation of the analytical results was tested by analysis of the BCR 032 Moroccan phosphate rock certified reference material.     

Concentrations of Arsenic, Cadmium, Copper, Lead, Selenium, and Zinc in Fish from the Mississippi River Basin, 1995

Fish were collected in late 1995 from 34 National Contaminant Biomonitoring Program (NCBP) stations and 12 National Water Quality Assessment Program (NAWQA) stations in the Mississippi River basin (MRB), and in late 1996 from a reference site in West Virginia. The NCBP sites represented key points (dams, tributaries, etc.) in the largest rivers of the MRB. The NAWQA sites were typically on smaller rivers and were selected to represent dominant land uses in their watersheds. The West Virginia site, which is in an Eastern U.S. watershed adjacent to the MRB, was selected to document elemental concentrations in fish used for other aspects of a larger study and to provide additional contemporaneous data on background elemental concentrations. At each site four samples, each comprising (nominally) 10 adult common carp (Cyprinus carpio, 'carp') or black bass (Micropterus spp., 'bass') of the same sex, were collected. The whole fish were composited by station, species, and gender for analysis of arsenic (As), lead (Pb), and selenium (Se) by atomic absorption spectroscopy and for cadmium (Cd), copper (Cu), and zinc (Zn) by inductively-coupled plasma emission spectroscopy. Concentrations of most of the elements examined were lower in both carp and bass from the reference site, a small impoundment located in a rural area, than from the NCBP and NAWQA sites on rivers and larger impoundments. In contrast, there were few overall differences between NCBP sites NAWQA sites. The 1995 results generally confirmed the continued weathering and re-distribution of these elemental contaminants in the MRB; concentrations declined or were unchanged from 1984-1986 to 1995 at most NCBP sites, thus continuing two-decade trends. Exceptions were Se at Station 77 (Arkansas R. at John Martin Reservoir, CO), where concentrations have been elevated historically and increased slightly (to 3.8-4.7 microg g-(1) in bass and carp); and Pb, Cd, and Zn at Station 67 (Allegheny R. at Natrona, PA), where levels of these metals were high in the past and increased from 1986 to 1995.     

A survey of Pb,Cu, Zn,Cd, Cr,As, and Se in earthworms and soil from diverse sites

Earthworms and soils were collected from 20 diverse sites in Maryland, Pennsylvania, and Virginia, and were analyzed for Pb, Cu, Zn, Cd, Cr, As, and Se. Correlation coefficients relating concentrations of the elements in earthworms to concentrations in soil were low (–0.20<r<+0.57). Species differences and ecological variables contributed to the variability in concentrations of these elements in earthworms. The maximum concentrations of Pb (2100 ppm), Zn (1600 ppm), Cd (23 ppm) and Se (7.6 ppm) detected in earthworms were in the range reported to be toxic to animals fed diets containing these elements; however, even in the absence of any environmental contamination, some species of earthworms may contain high concentrations of Pb, Zn, and Se. Earthworms of the genus Eisenoides, for example, were exceptional in their ability to concentrate Pb. When earthworms are used as indicators of environmental contamination, it is important to identify the species, to report the soil characteristics, and to collect similar earthworms from very similar but uncontaminated soil.     

The impact of terrorism and FDI on environmental pollution: Evidence from Afghanistan,Iraq, Nigeria,Pakistan, Philippines,Syria, Somalia,Thailand and Yemen

In this study, the relationships among environmental pollution, terrorism, foreign direct investments (FDI), energy consumption and economic growth is investigated for Afghanistan, Iraq, Nigeria, Pakistan, Philippines, Syria, Somalia, Thailand and Yemen covering the 1975–2017 period utilizing Panel cointegration tests, ANOVA tests, long-run estimators and panel trivariate Causality tests. ANOVA results are in favor of evidence of homogeneity between the selected countries. Long-run estimators reveal that terrorism, FDI, energy consumption and economic growth have statistically significant effects on environmental pollution. Panel trivariate Causality test determines the causal relationship between the variables. Accordingly, one-way causal nexus from terrorism to Carbon dioxide (CO₂) emissions and from FDI inflows to CO₂ emissions are found in the short-run. In the long-run, with strong causality results, the evidence of bi-directional causality between CO₂ emissions and other variables, namely, terrorism, FDI inflow energy consumption and economic growth are detected.     

Fluoride in groundwater, Varaha River Basin, Visakhapatnam District, Andhra Pradesh, India

Excess intake of fluoride through drinking water causes fluorosis on human beings in many States of the country (India), including Andhra Pradesh. Groundwater quality in the Varaha River Basin located in the Visakhapatnam District of Andhra Pradesh has been studied, with reference to fluoride content, for its possible sources for implementing appropriate management measures, according to the controlling mechanism of fluoride concentration in the groundwater. The area occupied by the river basin is underlain by the Precambrian Eastern Ghats, over which the Recent sediments occur. Results of the chemical data of the groundwater suggest that the considerable number of groundwater samples show fluoride content greater than that of the safe limit prescribed for drinking purpose. Statistical analysis shows that the fluoride has a good positive relation, with pH and bicarbonate. This indicates an alkaline environment, as a dominant controlling mechanism for leaching of fluoride from the source material. Other supplementary factors responsible for the occurrence of fluoride in the groundwater are evapotranspiration, long contact time of water with the aquifer material, and agricultural fertilizers. A lack of correlation between fluoride and chloride, and a high positive correlation between fluoride and bicarbonate indicate recharge of the aquifer by the river water. However, the higher concentration of fluoride observed in the groundwater in some locations indicates insufficient dilution by the river water. That means the natural dilution did not perform more effectively. Hence, the study emphasizes the need for surface water management structures, with people's participation, for getting more effective results.     

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。