Precise Synthesis and Thin Film Self-Assembly of PLLA-b-PS Bottlebrush Block Copolymers

The ability of bottlebrush block copolymers (BBCPs) to self-assemble into ordered large periodic structures could greatly expand the scope of photonic and membrane technologies. In this paper, we describe a two-step synthesis of poly(l-lactide)-b-polystyrene (PLLA-b-PS) BBCPs and their rapid thin-film self-assembly. PLLA chains were grown from exo-5-norbornene-2-methanol via ring-opening polymerization (ROP) of l-lactide to produce norbornene-terminated PLLA. Norbonene-terminated PS was prepared using anionic polymerization followed by a termination reaction with exo-5-norbornene-2-carbonyl chloride. PLLA-b-PS BBCPs were prepared from these two norbornenyl macromonomers by a one-pot sequential ring opening metathesis polymerization (ROMP). PLLA-b-PS BBCPs thin-films exhibited cylindrical and lamellar morphologies depending on the relative block volume fractions, with domain sizes of 46–58 nm and periodicities of 70–102 nm. Additionally, nanoporous templates were produced by the selective etching of PLLA blocks from ordered structures. The findings described in this work provide further insight into the controlled synthesis of BBCPs leading to various possible morphologies for applications requiring large periodicities. Moreover, the rapid thin film patterning strategy demonstrated (>5 min) highlights the advantages of using PLLA-b-PS BBCP materials beyond their linear BCP analogues in terms of both dimensions achievable and reduced processing time.     

焦炉上升管内壁结焦炭层的光谱学分析及结焦机理研究

以焦炉上升管内壁结焦炭层块为研究对象，采用X射线荧光光谱仪（XRF）、X射线衍射仪（XRD）、傅里叶红外光谱仪（FTIR）和激光共聚焦拉曼光谱仪（Raman）对结焦炭层的元素组成，以及各结焦炭层的矿物组成、组成结构和分子结构进行测试。分析从结焦炭层块外表面向内表面过渡的各结焦炭层的差异性，揭示焦炉上升管内壁结焦机理。结果表明焦炉上升管内粉尘中Fe，S和Cr极易催化荒煤气中蒽、萘等稠环芳烃化合物成炭，在焦炉上升管内壁形成炭颗粒沉积，为焦油凝结挂壁提供载体，在荒煤气温度降至结焦温度时易结焦积碳。结焦炭层均含有芳香层结构，随着结焦炭层从外表面向内表面过渡，各结焦炭层的面层间距(d₀₀₂)逐渐降低、层片直径(L_a)先降低后增加、层片堆砌高度(Lc)和芳香层数(N)先稳定后增加。结焦炭层石墨化过程是由结焦炭层内表面向外表面进行，主要包括其片层外缘的羧基和部分C-O结构的降解剥离，从而形成高度规整的共轭结构。结焦炭层块中C元素是以结晶碳与无定型碳的混合物形式存在。以上研究为解决焦炉上升管内壁结焦及腐蚀问题，提高换热器换热效率，有效回收焦炉荒煤气显热，降低焦化企业能耗提供实验基础和理论依据。     

电感耦合等离子体原子发射光谱法测定中药方剂煎煮液中的微量元素

本文采用HNO3－H2O2对中药方剂煎煮液进行处理，拟定了电感耦合等离子体原子发射光谱法同时测定试样中12个微量元素的方法，选择了仪器的最佳工作条件，考察了基本效应的影响。在选定条件下，12个微量元素的检出限为0．10－5．0ng/g，相对标准偏差为0.10%-9.5%(n=10),加标回收率为85％－103％。该方法简单、快速，已用于大量样品的检测，分析结果满意。     

Improvements in Depth Selective Electron Mössbauer Spectroscopy

The conditions for achievement of high resolving power of depth selective conversion electron Mössbauer spectroscopy method at a combined installation ‘electron spectrometer–nuclear gamma-resonance spectrometer’ have been obtained. There has been made a considerable step in development of the method at its realization at a magnetic sector electron spectrometer with double focusing, equipped with electron source (a sample under investigation) of large-area and position-sensitive detector. The paper presents a prospective symmetrical version of a magnetic sector electron spectrometer that allows realizing more completely possibilities of the method. It is noted that the proposed method is particularly valuable for investigations of nanosystems, nanostrutures that contain Mössbauer nuclei.     

利用场发射显微镜研究O2对单壁碳纳米管场发射的影响

利用场发射显微镜和四极质谱计研究了充入高纯O2的四极质谱和O2对单壁碳纳米管场发射的影响.单壁碳纳米管经过约1000℃的热处理得到清洁态场发射像后，充入O2，分别测量了O2吸附和脱附后场发射的I V特性.实验观测到在单壁碳纳米管上O2的吸附使场发射电流减小，说明逸出功增加.在10-4Pa的O2压强下对单壁碳纳米管进行约1000℃的热处理，可以产生氧化刻蚀作用，观测到场发射像的变化，并测量了氧化刻蚀产生的I V特性变化. 关键词： 单壁碳纳米管 场发射显微镜 场发射 四极质谱     

Decomposition Methods for Differentiable Optimization Problems over Cartesian Product Sets

This paper presents a unified analysis of decomposition algorithms for continuously differentiable optimization problems defined on Cartesian products of convex feasible sets. The decomposition algorithms are analyzed using the framework of cost approx imation algorithms. A convergence analysis is made for three decomposition algorithms: a sequential algorithm which extends the classical Gauss-Seidel scheme, a synchronized parallel algorithm which extends the Jacobi method, and a partially asynchronous parallel algorithm. The analysis validates inexact computations in both the subproblem and line search phases, and includes convergence rate results. The range of feasible step lengths within each algorithm is shown to have a direct correspondence to the increasing degree of parallelism and asynchronism, and the resulting usage of more outdated information in the algorithms.     

Efficient Sequential Quadratic Programming Implementations for Equality-Constrained Discrete-Time Optimal Control

Efficient sequential quadratic programming (SQP) implementations are presented for equality-constrained, discrete-time, optimal control problems. The algorithm developed calculates the search direction for the equality-based variant of SQP and is applicable to problems with either fixed or free final time. Problem solutions are obtained by solving iteratively a series of constrained quadratic programs. The number of mathematical operations required for each iteration is proportional to the number of discrete times N. This is contrasted by conventional methods in which this number is proportional to N ³. The algorithm results in quadratic convergence of the iterates under the same conditions as those for SQP and simplifies to an existing dynamic programming approach when there are no constraints and the final time is fixed. A simple test problem and two application problems are presented. The application examples include a satellite dynamics problem and a set of brachistochrone problems involving viscous friction.     

微波消解ICP-AES法同时测定花岗石中铜、镉、铬和砷

本文采用微波消解和ICP－AES法，同时测定花岗石样品的铅、镉、铬、砷4有害元素，检出限分别为0．0008、0．0007、0．0018、0．0012μg.mL^-1,回收率为93．4％－102．5％，RSD为1．3％－3．6％，该法准确、快速、简便，结果令人满意。     

ICP-AES测定饮用水源中的Cu、Mn、Pb、Cd、Zn

用ICP－AES法同时测定饮用水源中的Cu、Mn、Pb、Cd、Zn等重金属元素，具有基体效应小、测量范围宽等优点。检出限为0．2－4．0μg/L，回收率为91．5％－103．9％，相对标准偏差为0．29％－1．5％，测定密码样与实际样品，结果令人满意。     

The analysis of volatile trace compounds in landfill gases,compost heaps and forest air

Landfill gas, cryotrapped on a loop fashioned from a length of a capillary gas chromatography (GC) column, was examined for volatile organometallic compounds (VOMCs) and for volatile organic compounds (VOCs) by using GC–mass spectrometry (MS). A large number of organic components were present and many were identified, but the only VOMCs present in high enough concentrations to be detected were trimethylstibine and tetramethyltin. The use of inductively coupled plasma (ICP)‐MS as an element‐specific detector allowed the identification of a number of other organometallic species in the landfill gas, including trimethylarsine and trimethylbismuth, and, for the first time, butyltrimethyltin and dibutyldimethyltin. The presence of molybdenum hexacarbonyl was confirmed. Gas from a large‐scale compost heap and from compost incubated in the laboratory contained iodomethane but no common VOMCs (GC–ICP‐MS). Only VOCs were present in forest air (GC–MS). Copyright © 2003 John Wiley & Sons, Ltd.