介绍一个与材料相关的研究型综合化学实验——壳聚糖的制备与表征

在中国科学技术大学夏季学期的研究型实验课程"化学科研基础训练"中开设"壳聚糖的制备与表征"综合实验,以龙虾壳为原料,通过除蛋白、脱盐、脱色、脱乙酰等一系列反应,制备得到目标产物壳聚糖。运用红外光谱、核磁共振仪、黏度法、滴定等对产品的结构及性能进行表征。     

The Effect of the Spacer of Bis(biurea) Ligands on the Structure of A2L3‐type (A=anion) Phosphate Complexes

By tuning the length and rigidity of the spacer of bis(biurea) ligands L, three structural motifs of the A₂L₃ complexes (A represents anion, here orthophosphate PO₄^3?), namely helicate, mesocate, and mono‐bridged motif, have been assembled by coordination of the ligand to phosphate anion. Crystal structure analysis indicated that in the three complexes, each of the phosphate ions is coordinated by twelve hydrogen bonds from six surrounding urea groups. The anion coordination properties in solution have also been studied. The results further demonstrate the coordination behavior of phosphate ion, which shows strong tendency for coordination saturation and geometrical preference, thus allowing for the assembly of novel anion coordination‐based structures as in transition‐metal complexes.     

无序激光晶体及其超快激光研究进展

激光是受激辐射的光放大,所辐射的波长取决于增益介质中关键电子的能级结构,特别是其最外层电子的状态决定了可能实现的激光特性。激光发展60年来,激光晶体作为激光的重要激活材料,推动了激光技术的进步和普及,是一个研究历史长而又异常活跃的研究领域。当前,超短超强脉冲激光在加工、医疗、国防等关系国计民生的领域有重要需求,适合超短超强激光的激光晶体成为了本领域的研究热点,其关键是揭示最外层电子的影响因素及设计和生长具有宽波段发射性能的激光晶体。本论文从探讨影响激活离子光谱性能的关键因素出发,综述了以本课题组十余年研究的10余种无序激光晶体为主要部分的研究结果和进展,涉及晶体生长、晶体物理、激光器件设计及应用等工作,包含了高级、中级和低级对称性晶体及其获得的最短脉冲激光结果,希望能为本领域的后续研究提供一定的参考和借鉴。     

离子对反相高效液相色谱法同时测定尿液中复方α-酮酸片的5种有效成分

建立了同时测定尿液中复方α-酮酸片5种有效成分(消旋羟蛋氨酸钙(HMACa)、酮缬氨酸钙(KVCa)、消旋酮异亮氨酸钙(KILCa)、酮亮氨酸钙(KLCa)和酮苯丙氨酸钙(KPACa))的离子对反相高效液相色谱法。分别考察了离子对试剂浓度、缓冲盐浓度和流动相pH值等参数对分离情况的影响。最终采用Waters Symmetry C18色谱柱(250 mm×4.6 mm,5μm);以乙腈和含15 mmol/L四丁基氢氧化铵的20 mmol/L磷酸盐缓冲液(pH 7.0)为流动相进行梯度洗脱,流速为1.0 mL/min;柱温为35℃;检测波长为210 nm。在上述条件下,5种有效成分得到很好的分离,并且不受尿液中内源性基质的干扰,在20~200 mg/L范围内线性关系良好(r≥0.999 0);HMACa、KVCa、KILCa、KLCa和KPACa的检出限(S/N=3)分别为3.0、5.0、3.6、5.7和2.5 mg/L;定量限(S/N=10)分别为9.6、16.7、12.0、19.0和8.3 mg/L;日间、日内精密度均小于7%;平均回收率在86.79%~112.00%之间,RSD小于9%(n=5)。该方法准确,灵敏度高,重现性好,适用于尿液中这5种有效成分的检测。     

基于响应面法的直拉硅单晶生长工艺参数优化方法

在直拉法制备硅单晶的过程中,要得到优质的晶体必须建立合理的温度分布,而单晶炉内热场的分布与工艺参数的设定密切相关.其中以晶体转速、坩埚转速和拉速等三个工艺参数对热场分布的影响尤为显著.为了确定最佳热场分布下晶转、埚转及拉速的设定值,本文采用响应面算法通过方程拟合、回归分析等步骤求解这三个工艺参量与温度梯度之间的最佳函数模型,并在该模型下同时对这三个工艺参量进行优化分析,且通过仿真实验和拉晶实验表明该方法的有效性.     

Synthesis and Photophysical Properties of a Sc3N@C80‐Corrole Electron Donor–Acceptor Conjugate

Embedding endohdedral metallofullerenes (EMFs) into electron donor–acceptor systems is still a challenging task owing to their limited quantities and their still largely unexplored chemical properties. In this study, we have performed a 1,3‐dipolar cycloaddition reaction of a corrole‐based precursor with Sc₃N@C₈₀ to regioselectively form a [5,6]‐adduct ( 1 ). The successful attachment of the corrole moiety was confirmed by mass spectrometry. In the electronic ground state, absorption spectra suggest sizeable electronic communications between the electron acceptor and the electron donor. Moreover, the addition pattern occurring at a [5,6]‐bond junction is firmly proven by NMR spectroscopy and electrochemical investigations performed with 1 . In the electronically excited state, which is probed in photophysical assays with 1 , a fast electron‐transfer yields the radical ion pair state consisting of the one‐electron‐reduced Sc₃N@C₈₀ and of the one‐electron‐oxidized corrole upon its exclusive photoexcitation. As such, our results shed new light on the practical work utilizing EMFs as building blocks in photovoltaics.     

The High Energy X-ray telescope (HE) onboard the Insight-HXMT astronomy satellite

The Insight-Hard X-ray Modulation Telescope(Insight-HXMT) is a broadband X-ray and γ-ray(1-3000 ke V) astronomy satellite. One of its three main telescopes is the High Energy X-ray telescope(HE). The main detector plane of HE comprises 18 Na I(Tl)/Cs I(Na) phoswich detectors, where Na I(Tl) is used as the primary detector to measure ~ 20-250 ke V photons incident from the field of view(FOV) defined by collimators, and Cs I(Na) is used as the active shielding detector to Na I(Tl) by pulse shape discrimination. Additionally, Cs I(Na) is used as an omnidirectional γ-ray monitor. The HE collimators have a diverse FOV,i.e. 1.1°×5.7°(15 units), 5.7°×5.7°(2 units), and blocked(1 unit). Therefore, the combined FOV of HE is approximately5.7°×5.7°. Each HE detector has a diameter of 190 mm resulting in a total geometrical area of approximately 5100 cm2, and the energy resolution is ~15% at 60 ke V. For each recorded X-ray event by HE, the timing accuracy is less than 10 μs and the deadtime is less than 10 μs. HE is used for observing spectra and temporal variability of X-ray sources in the 20-250 ke V band either by pointing observations for known sources or scanning observations to unveil new sources. Additionally, HE is used for monitoring the γ-ray burst in 0.2-3 Me V band. This paper not only presents the design and performance of HE instruments but also reports results of the on-ground calibration experiments.