Fast sample preparation involving MASE and coupled column normal phase liquid chromatography for the rapid trace analysis of dioxins in air-dust samples from fire catastrophe emissions

A new approach has been developed and tested for the urgent analysis of dioxins in samples of air-dust filters originating from catastrophe emissions. The procedure consists of a fast extraction of the sample with microwave solvent extraction (MASE) and acetone as solvent followed by a fast cleanup of the extract with normal phase coupled column liquid chromatography (LC/LC).

The multi-dimensional LC/LC system employs a 50 mm×4.6 mm i.d. column packed with 3 μm silica and a 150 mm×4.6 mm i.d. column packed with 5 μm PYE as the first and second analytical column, respectively. Iso-hexane is used on both columns to perform cleanup and dichloromethane to perform efficient back-flush elution of the compounds from the second column. The obtained polarity-based separation in the first dimension and molecular-structure based separation in the second dimension provides a fast and powerful cleanup.

Validation was done by analysing samples of homemade RIVM air-dust with aged residues (n=8, spiking level about 15 pg mg⁻¹ per compound) of dioxins/furans and samples of reference Urban Dust SRM 1649a (n=4) with both the new approach and the existing conventional procedure and were instrumentally analyzed with capillary gas chromatography and high resolution mass spectrometric detection (GC/HRMS).

In comparison to the existing conventional procedure, the new approach reduces sample processing from several days to several hours per sample.

As regards the aged-residue air-dust samples, the new method shows a good accuracy, precision and high selectivity providing a performance in good agreement with the existing procedure. In SRM air-dust, the concentration of a few compounds obtained by the new method was below (10–50%) the certified value.     

Anomalous scaling in epitaxial growth on vicinal surfaces: meandering and mounding instabilities in a linear growth equation with spatiotemporally correlated noise

We have undertaken an extensive analytical and kinetic Monte Carlo study of the (2+1) dimensional discrete growth model on a vicinal surface. A non-local, phenomenological continuum equation describing surface growth in unstable systems with anomalous scaling is presented. The roughness produced by unstable growth is first studied considering various effects in surface diffusion processes (corresponding to temperature, flux, diffusion anisotropy). We found that the thermally activated roughness is well-described by a generalized Lai–Das Sarma–Villain model with non linear growth continuum equation and uncorrelated noise. The corresponding critical exponents are computed analytically for the first time and show a continuous variation in agreement with simulation results of a solid-on-solid model. However, the roughness related to the meandering instability is found, unexpectedly, to be well described by a linear continuum equation with spatiotemporally correlated noise.     

高效液相色谱法测定水体中的氯虫酰胺残留量

采用Kromasil C18不锈钢柱(250mm×4.6mm i.d..5μm),以甲醇-水混合溶剂(65:35,V/V)为流动相,流速1.0mL/min,光电二极管阵列检测器,检测波长236nm和柱温35C,建立了不同水体中氯虫酰胺残留的高效液相色谱分析方法.氯虫酰胺水样直接用二氯甲烷进行液-液分配萃取.在0.10-10mg/L的浓度范围内,氯虫酰胺峰面积(y)与质量浓度(x)呈现良好的相关性,其线性回归方程为y=2170.4x 2641.7,r2=0.9991.井水和池塘水中添加质量浓度为0.01-1.00mg/L时,其平均回收率分别为94.70%-100.37%和89.14%-100.22%,变异系数分别为0.81%-5.11%和1.81%-5.30%,水样中的氯虫酰胺最低检测质量浓度(LOQ)为7.5×10-3mg/L,方法快速、灵敏度高、重现性好,具有较好的准确度和精密度,可用于环境中水样和土壤样中氯虫酰胺的残留检测分析.     

Comparison of various extraction techniques for the determination of polycyclic aromatic hydrocarbons in worms

Two less laborious extraction methods, viz. (i) a simplified liquid extraction using light petroleum or (ii) microwave-assisted solvent extraction (MASE), for the analysis of polycyclic aromatic hydrocarbons (PAHs) in samples of the compost worm Eisenia andrei, were compared with a reference method. After extraction and concentration, analytical methodology consisted of a cleanup of (part) of the extract with high-performance gel permeation chromatography (HPGPC) and instrumental analysis of 15 PAHs with reversed-phase liquid chromatography with fluorescence detection (RPLC-FLD). Comparison of the methods was done by analysing samples with incurred residues (n=15, each method) originating from an experiment in which worms were exposed to a soil contaminated with PAHs. Simultaneously, the performance of the total lipid determination of each method was established. Evaluation of the data by means of principal component analysis (PCA) and analysis of variance (ANOVA) revealed that the performance of the light petroleum method for both the extraction of PAHs (concentration range 1-30 ng/g) and lipid content corresponds very well with the reference method. Compared to the reference method, the MASE method yielded somewhat lower concentrations for the less volatile PAHs, e.g., dibenzo[ah]anthracene and benzo[ghi]perylene and provided a significant higher amount of co-extracted material.     

Markoff triples and quasifuchsian groups

We study the global behaviour of trees of Markoff triples overthe complex numbers. We relate this to the space of type-preservingrepresentations of the punctured torus group into SL(2,C). Inparticular, we explore which Markoff triples correspond to quasifuchsianrepresentations. We derive a variation of McShane's identityfor quasifuchsian groups. In the case of non-discrete representations,we attempt to relate the asymptotic behaviour of Markoff triplesto the realisability of laminations in hyperbolic 3-space. Wealso consider how some of these issues might be related formore general surfaces. 1991 Mathematics Subject Classification:57M50.