A cost effective,sensitive, and environmentally friendly sample preparation method for determination of polycyclic aromatic hydrocarbons in solid samples

A simple, cost effective, and yet sensitive sample preparation technique was investigated for determining Polycyclic Aromatic Hydrocarbons (PAHs) in solid samples. The method comprises ultrasonic extraction, Stir Bar Sorptive Extraction (SBSE), and thermal desorption–gas chromatography–mass spectrometry to increase analytical capacity in laboratories. This method required no clean-up, satisfied PAHs recovery, and significantly advances cost performance over conventional extraction methods, such as Soxhlet and Microwave Assisted Extraction (MAE). This study evaluated three operational parameters for ultrasonic extraction: solvent composition, extraction time, and sample load. A standard material, SRM 1649 a (urban dust), was used as the solid sample matrix, and 12 priority PAHs on the US Environmental Protection Agency (US EPA) list were analyzed. Combination of non-polar and polar solvents ameliorated extraction efficiency. Acetone/hexane mixtures of 2:3 and 1:1 (v/v) gave the most satisfactory results: recoveries ranged from 63.3% to 122%. Single composition solvents (methanol, hexane, and dichloromethane) showed fewer recoveries. Comparing 20 min with 60 min sonication, longer sonication diminished extraction efficiencies in general. Furthermore, sample load became a critical factor in certain solvent systems, particularly MeOH. MAE was also compared to the ultrasonic extraction, and results determined that the 20-min ultrasonic extraction using acetone/hexane (2:3, v/v) was as potent as MAE. The SBSE method using 20 mL of 30% alcohol-fortified solution rendered a limit of detection ranging from 1.7 to 32 ng L⁻¹ and a limit of quantitation ranging from 5.8 to 110 ng L⁻¹ for the 16 US EPA PAHs.     

Testing Aluminum Alloy from Quasi-static to Dynamic Strain-rates with a Modified Split Hopkinson Bar Method

An aluminum alloy¹ was tested at quasi-static to dynamic strain-rates (from 10⁻¹ to 5 10³ s⁻¹), using a single measuring device, a modified Split Hopkinson Bar. A wave separation technique [Bussac et al., J Mech Phys Solids 50:321–350, 2002] based on the maximum likelihood method was applied to process the strain and velocity measurements recorded at various points on each bar. With this method, it is possible to compute the stress, strain, displacement and velocity at any point on the bar. Since the measurement time is unlimited, the maximum strain measured in a given specimen no longer decreases with the strain-rate, as occurs with the classical Split Hopkinson Bar method. ¹The authors wish to thank the automobile manufacturer who provided samples of the alloy used in this study. For reasons of commercial and industrial confidentiality, we were not informed about the composition of this alloy.     

Powdered activated carbons as effective phases for bar adsorptive micro-extraction (BAμE) to monitor levels of triazinic herbicides in environmental water matrices

Bar adsorptive micro-extraction using three powdered activated carbons (ACs) as adsorbent phases followed by liquid desorption and high performance liquid chromatography with diode array detection (BAμE(ACs)-LD/HPLC-DAD), was developed to monitor triazinic herbicides (atrazine, simazine and terbutylazine) in environmental water matrices. ACs used present apparent surface areas around 1000 m² g⁻¹ with an important mesoporous volume and distinct surface chemistry characteristics (pH_PZC ranging from 6.5 to 10.4). The textural and surface chemistry properties of the ACs adsorbent phases were correlated with the analytical data for a better understanding of the overall enrichment process. Assays performed on 10 mL water samples spiked at the 10.0 μg L⁻¹ levels under optimized experimental conditions yielded recoveries around 100% for the three herbicides under study. The analytical performance showed good precision (RSD < 15.0%), convenient detection limits (≈0.1 μg L⁻¹) and suitable linearity (1.0-12.0 μg L⁻¹) with good correlation coefficients (r² > 0.9914). By using the standard addition method, the application of the present method on real water matrices, such as surface water and wastewater, allowed very good performances at the trace level. The proposed methodology proved to be a suitable sorptive extraction alternative for the analysis of priority pollutants with polar characteristics, showing to be easy to implement, reliable, sensitive and requiring a low sample volume to monitor triazinic compounds in water matrices.     

Cork-based activated carbons as supported adsorbent materials for trace level analysis of ibuprofen and clofibric acid in environmental and biological matrices

In this contribution, powdered activated carbons (ACs) from cork waste were supported for bar adsorptive micro-extraction (BAμE), as novel adsorbent phases for the analysis of polar compounds. By combining this approach with liquid desorption followed by high performance liquid chromatography with diode array detection (BAμE(AC)-LD/HPLC-DAD), good analytical performance was achieved using clofibric acid (CLOF) and ibuprofen (IBU) model compounds in environmental and biological matrices. Assays performed on 30 mL water samples spiked at the 25.0 μg L(-1) level yielded recoveries around 80% for CLOF and 95% for IBU, under optimized experimental conditions. The ACs textural and surface chemistry properties were correlated with the results obtained. The analytical performance showed good precision (<15%), suitable detection limits (0.24 and 0.78 μg L(-1) for CLOF and IBU, respectively) and good linear dynamic ranges (r(2)>0.9922) from 1.0 to 600.0 μg L(-1). By using the standard addition methodology, the application of the present approach to environmental water and urine matrices allowed remarkable performance at the trace level. The proposed methodology proved to be a viable alternative for acidic pharmaceuticals analysis, showing to be easy to implement, reliable, sensitive and requiring low sample volume to monitor these priority compounds in environmental and biological matrices.     

增强碳纳米管场发射性能的沟槽形冷阴极制作(英文)

基于烧结工艺和丝网印刷技术,研发了一种新的沟槽形冷阴极.底部绝缘层由黑色绝缘浆料被烧结后制成,且在底部绝缘层中存在倾斜面.将银浆丝网印刷在条形电极上,依次经烘烤和烧结工艺后形成银电极.利用细砂纸,对银电极进行适当的抛光工艺,以便获得光滑的电极表面.由于特有的银电极形状,从而易于获得更大的场增强因子.将碳纳米管制备在银电极上,形成场发射极.致密的碳纳米管层完全覆盖银电极表面,特有的边缘场增强效应能够使得碳纳米管发射出更多的电子.顶部绝缘层则用于抑制碳纳米管的横向电子发射.结合沟槽形冷阴极,制作了三极结构的场致发射显示器,该显示器具有良好的场致发射特性及优良的发光图像均匀性.与普通冷阴极场致发射显示器相比,沟槽形冷阴极场致发射显示器能够将开启电场从1.86V/μm降低到1.78V/μm,将最大场致发射电流从1 537μA增加到2 863μA,且将最大发光图像亮度从1 386cd/m2提高到1 865cd/m2.该制作技术在场致发射显示器中具有较强的实际应用性.     

Application of bar adsorptive microextraction to determine trace organic micro-pollutants in environmental water matrices

The present work proposes the application of bar adsorptive micro-extraction (BAµE) coated with an N-vinylpyrrolidone polymer (NVP) combined with micro-liquid desorption (200 µL) followed by high-performance liquid chromatography with diode array detection (BAµE(NVP)-µLD/HPLC-DAD) for the determination of trace levels of emerging organic micro-pollutants in environmental water matrices. The model compounds selected include an antibacterial/antifungal agent (triclosan), two pharmaceuticals (carbamazepine and diclofenac) and two steroid hormones (17α-ethinylestradiol and 17β-estradiol), in which the latter three were recently included in the European Union watch list of substances to be monitored in the field of water policy. Assays performed on 25 mL of ultrapure water samples spiked at the 8.0 µg L^?1 level yielded average recoveries ranging from 81.9 to 102.4% for the compounds studied using optimised experimental conditions. The proposed analytical methodology demonstrated suitable detection limits (0.02–0.10 µg L^?1) and good linear dynamic ranges (0.1–20.0 µg L^?1) with determination coefficients higher than 0.9909. Using the standard addition method (SAM), the present analytical approach was applied on environmental water matrices, including surface, sea, river and groundwaters. The proposed method proved to be a suitable and alternative sorption-based static micro-extraction technique for monitoring trace levels of organic micro-pollutants in environmental water matrices.     

Propagation of a stress wave through a virtual functionally graded foam

Stress wave propagation through a Functionally Graded Foam Material (FGFM) is analysed in this paper using the finite element method. A finite element model of the Split Hopkinson Pressure Bar (SHPB) is developed to apply realistic boundary conditions to a uniform density foam and is validated against laboratory SHPB tests. Wave propagation through virtual FGFMs with various gradient functions is then considered. The amplitude of the stress wave is found to be shaped by the gradient functions, i.e., the stress can be amplified or diminished following propagation through the FGFMs. The plastic dissipation energy in the specimens is also shaped by the gradient functions. This property of FGFMs provides significant potential for such materials to be used for cushioning structures.     

Adsorptive micro-extraction techniques--novel analytical tools for trace levels of polar solutes in aqueous media

A novel enrichment technique, adsorptive μ-extraction (AμE), is proposed for trace analysis of polar solutes in aqueous media. The preparation, stability tests and development of the analytical devices using two geometrical configurations, i.e. bar adsorptive μ-extraction (BAμE) and multi-spheres adsorptive μ-extraction (MSAμE) is fully discussed. From the several sorbent materials tested, activated carbons and polystyrene divinylbenzene phases demonstrated the best stability, robustness and to be the most suitable for analytical purposes. The application of both BAμE and MSAμE devices proved remarkable performance for the determination of trace levels of polar solutes and metabolites (e.g. pesticides, disinfection by-products, drugs of abuse and pharmaceuticals) in water matrices and biological fluids. By comparing AμE techniques with stir bar sorptive extraction based on polydimethylsiloxane phase, great effectiveness is attained overcoming the limitations of the latter enrichment approach regarding the more polar solutes. Furthermore, convenient sensitivity and selectivity is reached through AμE techniques, since the great advantage of this new analytical technology is the possibility to choose the most suitable sorbent to each particular type of application. The enrichment techniques proposed are cost-effective, easy to prepare and work-up, demonstrating robustness and to be a remarkable analytical tool for trace analysis of priority solutes in areas of recognized importance such as environment, forensic and other related life sciences.