Applicability of microwave-assisted extraction combined with LC-MS/MS in the evaluation of booster biocide levels in harbour sediments

A new sample treatment method for the determination of four common booster biocides (Diuron, TCMTB, Irgarol 1051 and Dichlofluanid) in harbour sediment samples has been developed that uses liquid chromatography-tandem mass spectrometry (LC-MS/MS) after microwave-assisted extraction, followed by clean-up and a solid phase extraction preconcentration step (MAE-SPE). The effects of different variables on MAE-SPE were studied. The recoveries obtained were greater than 75%, and the relative standard deviation was less than 7%. The detection limits ranged between 0.1 and 0.3 ng g⁻¹. The developed methodology was successfully applied to the evaluation of the presence of booster biocides in sediment samples from different harbours and marinas of Gran Canaria Island (Canary Islands, Spain).     

微波辅助萃取技术及其在环境分析中的应用

微波辅助萃取技术是近年来发展较快的一种新型萃取方法,与传统的提取方式相比,具有省时、节能、简易、高效等优点.文章介绍了微波辅助萃取技术的特点和影响因素,综述了近年来其在环境分析中的应用情况.     

碱性微波提取-ICP/MS法测定土壤中六价铬

采用碱性微波提取法处理土壤样品,用电感耦合等离子体质谱（ICP/MS）法测定试样中的六价铬,以标准物质测定相对误差的绝对值作为试验指标建立正交模型,确定碱性微波消解的提取温度95 ℃、提取时间30 min、氯化镁用量005 g、提取液体积6 mL为最佳试验条件,采用He碰撞池技术和在线内标分别消除基体带来的质谱和非质谱干扰。条件优化后,方法检出限为0.10 mg/kg,实际样品6次测定结果的RSD分别为13.0%和5.7%,加标回收率为120%和106%。将该方法用于有证标准土壤样品的测定,测定结果均在标准值范围内。     

Study of factors affecting on the extraction efficiency of polycyclic aromatic hydrocarbons from soils using open-vessel focused microwave-assisted extraction

As part of an evaluation of focused microwave-assisted extraction (FMAE) using an open-vessel system, the effects of matrix, moisture content, ageing, and solvent have been studied on the extraction efficiency of polycyclic aromatic hydrocarbons (PAHs) from spiked soils. PAHs were spiked onto three different uncontaminated air dried and originally wet soil matrices with 1- and 20-day ageing periods. Solvents used were hexane–acetone (1:1), cyclohexane–acetone (1:1) and dichloromethane. FMAE only required a small amount of solvent (20 ml) and short extraction time (10 min) in the open cell under 90 W of microwave power. The results revealed that the extraction efficiency strongly depends on the nature of soil matrix; moisture content may enhance the recoveries of PAHs for many cases; and, the influence of the type of solvent is not significant. A comparison between microwave extraction and 16-h Soxhlet extraction has been made on spiked soils. It evidenced that the microwave method under ambient pressure is a suitable alternative to Soxhlet method for the analysis of PAHs in soils. For the evaluation of the developed FMAE method, three reference materials were used. The PAHs recovered from three reference materials were in a good agreement with reference values.     

Microwave-assisted preparation of two-dimensional amphiphilic nanoplate herding surfactants for offshore oil spill treatment

Oil spills are the uncontrolled release of liquid hydrocarbon by ruptured pipelines and tanker hulls, or blowouts and leaks from offshore storage facilities and drilling rigs, either by faulty human behaviors or inevitable natural aging processes. Spills cause disastrous environmental and economic consequences, with the effects of marine habitat damage for lasting decades, necessitating a critical need for efficient oil spill mitigation and leakage treatment. In this study, we develop a two-dimensional (2D) amphiphilic nanoplate as the herding surfactant for retracting spilled oil offshore on the seawater surface with various temperature and saline concentrations. Applying 2D nanoplate herding surfactant causes areas of thin oil slick floating on water to largely shrink and form a thick bulk layer. This transformation lays the foundation for the next-step oil treatment and recovery. Microwave-assisted synthesis method was used to fabricate the surface-modified zirconium phosphate (ZrP) nanoplates as the oil herder, which has an amphiphilic characteristic, containing both hydrophilic and hydrophobic properties. The 2D nanoplate surfactants decrease the air-water surface tension to facilitate the oil herding process efficiently. Using this herding procedure, we propose a biocompatible, high herding efficiency and cost-effective 2D herding surfactant fabrication method and offer a new direction for oil treatment in the offshore process safety field.