ICP-MS法快速测定丙烯腈/乙腈中的铁、铜

采用带八级杆碰撞/反应池(ORS)的电感耦合等离子体质谱法(ICP-MS),直接测定丙烯腈或乙腈产品中的Fe、Cu,标准加入法定量.结果表明,方法的线性范围宽,线性相关系数均大于0.999.2种元素的相对标准偏差均低于5%,加标回收率在90%~110%.该方法简便、快速、准确.     

丙烯氨氧化合成丙烯腈液体产物分析

本文利用１０３型气相层析仪与电子计算机联接，分析了丙烯氨氧化合成丙烯腈的液体产物。研究了分析方法的重复性和准确性，讨论了不同进样量和不同的校正因子对扁平乙腈峰的影响。结果表明，本方法可取代先有的丙烯腈化学分析方法。     

Plasma polymerization of cyano compounds

Plasma polymerizations of three cyano compounds—acrylonitrile (AN), 1,2-dicyanoethylene (FN), and tetracyanoethylene (TCE)—were investigated by FT IR and XPS, and the transforamtion of cyano groups during the plasma polymerization was discussed. The results pointed out an aspect of the preparation of plasma films with cyano groups. Plasma polymerizations of AN, FN, and TCE deposited brown or dark brown films that contained carbon, nitrogen, and oxygen. The elemental composition of the plasma films, especially N/C atomic ratio, showed a monomer dependence but no rf power dependence. The plasma films contained amide and amino groups, and ketene-imine and conjugated — C = N — structures as well as cyano groups as nitrogen functionalities, and carbonyl and carboxyl groups as oxygen functionalities. For the preparation of plasma films with cyano groups, compounds with more than two cyano groups themselves are not suitable as monomers. The operation of plasma polymerization under mild plasma conditions at low rf power and in no oxygen atmosphere is favorable for the preparation of plasma films with cyano groups. © 1992 John Wiley & Sons, Inc.     

Analysis of Low-k Organosilicon and Low-Density Silica Films Deposited in HMDSO Plasmas

Low-dielectric constant (low-k) films have been prepared by plasma-enhanced chemical vapor deposition from hexamethyldisiloxane (HMDSO). The films are analyzed by ellipsometry, infrared absorption spectroscopy while their electrical properties are deduced from C–V and I–V measurements performed on metal/insulator/silicon structures. First, it is shown that the carbon-containing silicon oxide films deposited in HMDSO and HMDSO/Ar plasmas have a dielectric constant equal to 3.0 ± 0.1 and are thermally stable at 400°C. The leakage current densities measured for an electric field of 1 MV/cm are less than 10^–9 A/cm² and the breakdown fields are in the range of 6–7 MV/cm. Then, a low-density silica film was obtained by exposing a film deposited in an HMDSO plasma to an O₂ plasma. The dielectric constant of this low-density silica film is 3.5 and its breakdown field is close to 6 MV/cm.     

傅里叶变换红外光谱和傅里叶变换拉曼光谱法无损鉴别药材的真伪

利用傅里叶变换红外（FT-IR）和近红外傅里叶变换拉曼（NIR FT-aman）光谱法对大黄（西宁大黄）与伪品大黄（华北大黄、山大黄、水根大黄）进行了无损快速的鉴别。结果表明：尽管正品大黄与伪品大黄差别较小，有大部分的化学成分有很大的相同之处，但在红外、拉曼谱图中各自的特征峰较突出，根据谱峰的强度和位置可容易地将它们区别开来。红外和拉曼光谱法相互印证，相互补充，具有快速、准确、操作简单、重复性好、不需对样品进行分离提取，可直接鉴别等特点。     

热解/红外光谱联用技术用于热解反应的快速检测

详细介绍了快速热解装置CDS2000／红外联用仪(Py／FTIR)的特点。带有样品的热解探头插入并固定在接口装置上，接口装置可直接置于FTIR的光路中，对热解产物进行直接、快速检测，并且可分析重质热解产物。CDS2000热丝裂解器具有极快的升温速度，升温速度从0．01℃／min到20000℃／s，可以有效避免热解过程中的二次反应，有助于推断结构和热解机理；另外，本文对CDS2000／FTIR热解／红外联用仪使用过程中的有关参数进行了分析，如分辨率的选择。本文应用CDS2000／FTIR联用仪对PVC、生物质和模型化合物进行了热解实验，取得了满意的结果。     

Design and synthesis of highly reactive photopolymerizable epoxy monomers

The synthesis of a series of novel cationically photopolymerizable epoxide monomers bearing benzyl, allyl, and propargyl acetal and ether groups that can stabilize free radicals was carried out. These monomers display enhanced reactivity in cationic photopolymerization in the presence of certain onium salt photoinitiators. Specifically, this article describes schemes for the synthesis of cycloaliphatic epoxy monomers bearing free‐radical stabilizing groups. During UV irradiation of an onium salt cationic photoinitiator, the aryl radicals that are generated abstract labile protons present in such monomers to generate the corresponding carbon‐centered radicals. Subsequently, these radicals can interact with the onium salt by a redox mechanism to induce the decomposition of these salts. The overall result is that additional cationic species are generated by this mechanism that increase the rate and extent of the cationic ring‐opening polymerization of the epoxide monomer. An investigation of the photopolymerizations of the monomers prepared during this work was carried out using Fourier transform real‐time infrared spectroscopy, and conclusions were drawn with respect to the relationship between their structures and reactivity. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 39: 2385–2395, 2001     

新型丝素蛋白膜的结构和热分解动力学机理

采用氯化钙-甲酸溶解新方法,制备了氯化钙含量分别为1.50%(w,质量分数)和3.00%(w)的新型丝素蛋白膜SF-1.5和SF-3.0。运用傅里叶变换红外光谱技术和X射线衍射技术对样品的分子构象和结晶结构进行了表征。同时,利用热重技术对比研究了两种膜的热稳定性和热分解特性,依据Kissinger、Ozawa和Vyazovkin模型,考察了氯化钙含量对丝素蛋白膜热分解反应的热力学参数和动力学参数以及其机理函数的影响。结果表明,丝素蛋白膜SF-1.5中蛋白分子主要以β-折叠结构为主,丝素蛋白膜SF-3.0中蛋白分子构象主要以无规卷曲为主;SF-3.0膜在不同升温速率下的分解温度、活化能和活化焓均低于SF-1.5膜,SF-1.5膜的热稳定性优于SF-3.0膜。另外,利用Achar法和Coats-Redfern法研究发现:丝素蛋白膜在190.00-330.00°C的热分解过程遵循二维扩散(圆柱形对称)机理。     

不同产地黄芪的红外光谱鉴别研究

采用红外光谱、二阶导数红外光谱和二维相关红外光谱,对四种不同产地的黄芪原药材进行了鉴别研究。结果表明:不同产地黄芪的红外光谱和二阶导数红外谱具有一定的相似度,与淀粉的红外谱图比对,4个不同产地的黄芪均含有淀粉,其中陕西绥德产黄芪的淀粉含量比其它3个产地黄芪的都要高。山西浑源和山西天镇产黄芪谱图的1 510、1 425cm-1木质素特征峰比内蒙古固阳和陕西绥德产黄芪的更为明显,说明前二者产黄芪中木质素含量高于后二者产黄芪。在二维相关红外谱图上,根据4个产地黄芪的相对峰强度的差异,可进行产地的鉴别。研究结果表明对于不同产地黄芪的鉴别,红外三级鉴定法是一种快速有效的新方法。     

二维相关红外光谱法与阿胶的真伪鉴别

采用傅里叶变换红外光谱法(FT-IR)和二维相关红外光谱技术(2D-IR)对几种阿胶进行了真伪鉴别。实验结果表明,伪品阿胶和黄明胶与标本东阿阿胶的谱图较为相似,尤其是黄明胶与阿胶极其相似,仅仅在1648cm^-1的酰胺I带的吸收峰和东阿阿胶有9个波数的区别;不同批次和厂家的正品阿胶的红外光谱图更为相似,难以区分开,借助于二维相关红外光谱法,获取了物质的微观结构信息,提高了谱图的分辨率,几种真品阿胶得到了直观有效的鉴别。     

Physicochemical properties of new cellulosic fibers from the bark of Acacia arabica

With the growing environmental consciousness toward carbon emissions, natural fibers are the best alternative and act as a substitute for synthetic fibers due to their potential properties. New cellulosic fibers were identified from Acacia arabica bark. This study aimed at understanding the characteristics of Acacia arabica fibers (AAFs) extracted from the bark of the A. arabica, and its physicochemical properties were examined by thermal stability analyses, X-ray diffraction, chemical constitutions, and Fourier transform infrared spectroscopy analysis. Cellulose content (68.1 wt%), density (1028 kg m^?3), and crystallinity index (51.72%) properties were identified.     

红外光谱法对肉苁蓉径向不同部位的分析与评价

采用傅里叶变换红外光谱、二阶导数谱和二维相关红外光谱技术对肉苁蓉由表及里3个部位的药材粉末及其水提物和醇提物进行了分析与评价研究.结果表明,肉苁蓉不同部位的一维光谱非常相似,三者相似系数分别为0.9605,0.944和0.976;二阶导数谱中峰位和峰强的差异明显.1430～1700 cm-1范围内的二维相关谱中皮部自动峰有3个,而中部及髓部均为4个,更直观的反映出三者的差异.不同部位水提物和醇提物的分析结果进一步明确了肉苁蓉皮部芳香类、环烯醚萜类及糖苷类物质与中部和髓部存在明显不同,而髓部的水溶性多糖、半乳糖醇和苯乙醇苷类物质均高于其它部位.可见红外光谱法结合二维相关红外光谱技术为同种药材不同部位的细微差异分析和评价提供了一种快速、全面和客观的方法和手段.     

傅里叶变换红外光谱对食道癌及相应正常组织的研究

研究了9例食道癌及相应正常组织的红外光谱，从光谱参数（形状、频率、强度等）方面进行了分析。结果表明：癌组织样品与政党组织样品存在明显的光谱上的差异。着重讨论了核酸中磷酸二酯基团（PO2^-)对称和反对称伸缩振动、膜脂中的碳氢基团（CH3，CH2）的伸缩及弯曲振动、蛋白质中C－O基团的伸缩振动峰的变化。从氢键角度以及膜脂碳氢链排列及构象变化角度分析了变化的原因。     

枝晶状Pt 薄膜的制备及其特殊红外效应

采用方波电位, 在10×10^-3 mol·L^-1 K₂PtCl₆+3×10^-4 mol·L^-1 PbAc₂+0.5 mol·L^-1 HClO₄溶液中, 于本体Pt 电极上电沉积制备出枝晶状Pt 薄膜. 随着沉积时间的增加, 枝晶长度逐渐由400 nm增加到900 nm, 且枝晶上的小晶粒(~10 nm大小)变得密集. 根据循环伏安(CV)曲线中氢吸脱附电量可得出Pt 薄膜具有中等粗糙度(C_r=9-36), 且电极表面的粗糙度随着沉积时间增加而增大. 观察到Pt 薄膜上吸附态CO的原位红外光谱具有明显的增强吸收效应, 当沉积时间为6 min 时所制得的枝晶Pt 电极的红外增强效应最大. CO呈现多种谱峰形状, 随着沉积时间的增加, 谱峰形状依次为左高右低的双极峰(类Fano 红外效应), 单极向下(表面增强红外吸收), 左高右低的双极峰, 单极向上(异常红外效应), 左低右高的双极峰和单极向下. 这表明纳米材料薄膜所呈现出的特殊红外性能, 与纳米材料的尺度和聚集状态等密切相关. 所制备的枝晶状Pt 薄膜有望为深入认识纳米材料的特殊红外性能提供一个良好的模型材料.     

Deposition of SiO2-Like Films by HMDSN/O2 Plasmas at Low Pressure in a MMP-DECR Reactor

The effects of process parameters such as O₂/HMDSN (hexamethyldisilazane) ratio, microwave discharge power and deposition pressure on the growth rate, chemical bonding nature, and refractive index of thin films deposited by microwave plasma from HMDSN with oxygen, have been investigated. The plasma was created in a Microwave Multipolar reactor excited by Distributed Electron Cyclotron Resonance. The films were deposited at room temperature and characterized by Fourier Transform Infrared spectroscopy and ellipsometry. Growth rate increased with the discharge power P or the deposition pressure but decreased significantly with increasing O₂/HMDSN ratio. A large change in the film composition was observed when the O₂/HMDSN ratio was varied: films deposited with only HMDSN precursor are polymer-like but as the O₂/HMDSN ratio increased, organic groups decreased. For relative pressure values over 70%, deposited films are SiO₂-like with refractive index values close to those found for thermal silicon dioxide.     

Design and development of pyrolyser to extract medicinal oil from the stem of Ziziphus jujuba

Pyrolysis as an extraction method of phytochemicals from plant parts for medicinal applications is less explored. Practitioners of traditional Indian medicine use a process which is a crude equivalent of pyrolysis, to extract oily substances from stem parts of plants and use them in treatment of various ailments. In this study, a prototype pyrolyser is fabricated to simulate the traditional method and the stem part of Ziziphus jujuba is subjected to pyrolysis using the pyrolyser under controlled conditions. Based on the principle of applied pyrolysis, the engineering design is conceptualized and drawing for a prototype extractor is made. Material selection for the main reactor vessel and the heating system with controller is finalized. The prototype is fabricated. The oily extract obtained is compared with the extract from the traditional method for compositional identity and phyto chemistry to validate the process. The chemical similarities of the extracts from both methods establishes pyrolsis as the basic principle behind the traditional method and this validates the design of the pyrolyser. The FTIR and GC-MS analysis of the extracted oily substance from both methods reveals the presence of various cyclic, nitrogenous, long chain and heterocyclic compounds which are believed to be the pyrolysates of various cyclopeptide alkaloids reportedly present in the stem of Ziziphus jujuba. These phytochemicals have sedative property and are likely to be responsible for the curative nature of the oil used in the treatment of various human disorders and the research substantiates the stem's historical use by traditional practitioners.     

6种燕窝的傅里叶变换红外光谱法原性状快速鉴别

首次利用微钻石ATR探头傅里叶变换红外光谱法（FTIR）无损快速鉴别了6种燕窝。结果表明：印尼燕、越南燕、马来西亚燕、泰国血燕、菲律宾草燕和香港市售燕窝均有自己的红外特征谱,据谱图吸收峰的波数位置和相对峰强度的差异可达到燕窝类同和伪品和鉴别。该方法快速、简便、可靠。     

Synthesis of epoxy monomers that undergo synergistic photopolymerization by a radical‐induced cationic mechanism

A series of novel, cycloaliphatic, cationically photopolymerizable epoxide monomers bearing benzyl ether groups were prepared. These monomers display a considerable enhancement in the rate of their cationic ring‐opening polymerizations in comparison with monomers that do not contain such groups. In this article, a synergistic free‐radical mechanism is proposed that accounts for this effect, and supporting evidence is offered for its verification. During UV irradiation of an onium salt cationic photoinitiator, the aryl radicals that are generated abstract labile benzyl hydrogens present in such monomers to generate the corresponding carbon‐centered radicals. Subsequently, these radicals are oxidized to benzyl carbocations by the onium salt via a nonphotochemical chain process. The observed increase in the rate and extent of the cationic ring‐opening polymerization of the epoxide monomers is due to the aforementioned mechanism, which effectively increases the number of reactive cationic species present during polymerization. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 39: 3578–3592, 2001     

急/慢性粒细胞白血病患者骨髓血细胞的FTIR研究

研究了急性粒细胞白血病（AML）和慢性粒细胞白血病（CML）患者的骨髓淋巴细胞、粒细胞和红细胞的傅立叶红外光谱（FTIR）。结果发现：（1）这三种细胞FTIR存在着差异性。（2）AML与CML之间淋巴细胞和粒细胞的谱图差异性不明显，但红细胞的谱图却存在可识别的差异性。与CML红细胞相比，AML红细胞酰胺Ⅰ带较宽，AML红外细胞蛋白质二级结构中α-螺旋结构的含量较低；1540cm^-1与1084cm^-1吸收峰面积的比值较低，范围较窄，该结果提示，AML和CML骨髓血红细胞中核红细胞的数量分布不同，同时提示骨髓红细胞的成熟可能与白血病细胞的增殖有关。