Determination of some selected polycyclic aromatic hydrocarbons in environmental samples by high-performance liquid chromatography with fluorescence detection

Summary Analytical methods for the determination in environmental samples, of some selected Polycyclic Aromatic Hydrocarbons (PAH's), which are included on the EPA Priority Pollutant list, have been developed and evaluated. The methodology involves the extraction of PAH's from water samples by solvent extraction with dichloromethane. Solid samples were ultrasonically extracted with acetone/hexane and the extract was cleaned up on a silica gel/alumina column. The concentrated and cleaned up extracts were analysed by HPLC on a polymeric C₁₈ column using a gradient of acetonitrile/water as the mobile phase and fluorescence detection. Typical detection limits lie in the range of 1–30 ng ml^–1 of the analytes, but after sample pretreatment detection limits of 10–300 ng l^–1 were obtained. The extraction, clean-up and HPLC methodology was applied to the determination of selected PAH's in coal washings samples and the method was validated by the quantification of PAH's in a natural contaminated and a spiked sediment.     

吹扫捕集-气相色谱分析海水和沉积物中的苯、甲苯、乙苯及二甲苯

单环芳烃苯、甲苯、乙苯和二甲苯（简称BTEX）是石油的重要组分，也是环境中需要重点监测的致癌污染物。本实验建立了动态顶空（吹扫捕集）和光离子化检测器的气相色谱测量海水、沉积物中痕量BTEX的方法。在120—1200ng／L的浓度范围，苯、甲苯、乙苯、间对二甲苯及邻二甲苯标准溶液的检出限分别为6．4、35．2、15．8、12．3、10．7ng／L，相对标准偏差0．9％-6．1％。样品无需预处理，海水中BTEX回收率为93．50％-98．40％。7个渤海表层海水样品中BTEX的浓度均低于140ng／L；海底沉积物中苯、甲苯、乙苯、间对二甲苯及邻二甲苯浓度分别为169—1243、531—1732、1308—5624、237—1136、510—5194ng／L。测量方法和结果对评价环境污染具有重要意义。     

Trace Element Speciation in Soils and Sediments Using Sequential Chemical Extraction Methods

Abstract

Several commonly used sequential chemical extraction procedures of heavy metals in soils and sediments are compared, and their advantages and disadvantages are discussed focusing on selected case studies. In particular, problems caused by handling of anoxic samples, and of specific phases (e.g. organic fractions and sulfides) are addressed.

Eventually, recommendations for the improvement of extraction selectivity as well as the reduction of readsorption effects are given.     

关于颗粒悬浮机理和悬浮动的讨论

从分析气体分子的悬浮和静水中Ｂｒｏｗｎ微粒的悬浮之机理出发，论述了重力场中粒子（分子、微粒等）的悬浮不一定需要其它外力，粒子本身的任何形式的无规则运动，达到一定强度后都能使粒子弥散悬浮．河流中的泥沙颗粒和气（水）力输送管道中的颗粒的悬浮也主要靠颗粒物的无规则运动．作用于颗粒的升力和其它力可改变颗粒悬浮沿高度的分布，但仅用这些力（若无任何无规则运动）无法解释颗粒的弥散悬浮状态．讨论了颗粒对流动阻力的双重作用：支持颗粒悬浮的湍流脉动因引入颗粒而削弱，这是颗粒的减阻作用；颗粒增阻的一个主要机制是，流体给予颗粒的水平动量在颗粒一壁面碰撞中不断地损失．用悬浮动概念解释颗粒引起的增阻是不正确的．     

Metals in water and surface sediments from Henan reaches of the Yellow River,China

The concentrations of Cd,Cr,Cu,Ni,Pb and Zn were determined in the water and surface sediments from the Henan reaches of the Yellow River.Twenty-three sampling sites along the Yellow River and its tributaries were selected.Generally,metal concentrations were found to decrease in sequences of Zn>Cu>Pb>Cr>Ni>Cd in water and Zn>Cr>Pb>Ni>Cu>Cd in sediments.High levels of metal concentration were determined at a few stations of the river and its tributaries,such as Yiluo River,Si River and Qin River.The pollutio...     

Study of matrix effects and spectral interferences in the determination of lead in sediments, sludges and soils by SR-ETAAS using slurry sampling

An interference-free, fast, and simple method is proposed for Pb determination in environmental solid samples combining slurry sampling and electrothermal atomic absorption spectrometry. Samples were ground to an adequate particle size and slurries were prepared by weighing from 0.05 g to 0.20 g of dry sediment, adding nitric acid, and a solution containing 0.1% Triton X-100. Ultrasonic agitation was employed for slurries homogenization. Analytical variables including acid pre-treatment conditions, particle size, slurry stability, temperature program of the graphite furnace, and type and concentration of the chemical modifier were studied. The undesirable effects of potential non-specific and spectral interferences on Pb signal were also taken into account. Continuum source and self-reversal methods for background correction were evaluated and compared. For calibration, synthetic acid solutions of Pb were employed. Calibration was linear within the range 1-30 μg L⁻¹ and 5-30 μg L⁻¹ when the 217.0 nm and 283.3 nm analytical lines were used. Correlation coefficients of 0.9992 and 0.9997 were obtained. Using optimized conditions, limits of detection (3σ) of 0.025 μg g⁻¹ and 0.1 μg g⁻¹ were achieved for the 217.0 nm and 283.3 nm analytical lines, respectively. The method was successfully applied to the determination of lead in soil, contaminated soil, municipal sludge, and sediment samples. The accuracy was assessed by the analysis of two certified reference materials: municipal sludge (QC MUNICIPAL SLUDGE A) and lake sediment (TRAP-LRM from IJS).     

An improved model for predicting hydrate phase equilibrium in marine sediment environment

Based on the models of hydrate phase equilibrium in bulk water and porous media, an improved model was proposed to predict the methane hydrate equilibrium in marine sediment environment. In the suggested model, mechanical equilibrium of force between the interfaces in hydrate-liquid-vapor system was considered. When electrolyte was present in pore water, interfacial energy between hydrate and liquid was corrected by an equation that is expressed as the function of temperature and electrolyte concentration. The activity of water is calculated based on the Pitzer model and the interfacial energy between liquid and gas is solved using the Li method. The prediction results show good agreement with the experimental data. By comparison with other models, it is proved that this model can improve the accuracy for predicting hydrate phase equilibrium in marine sediment environment.     

海河底泥中12种抗生素残留的液相色谱串联质谱同时检测

建立了同时检测河流底泥中12种抗生素(4种磺胺类、3种喹诺酮类、2种四环素类、2种大环内酯类、甲氧苄啶)残留的高效液相色谱串联质谱检测方法(HPLC-MS/MS)。样品提取过程中以NaF为离子交换剂,经2种提取液逐次提取,合并提取液,正己烷脱脂,萃取物经SAX-HLB固相萃取系统净化浓缩,氮吹,定容。以乙腈和0.3%甲酸为流动相,采用梯度洗脱进行液相色谱分离,以Simatone为内标物,用质谱检测器进行定性和定量分析。12种目标物的检出限为1.0~5.0 ng/g,回收率为65%~91%,相对标准偏差为0.6%~5.1%(n=4)。     

氢化物发生-原子荧光光谱法测定海洋沉积物中砷、锑、铋、汞、硒

提出了用盐酸-硝酸-水(3+1+4)混合酸消解样品,氢化物发生-原子荧光光谱法测定海洋沉积物样品中砷、锑、铋、汞、硒的方法。考察了原子荧光光谱仪的最佳工作条件。在最佳条件下砷、锑、铋、硒的检出限(3s/k)分别为0.018,0.004,0.001,0.003μg.g-1,汞的检出限(3s/k)为0.604ng.g-1。应用于3种海洋沉积物标准物质的测定,测定值与标准值吻合。     

The Influence of the Air-Drying Pretreatment of Sediment Samples for Metallic Element Mobilities

Chemical analysis of sediments provides an efficient tool for water quality management. Ten sediment samples collected in 2008 from two locations situated in the Danube Delta Biosphere were analyzed in a comparative study of mobile metallic elements via two different pre-treatment techniques: air-drying followed by sieving and wet sieving. The experimental data proved that air-drying procedure produces drastic changes in mobility of the metallic elements from the sediments which were studied as an effect of the oxidizing conditions. Wet sediment or oxygen-free dried sediment is recommended to be used in environmental studies regarding determination of mobile fractions from sediment samples.