火焰原子吸收光度法测定水中铝的方法改进

研究了在盐酸介质中，壬基酚聚氧乙烯-7醚（NP-7）活化下，火焰原子吸收光度法测定环境水体中铝的方法改进。在25mL容量瓶中，加入5．0mL体积分数为50％的盐酸、2．0mL质量浓度为0．01g／mL NP-7和4．0mL质量浓度为75．0μg/mL的铝标准溶液，在原子吸收分光光度计的最佳测定条件下测定吸光度。根据吸光度与铝质量浓度绘制了工作曲线，线性范围3．0～24．0μg/mL，检出限1．32μg/mL。该法用于环境水体中铝含量的测定，加标回收率为94．4％～101．4％，最大相对标准偏差5．8％，方法对比最大相对误差4．1％。     

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%。     

液相色谱-质谱法测定水中氨基甲酸酯类农药及其代谢物

建立了直接测定水中10种氨基甲酸酯类农药及其代谢物的超高效液相色谱-质谱分析方法。该方法对水样无需进行富集处理,水样过滤后就可以直接测定。实验结果表明:测定液中各氨基甲酸酯类农药及其代谢物的质量浓度与离子对峰面积在质量浓度0.5～1 000.0μg/L内具有良好的线性关系;方法检出限为0.1～5.0μg/L;加标回收率91%～103%;相对标准偏差为2%～5%。该方法具有简便快捷、灵敏度高的特点。     

氢化物发生-原子荧光法同时测定污水中的砷和硒

用HNO3-HClO4消解液消解水样,断续流动进样,在KBH4-酸体系中,采用氢化物发生-原子荧光法同时测定污水中的砷和硒。在含浓盐酸2．0mL的介质中加入硫脲-抗坏血酸溶液5mL,在温度高于15℃时放置30min后,以15g/L KBH4溶液为还原剂,5％(体积分数)HCl为载流测定砷、硒荧光强度。在最佳实验条件下,砷、硒的相对标准偏差分别小于4％和2％,检出限分别为0．89μg／L和0．51μg／L,加标回收率分别为91．5％～101．2％和94．0％～100．5％。该方法精密度高、测定结果稳定,达到环境监测要求。     

浊点萃取分光光度法测定水中Cr(Ⅵ)

利用二苯碳酰二肼显色,Triton X-100-正辛醇浊点萃取,建立了一种分光光度法测定水中Cr(Ⅵ)的新方法,并探讨了不同测定条件对测定效果的影响。优化后的测定条件为(总体积50 mL)1 mol/L稀硫酸加入量1.0mL、2 g/L二苯碳酰二肼溶液加入量1.5 mL、10 g/L Triton X-100溶液加入量1.5 mL、3 g/L苯甲酸溶液加入量4.0mL、正辛醇加入量5.0 mL。Cr(Ⅵ)质量浓度在0~20μg/L范围内符合朗伯-比尔定律,线性回归方程的相关系数为0.995 5。该方法应用于水样中痕量Cr(Ⅵ)的测定,相对标准偏差小于2.5%,加标回收率为95.7%。     

液相色谱法测定空气中17种醛酮类化合物

建立了一种用于测定空气中17种醛酮类化合物的高效液相色谱--二极管阵列检测(HPLC-PDA)分析方法.该法以2,4-二硝基苯肼(DNPH)的盐酸溶液作为吸收液,将醛酮类化合物转化为醛酮-DNPH衍生物,以醛酮-DNPH的特征吸收波长和色谱峰保留时间进行定性分析,并采用工作曲线法同时进行定量测定.色谱测定液中各醛酮类化合物的质量浓度在0.05～2.00μg/mL的范围内与色谱峰面积呈现很好的线性关系,相关系数均大于0.999 0,方法的平均回收率为91.5%～98.9%,相对标准偏差为3.6%～9.4%,检出限为2～10μg/m3,可用于化工装置尾气及环境空气中醛酮类有机污染物的检测.     

溴甲酚紫-十六烷基二甲基苄基溴化铵法测定废水中阴离子表面活性剂含量

采用溴甲酚紫-十六烷基二甲基苄基溴化铵法测定洗涤剂工业的生产废水或生活污水中阴离子表面活性剂的含量。实验表明:适合的溶液pH为8,测定波长λmax为588nm,在十六烷基二甲基苄基溴离子质量浓度为15.0mg/mL的条件下,十二烷基苯磺酸钠质量浓度在0—50μg/mL范围内符合比耳定律,其摩尔吸光系数为3.48×104L/(mol·cm),该方法的相对标准偏差小于4%,试样加标平均回收率为96%-102%。该法可用于测定工业废水、河流等环境水样中的阴离子表面活性剂含量。     

铬(Ⅵ)-溴酸钾-乙基紫催化光度法测定水中痕量铬(Ⅵ)

在磷酸介质中,利用铬(Ⅵ)对溴酸钾氧化乙基紫褪色反应有灵敏的催化作用,建立了测定痕量铬(Ⅵ)的新型催化光度法,考察了该褪色反应的最佳条件。在反应温度85℃、反应时间5m in、以醋酸钠作抑制剂的条件下,体系可稳定60m in以上,测定波长为600nm,方法的检出限为1×10-9g/mL,线性范围为0.004~0.094μg/mL,相对标准偏差小于2.5%,加标回收率为97.0%~101.5%。该法简便、灵敏、选择性好,用于水样中痕量铬(Ⅵ)的测定,结果令人满意。     

催化动力学光度法测定水中痕量亚硝酸根

根据盐酸介质中亚硝酸根对甲基红的溴酸钾氧化反应的催化作用,建立了测定水中痕量亚硝酸根的催化动力学光度法。实验结果表明,当盐酸溶液的加入量为1.0mL、溴酸钾溶液的加入量为0.2mL、甲基红溶液的加入量为3.5mL、加热时间为5min、加热温度为50℃时,方法的检出限为1.0×10-7g/L,线性范围为5.0×10-7~1.0×10-5g/L,回收率为97.8%~103.3%,相对标准偏差为1.8%~2.6%。该法已用于废水水样中亚硝酸根的测定,结果满意。     

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％：     

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.     

Effect of Coconut, Sisal and Jute Fibers on the Properties of Starch/Gluten/Glycerol Matrix

Coconut, sisal and jute fibers were added as reinforcement materials in a biodegradable polymer matrix comprised of starch/gluten/glycerol. The content of fibers used in the composites varied from 5% to 30% by weight of the total polymers (starch and gluten). Materials were processed in a Haake torque rheometer (120 °C, 50 rpm) for 6 min. The mixtures obtained were molded by heat compression and further characterized. Addition of lignocellulosic fibers in the matrix decreased the water absorption at equilibrium. The diffusion coefficient decreased sharply around 5% fiber concentration, and further fiber additions caused only small variations. The thermogravimetric (TG) analysis revealed improved thermal stability of matrix upon addition of fibers. The Young’s modulus and ultimate tensile strength increased with fiber content in the matrix. The storage modulus increased with increasing fiber content, whereas tanδ curves decreased, confirming the reinforcing effect of the fibers. Morphology of the composites analyzed under the scanning electron microscope (SEM) exhibited good interfacial adhesion between the matrix and the added fibers. Matrix degraded rapidly in compost, and addition of increased amounts of coconut fiber in the matrix caused a slowdown the biodegradability of the matrix. Names are necessary to report factually on available data; however, the USDA neither guarantees nor warrants the standard of the product, and the use of the name by USDA implies no approval of the product to the exclusion of others that may be suitable.     

Quantification of Polymerisation Processes During The Oxidative Degradation of 14C-Labelled Chlorophenols

In experiments employing the lignocellulose-decaying basidiomycetes Trametes versicolor and Stropharia rugosoannulata degrading uniformly¹⁴C-labelled 2,4-dichlorophenol and pentachlorophenol, acombination of size exclusion chromatography (SEC),fractionation, and -scintillation counting wasapplied to quantify polymerisation products formed duringchlorophenol degradation. Time-dependent mass balances weregenerated by analysis of ¹⁴C in polymerisation products,CO₂, as well as monomer non-polar and polar metabolites.Approximately 30% of the chlorophenols were found to bepolymerised. A major fraction of the polymerised productscorresponded to a molecular weight range from 0.24 – 40 kDa.Only a minor fraction could be attributed to a molecularweight >40 kDa. This method proved to be useful inquantification of polymerisation products and kinetics of thepolymerisation processes, whereas UV/Vis detection ofpolymerisation products separated by SEC led to false positiveresults. The SEC-¹⁴C method could also be applied forother complex processes where polymerisation ordepolymerisation occurs (humification, degradation oflignocellulose, formation of bound residues from xenobioticssuch as polycyclic aromatic hydrocarbons or 2,4,6-trinitrotoluene) and where spectrophotometric determinationsare difficult or impossible.     

The Relative Influences of Primary and Secondary Particulates to Urban Air Quality in the United Kingdom

This study uses a combination of data from U.K. monitoringstations and from modelling undertaken with the U.K.Meteorological Office's NAME Model to investigate therelative influences of primary and secondary particulateson total PM₁₀ levels at sites in the United Kingdom. Co-located PM₁₀ and sulphate aerosol measurementsindicate that sulphate has a disproportionately largeinfluence on the variation of PM₁₀ levels incomparison to its contribution to their total mass.Comparisons of measured PM₁₀ at urban centre, roadsideand rural sites suggest that local primary sources havevery little influence on daily mean levels. NAME has beenused to model both primary particles and sulphate aerosolfrom sources across the whole of Europe. The discrepanciesbetween modelled and observed PM₁₀ suggest that coarseparticles, such as windblown dust and resuspended roaddust,may comprise a very large, if not dominant, proportion ofobserved PM₁₀ levels. The apparently minor role ofprimary particles (especially locally-sourced ones) raisesa number of issues regarding the suitability of current U.K.and European legislation to addressing the particle problem.     

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.     

Changes in Extractability of Cr and Pb in a Polycontaminated Soil After Bioaugmentation With Microbial Producers of Biosurfactants, Organic Acids and Siderophores

Partly because of the low bioavailability of metals, the soil cleaning-up using phytoremediation is usually time-consuming. In order to enhance the amount of metals at the plant's disposal, the soil bioaugmentation coupled together with phytoextraction is an emerging technology. In this preliminary work, two agricultural soils which mainly differed in their Cr, Hg and Pb contents (LC, low-contaminated soil; HC, high-contaminated soil) were bioaugmented in laboratory conditions by either bacterial (Bacillus subtilis, Pseudomonas aeruginosa, Pseudomonas fluorescens or Ralstonia metallidurans) or fungal inocula (Aspergillus niger or Penicillium simplicissimum) and incubated during three weeks. The LC soil pots bioaugmented with A. niger and P. aeruginosa contained higher concentrations of Cr (0.08 and 0.25 mg.kg⁻¹ dw soil) and Pb (0.25 and 0.3 mg.kg⁻¹ dw soil) in the exchangeable fraction F1 (extraction with MgCl₂) by comparison with the non-bioaugmented soil where neither Cr nor Pb was detected. Conversely, immobilization of Cr and Pb in the soil were observed with the other microorganisms. The soil bioaugmentation not only modified the metal speciation for the most easily extractable fractions but also modified the distribution of metals in the other fractions, to a lesser extent nevertheless. The difference in microbial concentrations between the bioaugmented or not HC soils reached up to 1.8 log units. Thus the microorganisms that we chose for the soil bioaugmentation were competitive towards the indigenous microflora. The PCA analysis showed close positive relationships between the microorganisms which potentially produced siderophores in the soil and the amount of Cr and Pb in the fraction F1.     

Heavy Metals Removal by Biosorption and Flotation

The removal of a mixture of heavy (toxic) metal cations (copper, nickeland zinc) from liquid effluents was investigated in this study at pilotscale, using counter-current contact mode. The innovative processinvolved the abstraction of metal ions onto fungal biosorbents, followedby the application of flotation for the subsequent solid/liquid separationof biomass particles. The ability of microorganisms to remove metal ionsfrom aqueous solutions is a well-known phenomenon. Nevertheless,engineering considerations are very important in decisions, concerningthe commercial future of biosorption and practical solutions are neededfor certain problems, such as the efficient post-separation ofmetal-loaded biomass. The two processes (flotation and biosorption) caneffectively operate in combination, in what it was termed biosorptiveflotation process. The sorbents may be recycled, after appropriate elutionof metals, as well as the treated (clean) water.     

酸浸出法回收冶金污泥中的有价金属

采用二次酸浸出的方法回收镍钴湿法冶金工业污泥中的有价金属。先采用水和硫酸作为浸出剂浸出Mg和Na,最佳工艺条件为浸出液的pH 7.5、浸出时间5 min、浸出剂体积与干污泥质量的比(ω)为10 mL/g。再采用硫酸作为浸出剂、焦亚硫酸钠作为还原剂进行二次酸浸,在硫酸与污泥质量比为1.3、焦亚硫酸钠与污泥质量比为0.3、ω为5 mL/g、浸出温度85℃、浸出时间20 min的最佳工艺条件下,Co、Ni、Cu、Mn和Zn的浸出率分别达92.45%、93.48%、89.52%、97.78%和94.79%。经XRD表征,浸出后污泥中未见原污泥中的矿物相,说明原污泥中的矿物几乎全部被溶解。     

不同原料生物炭对NH4+-N、PO43--P吸附性能的差异性及其成因分析

以芦苇、小麦秸秆和竹子为原料,利用回流式炭化工艺制备3种生物炭。比较三者对NH_4~+-N、PO_4~(3-)-P的吸附性能,并对三者吸附性能差异的成因进行分析。实验结果表明:3种生物炭对PO_4~(3-)-P的吸附效果整体上优于NH_4~+-N,因为3种生物炭的阳离子交换容量CEC值和Zeta电位绝对值的水平均较低,不利于阳离子的吸附;竹炭Z-C对NH_4~+-N的吸附效果最佳,6 h去除率为3.59%,低的N含量、pH及Zeta电位绝对值对NH_4~+-N的吸附有利;芦苇炭LW-C中的O更多地与K、Mg等结合,形成能够与PO_4~(3-)反应生成磷酸盐沉淀或者晶体物质的金属氧化物,从而具有最好的PO_4~(3-)-P的吸附效果,6 h时去除率达16.91%。