Performance evaluation of polycyclic aromatic hydrocarbons analysis in sediment from proficiency testing with metrological reference values

This paper describes a metrological approach to evaluate the measurement capability of laboratories participating in two proficiency testing (PT) programmes involving the analysis of five polycyclic aromatic hydrocarbons (PAHs) in sediment samples. Reference values of PAHs in the programmes for performance assessment were obtained from an accurate isotope dilution gas chromatography mass spectrometry (ID-GCMS) method which was thoroughly validated and verified. Isotope dilution mass spectrometry (IDMS) technique usually has a well-defined measurement uncertainty budget and a traceability link to an International System of Units. Provision of the metrological reference values in PT enables the establishment of a technical platform to assess the actual competence of the participating laboratories in sediment PAHs analysis. Results of the PT programmes showed that about 80 % of the laboratories employed gas chromatography in their analyses and the remaining used liquid chromatography. Irrespective of the techniques being used, however, the majority of the participating laboratories were observed to underestimate values in which the mean values of the five reported PAHs were less than those of the ID-GCMS-derived reference values by 13–20 %. Only 41–44 % of the participating laboratories were able to achieve satisfactory z-scores. The present study revealed that the reinforcement of the capability for accurate measurement of PAHs in sediment samples in laboratories worldwide should be addressed.     

Effect of seed layer on the growth and the consequent gas sensing characteristics of ZnO nanorod arrays using aqueous chemical growth

The ZnO nanorod arrays are grown on the sol–gel-derived seed layer through aqueous chemical growth, and then assembled as gas sensors for detecting carbon monoxide (CO). It is found that the structural and photoluminescent properties of the ZnO nanorod arrays are different as they are grown on seed layers annealed at different temperature (300–700 °C), which is ascribed to distinct growth kinetics of nanorods on the annealed seed layer. Moreover, the correlation between the exposed surface area and the defect density of those ZnO nanorod arrays points out the intrinsic (interior) defects can dominate the green emission instead of surface defects in the present study. Furthermore, the quantities of chemisorbed oxygen on ZnO nanorod arrays can be estimated through XPS analysis. Consequently, the influence of intrinsic defects and chemisorbed oxygen on the electrical properties and gas sensitivities of ZnO nanorod arrays has been clearly elucidated. It is demonstrated that the more adsorbed oxygen and an appropriate amount of intrinsic defects is advantageous to obtain superior CO gas sensitivity for ZnO nanorod arrays.     

An Efficient Method for Preparing the α-Deuterated-α,β-Unsaturated Carbonyl Compounds by Reaction of Stable Phosphonium Ylides with Carbonyl Compounds in Deuterium Oxide

Carbonyl compounds reacted with stable phosphonium ylides in D₂O to give α-deuterated-α,β-unsaturated carbonyl compounds in the same flask. The chemical yield and deuterium incorporation are excellent under our procedure. The fragile group like ozonide was compatible with our reaction condition.     

Preparation and characterization of plutonium/IV/ phenyl acetate and plutonium/IV/ α-naphthyl acetate

Plutonium/IV/ compounds obtained in the reactions with phenylacetic acid and -naphthyl acetic acid in the pH range of 3.5–5.0 have been isolated and studied. Carbon, hydrogen and plutonium analyses have shown that plutonium/IV/ phenyl acetate and plutonium/IV/ -naphthyl acetate have the composition Pu/OH/₃/C₁₀H₇CH₂COO/, respectively. Infra-red and ultra-violet absorption spectral studies and thermogravimetric analysis have corroborated these chemical formulas.     

Synthesis and Characterization of Novel 1‐Methyl‐3‐(4‐phenyl‐4H‐1,2,4‐triazol‐3‐yl)‐1H‐indazole Derivatives

A series of novel 1‐methyl‐3‐(4‐phenyl‐4H‐1,2,4‐triazol‐3‐yl)‐1H‐indazoles was synthesized in three steps from 5‐(1‐methyl‐1H‐indazol‐3‐yl)‐4‐phenyl‐2H‐1,2,4‐triazole‐3(4H)‐thiones. 5‐(1‐Methyl‐1H‐indazol‐3‐yl)‐4‐phenyl‐2H‐1,2,4‐triazole‐3(4H)‐thiones were converted into 1‐methyl‐3‐(5‐(methylsulfonyl)‐4‐phenyl‐4H‐1,2,4‐triazol‐3‐yl)‐1H‐indazoles upon methylation followed by treatment with aq. KMnO₄. The reaction of 1‐methyl‐3‐(5‐(methylsulfonyl)‐4‐phenyl‐4H‐1,2,4‐triazol‐3‐yl)‐1H‐indazoles with Raney nickel resulted in desulphonylation to afford corresponding 1‐methyl‐3‐(4‐phenyl‐4H‐1,2,4‐triazol‐3‐yl)‐1H‐indazoles. All the new synthesized compounds were characterized by spectral techniques.     

A tridentate CNO‐donor palladium(II) complex as efficient catalyst for direct C―H arylation: Application in preparation of imidazole‐based push–pull chromophores

A series of imidazolium chlorides for the formation of tridentate CNO‐donor palladium(II) complexes featuring N‐heterocyclic carbene moieties have been developed from cheap and readily available starting materials with high yields. Their palladium complexes were prepared by reactions between the ligand precursors and PdCl₂ using K₂CO₃ as base in pyridine with reasonable yields. These air‐stable metal complexes were characterized using ¹H NMR and ¹³C{¹H} NMR spectroscopy and elemental analyses. Heteronuclear multiple bond correlation experiments were performed to identify key NMR signals of these compounds. The structures of two of the complexes were also established by single‐crystal X‐ray diffraction analysis. One of these complexes was successfully applied in the direct C―H functionalization reactions between heterocyclic compounds and aryl bromides, producing excellent yields of coupled products. The coupling reactions were scalable, allowing grams of coupled products to be obtained with a mere 2 mol% of Pd loading. The catalyst system developed allowed the large‐scale preparation of several push–pull chromophores straightforwardly. Photophysical properties based on UV–visible and fluorescence spectroscopy for these chromophores were investigated. Deep blue photoluminescence with moderate quantum efficiency and twisted intramolecular charge transfer excited state were observed for these chromophores. Density functional theory (DFT) and time‐dependent DFT calculations were performed to support the experimental results.     

Blow‐up behavior of the Solution for the problem in a subdiffusive mediums

The diffusion problem in a subdiffusive medium is formulated by using the fractional differential operator. In this paper, we consider a fractional differential equation with concentrated source. The existence of the solution in a finite time is given. The finite time blow‐up criteria for the solution of the problem is established, and the location of the blow‐up point is investigated.     

A stochastic expectation-maximization algorithm for the analysis of system lifetime data with known signature

Statistical estimation of the model parameters of component lifetime distribution based on system lifetime data with known system structure is discussed here. We propose the use of stochastic expectation-maximization (SEM) algorithm for obtaining the maximum likelihood estimates of model parameters based on complete and censored system lifetimes. Different ways of implementing the SEM algorithm are also studied. We have shown that the proposed methods are feasible and are easy to implement for various families of component lifetime distributions. The proposed methodologies are then illustrated with two popular lifetime models—the Weibull and Birnbaum-Saunders distributions. Monte Carlo simulation is then used to compare the performance of the proposed methods with the corresponding estimation by direct maximization. Finally, two illustrative examples are presented along with some concluding remarks.     

Super quasiperiodic wave solutions and asymptotic analysis for $$ \mathcal{N} = 1 $$ supersymmetric KdV-type equations

Based on a general multidimensional Riemann theta function and the super Hirota bilinear form, we extend the Hirota method to construct explicit super quasiperiodic (multiperiodic) wave solutions of $ \mathcal{N} = 1 $ \mathcal{N} = 1 supersymmetric KdV-type equations in superspace. We show that the supersymmetric KdV equation does not have an N-periodic wave solution with arbitrary parameters for N ≥ 2. In addition, an interesting influencing band occurs among the super quasiperiodic waves under the presence of a Grassmann variable. We also observe that the super quasiperiodic waves are symmetric about this band but collapse along with it. We present a limit procedure for analyzing the asymptotic properties of the super quasiperiodic waves and rigorously show that the super periodic wave solutions tend to super soliton solutions under some “small amplitude” limits.     

Discretized Tikhonov regularization by reproducing kernel Hilbert space for backward heat conduction problem

In this paper we propose a numerical reconstruction method for solving a backward heat conduction problem. Based on the idea of reproducing kernel approximation, we reconstruct the unknown initial heat distribution from a finite set of scattered measurement of transient temperature at a fixed final time. Standard Tikhonov regularization technique using the norm of reproducing kernel is adopt to provide a stable solution when the measurement data contain noises. Numerical results indicate that the proposed method is stable, efficient, and accurate.