Efficient synthesis of morolic acid and related triterpenes starting from betulin

Morolic acid (1) is a naturally occurring pentacyclic triterpene whose derivatives exhibit promising anti-HIV and other biological activities. An efficient synthesis of 1 has been accomplished in 11 steps with a total yield of 24% starting from betulin. Some related natural triterpenes including moradiol (4), acridocarpusic acid D (5), acridocarpusic acid E (6), and moronic aldehyde (7) have also been synthesized. Biological assay results showed that 1, 5, and 6 exhibited moderate inhibitory activity against glycogen phosphorylase.     

Directed 3-cycle decompositions of complete directed graphs with quadratic leaves

Let G be a vertex-disjoint union of directed cycles in the complete directed graph D_t, let |E(G)| be the number of directed edges of G and suppose or if t=5, and if t=6. It is proved in this paper that for each positive integer t, there exist -decompositions for D_t−G if and only if .     

Determination of soil amino acids by high performance liquid chromatography-electro spray ionization-mass spectrometry derivatized with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate

Determination of amino acids by mass spectrometry (MS) is an important technique to investigate soil nitrogen transformation and cycling as amino acids being the major nitrogen-containing compounds in soil organic matter. However, researchers have long faced a critical problem in coupling an efficient separation technique to a sensitive MS detection system simultaneously. In this context, we established a new method of liquid chromatography coupled to mass spectrometry based on the 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) derivatization method for convenient and accurate quantification of amino acids in soil samples. Baseline separation of 17 amino acid AQC-derivatives was achieved on an XTerra^R MS C₁₈ column using ammonium formate as a mobile phase modifier. The concentration of ammonium formate and the pH of the mobile phase were optimized in order to obtain sensitive MS signals. The response curves were linear over the range of 50-800 μmol L⁻¹ amino acids. The detection limits were 0.20-0.60 pmol μL⁻¹ on column and 0.07-0.24 μg g⁻¹ soil under the optimized conditions. The method has been applied successfully for the first time to determine amino acids in 4 types of soil samples, in which 15 amino acids were quantified by MS detector but methionine and cystine were below the detection limits. Both the recovery and the precision were satisfactory. Hence, this proposed technique shows a potential for the identification of amino acids in soil as well as tracing the transformation of soil amino acids with isotope dilution technique in nitrogen cycling investigation.     

An immunoassay for bisphenol A based on direct hapten conjugation to the polystyrene surface of microtiter plates

Based on direct hapten coated format a competitive indirect enzyme-linked immunosorbent assay (ciELISA) for bisphenol A (BPA) was developed. Polystyrene surface was modified by 3-Aminopropyltriethoxysilane (APTES) to produce amino groups after H₂SO₄/HNO₃-pre-treatment. 4,4-bis (4-hydroxyphenyl) valeric acid (BVA) which is analogue of BPA, was successfully immobilized on the surface of microtiter plates by N,N′-dicyclohexylcarbodiimide (DCC) method. The essential steps of the assay were optimized, especially blocking procedure which is key step to prevent unspecific binding of antibody. The results indicated that compared with hapten-protein coated format (IC₅₀ = 176.67 ng ml⁻¹, LOD = 15.90 ng ml⁻¹), the direct hapten coated format (IC₅₀ = 23.50 ng ml⁻¹, LOD = 0.27 ng ml⁻¹) could improve assay sensitivity and the detection ranges were 2.30 ng∼157.60 ng ml⁻¹ with good signal reproducibility (P value > 0.05) after careful optimization of assay conditions. Tap water samples and seawater samples were spiked with a known amount of BPA and measured by ciELISA. The average recoveries were between 70 and 142%. As far as we are aware this is the most sensitive ELISA for BPA yet reported.     

Chemical oxidative degradation of Polybenzimidazole in simulated environment of fuel cells

The chemical oxidative degradation process of poly [2,2′-(m-phenylene)-5,5′-bibenzimidazole] (PBI) in simulated environment of fuel cells was evaluated. From the mechanical properties and the intrinsic viscosity of PBI, it was observed that the stress at break of PBI membranes decreased and the macromolecular chains of PBI were broken after the treatment in Fenton reagent for 24 h. From the photos of Scanning Electron Microscope, it was identified that there were lots of corroded holes in PBI membranes. By means of FTIR and ¹H NMR analysis, it was shown that during the treatment of PBI in the presence of HO or HOO free radicals the hydrogen atom of N-H bond in imidazole ring was liable to be oxidized, and the phenyl was oxidized with the formation of quinine and dicarboxylic acid structures. In the end, the possible mechanism of the chemical oxidative degradation of PBI was proposed.     

Measurements of effective delayed neutron fraction in a fast neutron reactor using the perturbation method

A perturbation method is proposed to obtain the effective delayed neutron fraction β_(eff) of a cylindrical highly enriched uranium reactor.Based on reactivity measurements with and without a sample at a specified position using the positive period technique,the reactor reactivity perturbation △ρ of the sample in β_(eff) units is measured.Simulations of the perturbation experiments are performed using the MCNP program.The PERT card is used to provide the difference dκ of effective neutron multiplication factors with and without the sample inside the reactor.Based on the relationship between the effective multiplication factor and the reactivity,the equation β~(eff)=dκ/△ρ is derived.In this paper,the reactivity perturbations of 13 metal samples at the designable position of the reactor are measured and calculated.The average β_(eff) value of the reactor is given as 0.00645,and the standard uncertainty is 3.0%.Additionally,the perturbation experiments for β_(eff) can be used to evaluate the reliabilities of the delayed neutron parameters.This work shows that the delayed neutron data of ~(235)U and ~(238)U from G.R.Keepin's publication are more reliable than those from ENDF-B6.0.ENDF-B7.0,JENDL3.3 and CENDL2.2.     

燃爆冲击作用下岩石初始破坏区形成机制与主控因素

为揭示燃爆冲击作用下井周岩石破坏区的形成机制,并分析影响初始破坏区(破碎区和初始裂隙区)的主控因素,开展了两种岩样在不同加载速率下的冲击破坏实验, 分析了岩石冲击破坏模式及岩石对加载速率的响应, 借助基于Von Mise准则建立的岩石冲击破坏的破碎区和初始裂隙区计算模型可知:加载速率低于190 GPa/s时,可依据冲击峰值压力引导的应力分布确定破碎区和初始裂隙区作用范围;燃爆压裂在近井地带主要产生破碎区和裂隙区,破碎区直径为井眼直径的1~3倍,初始裂隙区直径为井眼直径的5~7倍;冲击载荷作用下,初始破坏区与加载速率、脆性指数呈正相关,且受脆性指数影响更显著。研究结果可提高对燃爆压裂过程中岩石的破坏模式及其主控因素的认识深度,为燃爆压裂冲击条件设计提供指导。     

铝盐与氢氧化钠反应生成氢氧化铝沉淀的实验探究

通过数字实验对Al2(SO4)3溶液与NaOH反应过程中pH的变化进行探究,得出pH与NaOH溶液的体积(V)之间的变化曲线,从而建立铝盐与NaOH溶液反应时,Al(OH)3沉淀的生成与溶解和NaOH量的变化关系。此研究可以改变人们在Al(OH)3两性认识上存在的误区,对中学化学教学起到积极的作用。     

磁性和非磁性元素掺杂的自旋梯状化合物Sr_(14)(Cu_(0.97)M_(0.03))_(24)O_(41)(M=Zn,Ni,Co)的结构和电输运性质

利用固相反应法制备了Sr14Cu24O41及其系列B位掺杂Sr14(Cu0.97M0.03)24O41(M=Zn,Ni,Co)的样品.X射线衍射分析显示,所有样品均为纯相,晶格常数a与c没有明显的变化;Zn掺杂样品晶格常数b没有明显变化,而Ni,Co掺杂样品晶格常数b分别稍有增加.选区电子衍射研究揭示:磁性元素Ni,Co及非磁性元素Zn掺杂,可能主要替代了Sr14Cu24O41结构中自旋链上的Cu原子,从而影响了自旋链上的dimer排列,破坏电荷有序超结构.电输运测量显示:Zn2+,Ni2+,Co3+离子掺杂样品的电阻率降低,但仍体现半导体行为,所有的掺杂样品都存在一个渡越温度Tρ,当TTρ时,其导电机理是以单空穴热激发导电占主要地位,在TTρ时,配对的局域化空穴的一维变程跳跃导电占主要优势;在相同的掺杂量下,非磁性元素Zn掺杂对电阻率值的影响大于磁性元素Ni,Co掺杂的影响,而磁性元素Ni,Co掺杂对渡越温度Tρ的影响大于非磁性元素Zn掺杂的影响.     

Modulational instability in a layered Kerr medium: theory and experiment

We present the first experimental investigation of modulational instability in a layered Kerr medium. The particularly interesting and appealing feature of our configuration, consisting of alternating glass-air layers, is the piecewise-constant nature of the material properties, which allows a theoretical linear stability analysis leading to a Kronig-Penney equation whose forbidden bands correspond to the modulationally unstable regimes. We find very good quantitative agreement between theoretical, numerical, and experimental diagnostics of the modulational instability. Because of the periodicity in the evolution variable arising from the layered medium, there are multiple instability regions rather than just one as in a uniform medium.