固相微萃取—气相色谱法测定水中痕量硝基苯类化合物

建立了固相微萃取种类与气相色谱联用测定地下水中12种硝基苯类化合物的分析方法,对萃取头种类、萃取时间、萃取温度、进样口衬管种类等分析条件进行了优化。实验结果表明,该方法的检出限为0.001~0.050 μg/L,线性范围0.005~500 μg/L（相关系数大于0.997）,加标回收率为72.1%~122.0%,相对标准偏差为3.65%~12.60%。应用该方法对地下水及地表水样品进行分析,结果表明该方法具有环保、灵敏、快速、简便等特点,适用于水中痕量硝基苯、硝基甲苯类化合物和硝基氯苯类化合物的测定。     

专利文摘

<正>一种选择性降解高毒性多氯联苯及类二噁英的方法该专利涉及一种选择性降解高毒性多氯联苯及类二噁英的方法,解决了现有方法选择性差、不易操控且容易造成二次污染等问题。该专利以蒙脱土为模板,在蒙脱土层间原位合成Fe~0-Ni~0双金属材料,在厌氧条件下对多氯联苯及类二噁英进行降解,通过蒙脱土结构提高金属对多氯联苯及类二噁英脱氯加氢的能力,且通过黏土特殊的层板结构实     

液液萃取—GC-MS法同时测定石化废水中双酚A和邻苯二甲酸二乙酯

建立了液液萃取(LLE)—气相色谱-质谱(GC-MS)法同时测定石化废水中双酚A(BPA)和邻苯二甲酸二乙酯(DEP)的新方法,对液液萃取条件进行了优化。最佳的液液萃取条件为:萃取剂为乙酸乙酯,水样调成酸性(pH2),每次加入萃取剂0.1 mL/mL、盐析剂NaCl 0.1 g/mL,萃取次数为6次,每次萃取时间为2 min。实验结果表明:在质量浓度1～100 mg/L的范围内,BPA和DEP测定标准曲线的线性关系良好;BPA和DEP的检出限(LOD)分别为5.18μg/L和0.89μg/L,定量限(LOQ)分别为17.11μg/L和2.96μg/L,回收率为81.4%～124.9%,相对标准偏差(RSD)(n=7)小于5.5%。     

盐析分相微萃取—高效液相色谱法测定水中含氯除草剂

采用盐析分相微萃取—高效液相色谱法同时测定水中3种含氯除草剂，建立并优化了反相离子对液相色谱条件，考察了萃取剂种类、盐析剂的种类和加入量及试样pH对萃取效果的影响。对氯苯氧乙酸、2，4-二氯苯氧乙酸和2，4-滴丁酯的质量浓度在0.1~100.0mg/L内与色谱峰面积呈良好的线性关系，相关系数不低于0.9992。平均回收率分别为96.29%、79.16%和70.21%，相对标准偏差小于5.3%。该方法操作简便、绿色环保，适合于水中含氯除草剂的测定。     

流动注射-氢化物发生-原子吸收法测定土壤中微量砷

用混酸消解土壤试样，用体积分数为20％的盐酸作酸介质，质量分数为1．5％的硼氢化钾作还原剂，体积分数为1％的盐酸作载液，采用流动注射-氢化物发生三-原子吸收法定量测定土壤中的微劈砷。通过实验确定，在原子化温度为920℃、土壤中共存元素含量低于5mg／kg时对测定无干扰。该方法的榆出限为0．5μg/L，线性范嘲为5～100μg/L．相对标准偏差为0．89％，平均回收率达98．99％：     

盐析分相微萃取—高效液相色谱法测定水中取代苯

建立了测定水中三种取代苯的盐析分相微萃取—高效液相色谱分析方法。实验结果表明,当异丁醇萃取剂加入量为300μL、(NH_4)_2SO_4加入量为14 g、流动相V(甲醇):V(水)为80:20、检测波长为220 nm时,邻氯苯酚、氯苯、乙苯的工作曲线均呈现良好线性(相关系数大于0.999 9),方法检出限分别为0.07,0.2,9.0μg/L,加标回收率为71.66%～92.96%,相对标准偏差为1.17%～5.17%。     

还原去氯—高压液相色谱法测定变电站土壤中残留的多氯联苯

本文叙述了用氢化铝锂将多氯联苯去氯还原成联苯,然后用带萤光检测器的高压液相色谱法测定变电站土壤样品中残留的多氯联苯的实验方法,检测限可达0.5毫微克。该方法无需用多氯联苯标样作对照,操作简便、实用。     

液液萃取—GC-MS法同时测定石化废水中双酚A和邻苯二甲酸二乙酯

建立了液液萃取（LLE）—气相色谱-质谱（GC-MS）法同时测定石化废水中双酚A（BPA）和邻苯二甲酸二乙酯（DEP）的新方法,对液液萃取条件进行了优化。最佳的液液萃取条件为：萃取剂为乙酸乙酯,水样调成酸性（pH<2）,每次加入萃取剂0.1 mL/mL、盐析剂NaCl 0.1 g/mL,萃取次数为6次,每次萃取时间为2 min。实验结果表明：在质量浓度1~100 mg/L的范围内,BPA和DEP测定标准曲线的线性关系良好;BPA和DEP的检出限（LOD）分别为5.18 μg/L和0.89 μg/L,定量限（LOQ）分别为17.11 μg/L和2.96 μg/L,回收率为81.4 %~124.9 %,相对标准偏差（RSD）（n=7）小于5.5 %。     

从苯酐生产废水中萃取富马酸

用三辛癸胺和三辛胺为萃取剂,在无稀释剂的条件下,对苯酐生产废水中的富马酸进行了络合萃取研究。研究结果表明,萃取剂的负荷量与相比呈递减的幂函数关系,三辛癸胺比三辛胺的络合酸度大;温度对萃取处理效果有明显影响,温度为10～40℃时,萃取剂的负荷量随着温度的升高而增加,但温度过高易造成乳化,最佳操作温度为30～40℃;用氢氧化钠溶液再生萃取剂,最佳反萃操作条件为:振荡时间60s、相比(水/油,体积比)2、温度60℃、碱液质量浓度12g/L;萃取剂9次循环萃取和再生使用过程中,萃取率稳定在71 8%±1 7%,再生效率稳定在94 3%±1 9%,9次循环后萃取剂的损失量为4%;从每吨废水中可回收富马酸4 8kg,可获益24元。     

膜过滤-气相色谱法测定涂料中的苯系物、环己酮和甲苯二异氰酸酯

采用膜过滤-气相色谱法测定涂料中的苯系物、环己酮和甲苯二异氰酸酯（TD I）。用7种规格的石英毛细管色谱柱对混合标准溶液和涂料试样进行了分析实验,实验结果表明,不同属性的涂料试样添加固定量的正十四烷作内标物,经膜过滤净化后,苯系物、环己酮和TD I可采用DB-1-3或DB-1-2色谱柱同时分离并测定。测试数据经多级校准曲线处理后涂料试样中苯系物、环己酮和TD I的加标回收率为98.6%～101.8%,各组分分析结果的变异系数均小于2.0%,检出限均小于1.50×10^-5g。     

Distribution of Cd,Ck, Pb and Zn in Soil and Vegetation Compartments in Stands of Five Boreal Tree Species in N.E. Sweden

Concentrations and total quantity of cadmium (Cd), cupper (Cu),lead (Pb) and zink (Zn) were determined in biomass and soil compartments in a replicated tree species experiment with 27-yr-old stands growing on former farmland in N.E. Sweden. Sequentialextractions of soil samples were performed in order to estimate the exchangeable and an organically bound fraction of each element. The tree species included were Picea abies (L.)H. Karst., Pinus sylvestris L., Pinus contorta Dougl., Larix sibirica Ledeb., and Betula pendula Roth.Tree species influenced the rate of removal of Cu, Pb and Zn incase of stemwood harvesting, and of Cd, Cu and Zn in the case ofwhole-tree harvesting. B. pendula and P. abies had higher quantities and average concentrations of Zn in the biomass. For all species, >50% of the Zn in the stems was found in the bark. P. abies and L. sibirica had higher quantities of Cu in the biomass than the other species.P. abies and P. contorta had high quantities of Cd inthe biomass in relation to the other species. Branches and stembark contained high concentrations of Cd and Pb in relation to foliage and stemwood. Dead branches had especially high concentrations of Pb. The high accumulation rate of Zn in thebiomass of B. pendula was related to a low exchangeable amount of Zn in the A horizon. In the superficial centimeters ofthe A horizon, a depletion similar to that found for Zn was detected for Cu, whereas for Cd and Pb, no correlations were found between quantities of elements in the trees and element pools in the soil.     

Programs assessing implementation and effectiveness of state forest practice rules and BMPs in the West

The major forest nonpoint source control programs in the West are largely regulatory, either under forest practices acts (California, Idaho, New Mexico, Nevada, Oregon, and Washington) or a streamside management act (Montana). These programs and the specific rules they enforce continue to undergo intensive scrutiny. Still, the questions are the same for these regulatory programs as for states that base nonpoint source control on voluntary BMPs (Arizona, Colorado, Utah, Wyoming). Are the rules or BMPs being applied, and are they effective in reducing nonpoint source pollution to levels that protect beneficial uses of water? The level of debate about forestry in the West has resulted in detailed monitoring and research to answer these questions. In the past, state agencies have assumed levels of BMP compliance based on the percent of operations without enforcement actions. These estimates are being replaced by statistically valid and reproducible monitoring of forest practices rules and BMP compliance levels. BMP effectiveness is being assessed using both qualitative and quantitative methods. This can involve field assessments, process-based research, and control watershed studies. Some trend monitoring is also beginning. With the regional implementation rate for forestry BMPs at about 94% and rising, it is likely that effectiveness testing will continue to be a priority and consume the majority of assessment resources for this region.     

Starch-plastic materials—Preparation,physical properties,and biodegradability (a review of recent USDA research)

Recent starch-plastic research at the National Center for Agricultural Utilization Research is reviewed and related worldwide efforts are noted. Properties of starch that influence its formulation and performance in plastics are discussed. Methods are given for preparation of starch-poly(methyl acrylate) graft copolymer, starch-poly(ethylene-co-acrylic acid), and starch-poly(ethylene-co-acrylic acid)-polyethylene plastics. Their physical properties are discussed, as is degradability by enzymes or amylolytic organisms from soil, ponds, and streams.The mention of firm names or trade products does not imply that they are endorsed or recommended by the U.S. Department of Agriculture over other firms or similar products not mentioned.     

四氮唑废水处理工艺设计

高浓度、高盐分的四氮唑生产废水通过三效蒸发浓缩，馏出液经铁炭氧微电解和混凝预处理，再采用水解酸化一接触氧化一反应二沉主体组合工艺进行处理。研究了该工艺所需构筑物和设备的设计与选型。该工艺在正常运行条件下，处理后出水pH6～9，COD 302mg／L，BOD5 108mg／L，SS30mg／L，色度36倍，水质达到GB8978--1996（污水综合排放标准》三级标准。     

Application of Cellulose Microfibrils in Polymer Nanocomposites

Cellulose microfibrils obtained by the acid hydrolysis of cellulose fibers were added at low concentrations (2–10% w/w) to polymer gels and films as reinforcing agents. Significant changes in mechanical properties, especially maximum load and tensile strength, were obtained for fibrils derived from several cellulosic sources, including cotton, softwood, and bacterial cellulose. For extruded starch plastics, the addition of cotton-derived microfibrils at 10.3% (w/w) concentration increased Young’s modulus by 5-fold relative to a control sample with no cellulose reinforcement. Preliminary data suggests that shear alignment significantly improves tensile strength. Addition of microfibrils does not always change mechanical properties in a predictable direction. Whereas tensile strength and modulus were shown to increase during addition of microfibrils to an extruded starch thermoplastic and a cast latex film, these parameters decreased when microfibrils were added to a starch–pectin blend, implying that complex interactions are involved in the application of these reinforcing agents.     

Hysteresis in Reversal of Central European Mountain Lakes from Atmospheric Acidification

Extremely high emissions of S and N compounds in Central Europe (both 280 mmol m^-2 yr^-1) declined by 70and 35%, respectively, during the last decade. Decreaseddeposition rates of SO₄ ^-2, NO₃ ^-, and NH₄ ⁺ in the region paralleled emission declines. The reduction in atmospheric inputs of S and N to mountain ecosystemshas resulted in a pronounced reversal of acidification in the Tatra Mountains and Bohemian Forest lakes. Between the 1987–1990and 1997–1999 periods, concentrations of SO₄ ^-2 and NO₃ ^- decreased (average ± standard deviation) by 22±7 and 12±7 mol L^-1, respectively, in theTatra Mountains, and by 19±7 and 15±10 mol L^-1, respectively, in the Bohemian Forest. Their decrease was compensated in part (1) by a decrease in Ca²⁺ + Mg²⁺ (17±7 mol L^-1) and H⁺ (4±6 mol L^-1), and an increase in HCO₃ ^-(10±10 mol L^-1) in the Tatra Mountains lakes, and (2) by a decrease in Al (7±4 mol L^-1), Ca²⁺ + Mg²⁺ (9±6 mol L^-1), and H⁺ (6±5 mol L^-1), in Bohemian Forest lakes. Despite the rapid decline in lake water concentrations of SO₄ ^-2 and NO₃ ^- in response to reduced S and N emissions, their present concentrations in some lakes are higher than predictionsbased on observed concentrations at comparable emission rates during development of acidification. This hysteresis in chemical reversal from acidification has delayed biological recovery of the lakes. The only unequivocal sign of biological recovery hasbeen observed in erné Lake (Bohemian Forest) where a cladoceran species Ceriodaphnia quadrangular has recentlyreached its pre-acidification abundance.     

Reconstruction of Long-Term Changes in Lake water Chemistry,Zooplankton and Benthos of a Small,Acidified High-Mountain Lake: Magic Modelling and Palaeolimnogical Analysis

Starolesnianske pleso is a small and shallow acid lake in the High Tatra Mountains, situated at 2000 m above sea level, on granitic bedrock, with sparse and thin soil cover. When detailed measurements began in the 1980s Starolesnianske pleso had pH below 5 and only one species of cladoceran zooplankton, the ubiquitous Chydorus sphaericusPalaeolimnological investigations show changes in cladoceran zooplankton and chironomid zoobenthic assemblages since about 1920 and a major change in 1970–1980. The dynamic acidification model MAGIC was used to reconstruct changes in water chemistry over the past 150 years. The results from MAGIC agree well with the sediment record; pH levels gradually decreased from 6.5 in the mid-1800s to about 5.6 in 1920 (first response in biota) to below 5.0 by 1970, and concentrations of inorganic aluminium rose dramatically beginning about 1960. In the 1990s the lake water chemistry showed clear signs of reversal in acidification brought about by a major decline in S deposition.     

Bioassessment of silvicultural impacts in streams and wetlands of the Eastern United States

Bioassessment is a useful tool to determine the impact of logging practices on the biological integrity of streams and wetlands. Measuring biota directly has an intuitive appeal for impact assessment, and biota can be superior indicators to physical or chemical characteristics because they can reflect cumulative impacts over time. Logging can affect stream and wetland biota by increasing sedimentation rates, altering hydrologic, thermal, and chemical regimes, and changing the base of food webs. Biotic impacts of logging on streams compared to wetlands probably differ, and in this paper we review some of those differences. In streams, invertebrates, fishes, amphibians, algae, and macrophytes have been used as indicators of logging impacts. In wetlands, bioassessment is just beginning to be used, and plants and birds are the most promising indicator taxa. Various best management practices (BMPs) have been developed to reduce the impacts of logging on stream and wetland biota, and we review quantitative studies that have evaluated the efficacy of some of these techniques in streams and wetlands in the eastern United States. Remarkably few studies that address the overall efficacy of BMPs in limiting biotic changes in streams and wetlands after BMP implementation have been published in scientific journals, although some work exists in reports or is unpublished. We review these works, and compile conclusions about BMP efficacy for biota from this body of research.     

Characterization of air emissions and residual ash from open burning of electronic wastes during simulated rudimentary recycling operations

Air emissions and residual ash samples were collected and analyzed during experiments of open, uncontrolled combustion of electronic waste (e-waste), simulating practices associated with rudimentary e-waste recycling operations. Circuit boards and insulated wires were handled separately to simulate processes associated with metal recovery. The average emissions of polychlorinated dibenzodioxins and dibenzofurans (PCDD/PCDFs) were 92 ng toxic equivalency (TEQ)/kg [n = 2, relative standard deviation (RSD) = 98%] and 11 900 ng TEQ/kg (n = 3, RSD = 50%) of the initial mass of the circuit boards and insulated wire, respectively. The value for the insulated wire is about 100 times higher than that for backyard barrel burning of domestic waste. The emission concentrations of polybrominated dibenzodioxins and dibenzofurans (PBDD/PBDFs) from the combustion of circuit boards were 100 times higher than for their polychlorinated counterparts. Particulate matter (PM) sampling of the fly ash emissions indicated PM emission factors of approximately 15 and 17 g/kg of the initial mass for the circuit boards and insulated wire, respectively. Fly ash samples from both types of e-waste contained considerable amounts of several metallic elements and halogens; lead concentrations were more than 200 times the United States regulatory limits for municipal waste combustors and 20 times those for secondary lead smelters. Leaching tests of the residual bottom ash showed that lead concentrations exceeded U.S. Environmental Protection Agency landfill limits, designating this ash as a hazardous waste.     

Does Soil Acidification Affect Spruce Needle Chemical Composition and Tree Growth?

In 1994, a large survey of soil chemistry was undertaken in thecounty of Värmland in central Sweden (Lundström et al., 1998).The southern part of the county was affected by soilacidification whereas there were no such indications in thenorthern part. To investigate the influence of soil chemistryon the trees at the specific sites, the survey was continued byan analysis of needle chemistry (Norway spruce) which wasundertaken at 150 of the 180 sites, and of tree growth at 65 ofthe 180 sites. Growth was expressed as a ratio between expectedgrowth, estimated with a national, empirical growth model, andthe growth observed in the field. In statistical analyses,using rank correlation, PCA and PLS, there were only weakindications of an influence of soil chemistry on needlechemistry and on tree growth. A moderate correlation betweennitrogen and sulphur in needles was found, which wasinterpreted as an effect of deposition and of processes in thetree canopy. No obvious regional pattern of the growth ratiowas found, in contrast to the clear pattern of soilacidification. The statistical analysis could not with anycertainty point out any of the soil chemistry variables asespecially important for the tree growth ratio.