正交试验法优选穿心莲内酯硫酸酯化反应工艺

硫酸酯化反应以分子结构中的羟基为反应位点,向有机分子中引入硫酸酯基,是一种有效改善天然产物水溶性的结构修饰途径[1]。有些药物因水溶性差,致使其在临床应用中存在一些问题,如生物利用度不高,服用量大,制成的片剂或胶囊体内吸收缓慢等。这类化合物经硫酸酯化后不但可以增加     

DMF溶液中导电玻璃上沉积类金刚石薄膜

液相法制备类金刚石膜设备简单,操作容易,能大面积成膜,越来越受到研究者们的关注．Ｎａｍｂａ［１］以乙醇为介质,在１２００Ｖ电压７０℃以下沉积膜,得到了类金刚石膜;Ｓｕｚｕｋｉ等［２］以水乙二醇溶液为介质制膜,只得到了石墨相的碳膜;以乙醇的水溶液为介质利用电解热沉积膜,得到了玻璃碳和石墨碳,同时阴极钨发生碳化有ＷＣ和Ｗ２Ｃ生成［３］;Ｎｏｖｉｋｏｖ等［４］在乙炔的液氨溶液中沉积膜,Ｒａｍａｎ谱表明他们得到了类金刚石（ＤＬＣ）膜;Ｋｗｉａｔｅｋ等［５］重复了Ｎａｍｂａ的实验,证明沉积膜主要为非晶态…     

金刚石纳米线氮空位色心的表面与尺寸效应

使用大规模自旋极化密度泛函理论计算研究了表面修饰和尺寸对金刚石纳米线(DNs)中氮空位(NV)色心的几何结构、 电子结构、 磁性和稳定性的影响. 理论上设计了几种不同的DNs, 这些DNs具有不同的表面修饰(干净、 氢化和氟化), 并且直径达数百个原子. 实验结果证明, 中性(NV⁰)和带1个负电荷(NV^-)的NV色心的电子结构不受半导体表面修饰和DNs直径大小的影响, 但NV色心的稳定性对这两个因素具有不同的响应. 此外, 研究中还发现, 由于DNs中存在圆柱形表面电偶极子层, 对DNs中掺杂的NV^-色心的稳定性, 表面改性诱导了不依赖尺寸的长程效应. 特别地, 对于n型氟化金刚石表面, 掺杂在DN中的NV^-色心可以稳定存在, 而对于p型氢化表面, NV⁰则相对更稳定. 因此, 表面修饰为控制金刚石纳米线中的NV色心的电子结构和稳定性提供了一种精确有效的调控方法.     

Simultaneous voltammetric determination of carbendazim and carbaryl in medicinal plant infusions with a boron-doped diamond electrode

This study is aimed to develop an electroanalytical methodology using a boron-doped diamond electrode to determine simultaneously and selectively carbendazim (CBZ) and carbaryl (CAR). In previous studies using cyclic voltammetry oxidation, peaks were observed at 1.03 V (CBZ) and 1.44 V (CAR), with characteristics of an irreversible process controlled by diffusion of species, with a supporting electrolyte of BR buffer (0.1 mol L^?1) and pH adjusted to 6.0. The differences between the potentials for both pesticides, about 400 mV, indicate the possibility of selective determination of CBZ and CAR. The square-wave voltammetric parameters were optimised. The best separation conditions were pH 6.0, square-wave frequency of 100 s^?1, pulse amplitude of 50 mV and scan increment of 2.0 mV. These parameters were used to obtain the calibration curves of CBZ and CAR. An analytical curve was constructed in the range concentration of CBZ of 1.3 mg L^?1 to 15.3 mg L^?1 and CAR of 1.0 mg L^?1 to 11.4 mg L^?1, respectively. The limits of detection (LOD) and limits of quantification (LOQ) for CBZ were 0.40 mg L^?1 and 1.30 mg L^?1, respectively. For CAR, the LOD and LOQ were 0.30 mg L^?1 and 1.00 mg L^?1, respectively. Sensitivity values were 0.78 and 2.60 µA/mg L^?1 for CBZ and CAR, respectively. The electroanalytical method was applied in Mikania glomerata infusions. The recovery values were 106.2% and 116.5% for CBZ and CAR, respectively. The results show that the developed method is suitable for application in medicinal plant samples.     

以磷化铁为添加剂沿(111)面生长磷掺杂金刚石大单晶

掺杂是调控金刚石性能的一种重要手段。本文采用温度梯度法,在5.6 GPa、1 312 ℃的条件下,选用Fe₃P作为磷源进行磷掺杂金刚石大单晶的合成。金刚石样品的显微光学照片表明,随着Fe₃P添加比例的增加,金刚石晶体的颜色逐渐变深,包裹体数量逐渐增加,晶形由板状转变为塔状直至骸晶。金刚石晶形的变化表明Fe₃P的添加使生长金刚石的V形区向右偏移,这是Fe₃P改变触媒特性的缘故。红外光谱分析表明,Fe₃P的添加使金刚石晶体中氮含量上升,这说明磷的进入诱使氮原子更容易进入金刚石晶格中。激光拉曼光谱测试表明,随着Fe₃P添加比例的增加,所合成的掺磷金刚石的拉曼峰位变化不大,其半峰全宽(FWHM)值变大,这说明磷的进入使得金刚石晶格畸变增加。XPS测试结果显示,随着Fe₃P添加比例的增加,金刚石晶体中磷相对碳的原子百分含量也会增加,这意味着添加Fe₃P所合成的金刚石晶体中有磷存在。     

测定金刚石膜断裂强度及断裂韧性的力控制法研究

人造金刚石膜是一种新材料,断裂强度及断裂韧性是其主要力学性能指标,目前国内、外尚无相应的强度测试方法标准,一般采用类比陶瓷测定断裂强度与断裂韧性的方法进行,即采用位移控制法进行检测,基于金刚石膜是一种硬度比陶瓷更高的材料,本文首次提出对金刚石膜用一种力控制法进行检测,在试验时采用专用的弹性压力头加载,加载速度可调,加载平衡、可靠,收到了很好的效果。     

膨胀管残余应力测试

膨胀管残余应力是影响膨胀管抗外挤、内压强度的重要因素之一。确定膨胀管的残余应力,测试方法至关重要。在常用测试方法中,机械测量法中的盲孔法体现出测试的优越性。应用盲孔法测试J55、K55两种规格膨胀管的残余应力,并根据实际测试的应力水平和实验误差,采用应变释放系数分级法对试验结果进行修正,以提高测试结果的精度。实验结果表明,膨胀管膨胀后存在环向、轴向的残余应力,且外表面总是压残余应力。将实验结果与仿真结果对比,误差满足工程要求,说明盲孔法测试膨胀管残余应力方便、快捷、准确、有效。     

On the cut‐off phenomenon for the transitivity of randomly generated subgroups

Consider K ≥ 2 independent copies of the random walk on the symmetric group S_N starting from the identity and generated by the products of either independent uniform transpositions or independent uniform neighbor transpositions. At any time $n\in \mathbb{N}$, let G_n be the subgroup of S_N generated by the K positions of the chains. In the uniform transposition model, we prove that there is a cut‐off phenomenon at time N ln(N)/(2K) for the non‐existence of fixed point of G_n and for the transitivity of G_n, thus showing that these properties occur before the chains have reached equilibrium. In the uniform neighbor transposition model, a transition for the non‐existence of a fixed point of G_n appears at time of order $N^{1+\frac{2}{K}}$ (at least for K ≥ 3), but there is no cut‐off phenomenon. In the latter model, we recover a cut‐off phenomenon for the non‐existence of a fixed point at a time proportional to N by allowing the number K to be proportional to ln(N). The main tools of the proofs are spectral analysis and coupling techniques. © 2011 Wiley Periodicals, Inc. Random Struct. Alg., 2012     

Graphite–boron composite heater in a Kawai-type apparatus: the inhibitory effect of boron oxide and countermeasures

We have investigated the performance of a graphite–boron composite (GBC) with 3?wt % boron as a precursor for a boron-doped diamond heater in a Kawai-type apparatus at 15?GPa. We first tested a machinable cylinder of GBC sintered at 1000°C in Ar/H₂ gas (99:1 molar ratio). Boron oxide (B₂O₃) formed during sintering frequently hindered the GBC heater from stable operation at temperatures higher than 1400°C by producing melt throughout the heater together with oxide and/or silicates. We then rinsed the GBC heater in hydrochloric acid to remove B₂O₃. After rinsing, we succeeded in stably generating temperatures higher than 2000°C. We also improved a molding process of different-sized GBC tubes for convenient use and tested the molded GBC heater. It was free from the B₂O₃ problem. The electromotive force of the W/Re thermocouple was successfully monitored up to 2400°C.     

A comparison of the magnetic properties of proton- and iron-implanted graphite

In this work we have investigated the changes of the magnetic properties of highly oriented pyrolytic graphite samples after irradiation either with ~3×10¹⁴ protons or 3.5×10¹³ ... 3.5×10¹⁴ iron ions with energies in the MeV range. Our results show that iron and proton irradiations can produce similar paramagnetic contributions depending on the implantation temperature. However, only protons induce a ferromagnetic effect.