Reversible 5′-end biotinylation and affinity purification of synthetic RNA

A reversible biotinylation phosphoramidite was synthesized and incorporated onto the 5′-end of an oligoribonucleotide on a solid phase synthesizer. After cleavage and deprotection, the crude synthetic oligomer mixture was incubated with NeutrAvidin^® coated microspheres, and the failure sequences removed by washing with a buffer followed by treating the microspheres with tetrabutylammonium fluoride to give a high quality unmodified full-length oligoribonucleotide.     

Preparation of Y2Ba4Cu7O15-δ Superconductor without High Oxygen Pressure

The synthesis of bulk Y₂Ba₄Cu₇O_15-δ superconductor at atmospheric oxygen pressure via solid state sintering is reported. Temperature ranging from 860 to 890 °C as well as time interval over 2 to 15 days were used to investigate the formation of the Y₂Ba₄Cu₇O_15-δ phase. A time-temperature profile characterizing the conditions for the preparation of Y₂Ba₄Cu₇O_15-δ phase suggests the optimal condition to be sintering at 890 °C for over 10 days. Detailed results of X-ray diffraction, electrical resistivity, iodometric titration and magnetization measurements are described.     

Syntheses of macrocyclic bisbibenzyls on solid support

We describe a route for the polymer supported total synthesis of the cyclic bisbibenzyls of the isoplagiochin type found in liverworts. TentaGel^® resins were used as solid support for a sequence involving Suzuki, Wittig and hydrogenation protocols. The polymer linked intermediates could be characterized by HR-MAS NMR. This route is to be extended to the synthesis of small libraries of differently halogenated derivatives.     

Synthesis, crystal structure and magnetic property of a new nickel selenite chloride: Ni5(SeO3)4Cl2

The new nickel selenite chloride, Ni₅(SeO₃)₄Cl₂, was obtained by high-temperature solid state reaction of NiCl₂, Ni₂O₃ and SeO₂ in a 1:2:4 molar ratio at 700 °C in an evacuated quartz tube. Its structure was established by single-crystal X-ray diffraction. Ni₅(SeO₃)₄Cl₂ crystallizes in the triclinic system, space group P-1 (No. 2) with cell parameters of a=8.076(2), b=9.288(2), c=9.376(2) Å, α=101.97(3), β=105.60(3), γ=91.83(3)° and Z=2. All nickel(II) ions in Ni₅(SeO₃)₄Cl₂ are octahedrally coordinated by selenite oxygens or/and chloride anions (([Ni(1)O₅Cl], [Ni(2)O₄Cl₂], [Ni(3)O₅Cl], [Ni(4)O₆] and [Ni(5)O₄Cl]). The structure of the title compound features a condensed three-dimensional (3D) network built by Ni(II) ions interconnected by SeO₃²⁻ anions as well as Cl⁻ anions. Magnetic property measurements show strong antiferromagnetic interaction between nickel(II) ions.     

Analysis of organic compounds in environmental samples by headspace solid phase microextraction

The analysis of samples contaminated by organic compounds is an important aspect of environmental monitoring. Because of the complex nature of these samples, isolating target organic compounds from their matrices is a major challenge. A new isolation technique, solid phase microextraction, or SPME, has recently been developed in our laboratory. This technique combines the extraction and concentration processes into one step; a fused silica fiber coated with a polymer is used to extract analytes and transfer them into a GC injector for thermal desorption and analysis. It is simple, rapid, inexpensive, completely solvent-free, and easily automated. To minimize matrix interferences in environmental samples, SPME can be used to extract analytes from the headspace above the sample. The combination of headspace sampling with SPME separates volatile and semi-volatile analytes from non-volatile compounds, thus greatly reducing the interferences from non-target compounds. This paper reports the use of headspace SPME to isolate volatile organic compounds from various matrices such as water, sand, clay, and sludge. By use of the technique, benzene, toluene, ethyl-benzene, and xylene isomers (commonly known as BTEX), and volatile chlorinated compounds can be efficiently isolated from various matrices with good precision and low limits of detection. This study has found that the sensitivity of the method can be greatly improved by the addition of salt to water samples, water to soil samples, or by heating. Headspace SPME can also be used to sample semi-volatile compounds, such as PAHs, from complex matrices.     

Determination of the optical second harmonic response of pharmaceutical solid–solid mixtures

We report on a new method for characterising crystallinity and polymorphism of pharmaceutical drugs and excipients in the solid state. The optical nonlinearity of certain crystalline structures allows under certain circumstances the quantitative determination of polymorphism or crystallinity. An apparatus was set up to measure the second harmonic response of powdered samples when irradiated with a pulsed laser source. Here we present experimental results from various pharmaceutically interesting materials. This rapid, novel technique has potential for industrial monitoring of pharmaceutical manufacturing processes.     

Clarification of regimes determining sonochemical reactions in solid particle suspensions

Although there has been extensive research on the factors that influence sonochemical reactions in solid particle suspensions, the role that solid particles play in the process remains unclear. Herein, the effect of monodisperse silica particles (10–100 μm, 0.05–10 vol%) on the sonochemical activity (20 kHz) was investigated using triiodide formation monitoring and luminol tests. The results demonstrate that, in the particle size range considered, the sonochemical yields were enhanced in dilute suspensions (0.05–1 vol%), while further particle addition in semi-dilute suspensions (1–10 vol%) decreased the yields. Two regimes, namely the site-increasing regime and sound-damping regime, are identified in respect of the enhancing and inhibiting effects of the particles, respectively, and their dependence on particle characteristics is analyzed. Both regimes are confirmed based on the cavitation erosion test results or cavitation noise analysis. The clarification of the two regimes provides a better understanding of the dominant factors controlling sonochemistry in the presence of solid particles, as well as a guide for sonochemical efficiency prediction.     

Solution processed Al-doped ZnO and its performance in dye sensitized solar cells

Al-doped ZnO rods of nanometer to sub-micrometer size range have been successfully synthesized by a simple yet cost-effective solution processed sonochemical technique. Systematic XRD analysis established the solid solubility limit for Al in the ZnO lattice to be ca. 3 mol% at an elevated annealing temperature of 800 °C. The secondary ZnAl₂O₄ phase appears with increasing dopant concentrations and at lower annealing temperatures. Significant variations in the optoelectronic properties are induced by modifications in the surface defects of ZnO rods as a result of Al doping. As a consequence, an improved fill factor (FF) of 74.78 and 75.76% with a conversion efficiency (η) of 1.59 and 1.79% have been achieved for the fabricated DSSC devices made of the 800 °C annealed ZnO rods doped by 1 and 3 mol% Al, respectively.     

HL-2M 装置固态亚毫米波干涉系统研制

发展了一套固态亚毫米波外差干涉系统和一种基于全相位快速傅里叶变换(apFFT)的相位处理方法用 于测量 HL-2M 初始等离子体电子密度。该系统采用平面型二极管倍频技术对低频的锁相微波源进行高次倍频以 产生功率大于 0.1MW、频率 306.9GHz 的探测波。基于 apFFT 的相位处理数值算法可以从原始信号中提取相位信 息,缓解由可能的高水平密度扰动导致的相位跳变。系统的固有时间分辨率为 5μs,电子密度测量范围在 10¹⁶~10²⁰m⁻³。在 HL-2M 装置首次实验期间,该系统被安装在中平面上,利用装置内壁反射实现干涉测量,成功 测量了线平均电子密度。