杂多蓝质子化点位的新证据──现场光透薄层FTIR光谱电化学的研究结果

杂多阴离子在质子介质中的电还原行为已有大量报道“,“,已经证明杂多阴离子在还原后有质子化的过程发生,然而仅能从理论上推断质子化发生在桥氧上,尽管中子衍射可确定结晶中的质子位置,但是该方法太复杂,并且无法在溶液中进行现场研究．本文以现场FTIR光谱电化学方法对杂多阴离子PMO;刀X在质子介质中的电还原行为进行了研究,给出了杂多蓝质子化发生在桥氧上的新证据．考虑到红外光谱电化学方法中使用NaCI盐窗的要求和水溶液的强吸收等问题,我们选用经高氯酸酸化的乙脂溶液作为研究体系．1实验部分按文献［’1方法制备TBAsP…     

钯-氧化石墨烯-Fe3O4催化剂的制备及其对Heck反应催化研究

采用离子交换和共沉淀两步法合成了氧化石墨烯-四氧化三铁复合物（GO—Fe3O4）,并负载钯（Pd）纳米颗粒得到了催化剂Pd—GO—Fe3O4．用SEM和FTIR对其表面形貌和组成进行了表征．160℃下,以N,N-二甲基甲酰胺（DMF）为溶剂,将该催化剂用于溴苯和丙烯酸酯的Heck偶合反应中,产率可达98．6％,且连续使用4次后,产率仍可保持97．51％．     

大孔径液晶毛细管柱GC/FTIR联用的研究EPMB液晶毛细管柱与Nicolet 5-SXCFTIR联用

本文研究了EPMB液晶大孔径毛细管柱与短光管FTIR的联用。实验表明,大孔径毛细管柱与短光管FTIR是完全匹配的,在光管尾吹量为零时,系统可获得最佳分辨。大孔径液晶毛细管柱对芳烃异构体的选择性高,柱容量和载气流量大,因而,特别适用于与FTIR联用分离鉴定芳烃异构体。本文使用的高温液晶EPMB大孔径毛细管柱,能在较低柱温下工作,与FTIR联用成功地分离鉴定了一些单环、双环、三环及四环的芳烃异构体。     

聚丁二酸丁二酯/纳米高岭土共混体系结晶及力学性能研究

用熔融共混法制备聚丁二酸丁二酯(PBS)/纳米高岭土(nano kaolin)复合降解材料,利用FTIR、DSC、万能拉力机和SEM对其微观结构、结晶、力学性能及分散性进行研究.FTIR光谱分析结果表明,改性剂与nano kaolin发生了化学键合作用;DSC结果表明,在PBS中加入nano kaolin,提高了结晶起...     

一种不含β-氢的苯并噁嗪的表征分析及催化固化研究

以邻烯丙基双酚A、多聚甲醛和烯丙基胺为原料，采用无溶剂的方法合成了一种不含β-氢的苯并噁嗪(2，2-二(3，8-二烯丙基-3，4-二氢-2H-1，3-苯并噁嗪)-丙烷(B—dbo)．GPC和元素分析结果表明，此噁嗪中间体主要是单量体和二聚体．用FTIR和^1H NMR对中间体结构进行了表征．结果表明，此苯并噁嗪的分子结构中存在三种反应官能团：噁嗪环、N-烯丙基、Ar-烯丙基．用DSC和FTIR研究三种反应基团在固化时的反应情况．将双酚A、邻烯丙基双酚A、TiCl4和PCl5作为催化剂按适量的比例加入B—dbo中，用DSC研究其固化行为，并对TiCl4催化试样在不同的固化温度下进行FTIR测试分析，提出在TiCl4催化下苯并噁嗪环副反应及开环固化机理．     

等价组态光谱项速算法

原子光谱项对研究原子结构和原子光谱具有重要地位,在原子物理学,量子化学,结构化学和配位化学等书中都有一定的阐述。其中求取等价组态光谱项是一大难点,如“电子排布法”、“逐级消去法”、“行列式波函数法”是常用方法,但是,若求出较复杂组态的光谱项(如具有成百上千种微状态的谱项),这些方法很繁琐以致在实际中无法使用;对“Slater 图解法”、     

pH值和离子强度对放射性核素镍在MX-80黏土上的吸附影响和模型研究

利用酸碱滴定、XRD和FTIR对MX-80黏土进行了详细的表征和分析．用静态法研究了离子强度、固相浓度和pH值对放射性核素^63Ni（Ⅱ）在MX-80黏土上的吸附,并用扩散模型（diffuse layer model（DLM））和FITEQL 3．1软件对吸附数据进行模型拟合研究．研究结果表明,放射性核素^63Ni（Ⅱ）在MX-80黏土上的吸附主要受表面络合作用,在低pH条件下离子交换作用也起一定的影响．利用Langmuir和Freundlich模型对吸附等温线进行拟合研究,表明Freundlich模型可以更好的拟合放射性核素^63Ni（Ⅱ）在MX-80黏土的吸附．研究结果对于评估放射性核素^63Ni（Ⅱ）在作为填充材料的MX-80黏土中的吸附和迁移具有重要的意义．     

化合物分子表面积计算方法的研究

化合物的分子表面积是重要的物理化学性质参数．根据不同的应用领域及数学方法,提出了多种分子表面积算法[1-10],由此产生了“分子表面积法”,各方法的有效性在各具体应用领域都已被验证．本文将统计方法中的随机变量引入计算化合物分子表面积体系,由分子模型化技术得到化合物分子的原子坐标,不考虑化合物分子中原子的相互作用及分子间近似,直接计算分子表面积．使用该方法可以计算“净”分子表面积、“溶剂可及表面积”、甚至分子结构片段,分子结构中有交叉重叠片段及存在“空洞”的各种分子表面积,该算法及程序较简捷,适应范围广,计算结果较为满意．     

变径毛细管柱GC／FTIR联用技术的研究

本文介绍了使用新型变径毛细管柱的气相色谱/傅里叶变换红外光谱联用技术(GC/FTIR)。以正构烷烃的混合物为样品,研究了载气速流、色谱进样量及柱后死体积对联用效果的影响。分别在变径毛细管柱GC/FTIR和普通毛细管柱GC/FTIR联用系统上分析了烷烃芳烃混合物和合成汽油样品,并利用软件系统提供的程序和红外标准谱库对所得光谱进行了检索。实验结果表明,变径毛细管柱GC/FTIR系统具有色谱进样量大,可鉴定组分多,分离能力强和检测灵敏度高等显著优点。     

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。     

Noninvasive biochemical monitoring of physiological stress by Fourier transform infrared saliva spectroscopy

Physical stress affects the immune system, activates the sympathetic (SNS) and parasympathetic (PNS) subsystems of autonomic nervous system (ANS), and increases the activity of the hypothalamic-pituitary-adrenal axis (HPA). The specific response of the major regulatory systems depends on the human functional state. Saliva is a unique diagnostic fluid, the composition of which immediately reflects the SNS, PNS, HPA and immune system response to stress. A new method of saliva biomarker determination by Attenuated Total Reflection Fourier-Transform Infrared (ATR FTIR) spectroscopy has been developed to monitor the exercise induced metabolic changes in saliva from male endurance athletes. The method has been tested using a group of professional athletes by analysing saliva samples collected before and after the exercise, and the saliva composition monitoring by ATR FTIR spectroscopy was shown to be suitable for real-time checking of response to stress.     

Hyphenation of Curie-point-pyrolysis high-resolution gas chromatography with several spectroscopic methods for the analysis of cured epoxy resins

The coupling of Curie-point pyrolysis (Py) with gas chromatography (GC) and mass spectrometry (MS) or Fourier transform infrared spectroscopy (FTIR) has been widely reported. The approach reported in this paper combines chromatographic separation with eluent monitoring by use of three different spectroscopic detectors (MS, FTIR and Atomic Emission Detector [AED]). The features of these detectors, with different selectivities, are shown for the analysis of cured epoxy resins. Besides characterisation of major resin constituents by identification of the pyrolysis products, the usefulness of the AED is also revealed by the detection of minor compounds (such as coupling agents) in cured epoxy resins.     

A fiber-optic sensor system for monitoring chlorinated hydrocarbon pollutants

We have developed and field-tested a fiber-optic chemical sensor system for use in environmental monitoring and remediation. The system detects chlorinated hydrocarbon pollutants with colorimetry, and is based on an irreversible chemical reaction between the target compound and a specific reagent. The reaction products are detected by their absorption at 560 nm and can be monitored remotely with optical fibers. Continuous measurements are made possible by renewing the reagent from a reservoir with a miniature pumping system. The sensor has been evaluated against gas chromatography standards and has demonstrated accuracy and sensitivity (5 ppbw) sufficient for the environmental monitoring of trichloroethylene and chloroform. Successful preliminary field tests have been conducted in a variety of contamination monitoring scenarios.     

In-vitro assays for determination of oestrogenic activity

At present, in-vitro bioassays are predominantly being seen as tools to identify, through screening programs, whether or not individual chemical compounds have an effect on the endocrine system. However, as the techniques mature, they are likely to find use in the future in monitoring of discharges to the environment for any biological effect and will compliment the range of chemical and biological techniques also available for monitoring environmental quality. Such an approach has already been utilised by a number of workers to fractionate mixtures (e.g. final effluents from STW), to isolate the oestrogenically active components and subsequently identify the compounds which are active. This paper reviews the present state of in-vitro techniques for determination of oestrogenic activity and discusses present approaches to their use in environmental monitoring in conjunction with chemical analyses in toxicity identification and evaluation.     

Fourier transform infrared imaging for high-throughput analysis of pharmaceutical formulations

Fourier transform infrared (FTIR) spectroscopic imaging with infrared array detectors has recently emerged as a powerful materials characterization tool. We report a novel application of FTIR imaging for high-throughput analysis of materials under controlled environment. This approach combines the use of spectroscopic imaging with an attenuated total reflection (ATR)-IR cell, microdroplet sample deposition system, and a device that controls humidity inside the cell. By this approach, it was possible to obtain "chemical snapshots" from a spatially defined array of many different polymer/drug formulations (more than 100) under identical conditions. This method provides direct measurement of materials properties for high-throughput formulation design and optimization. Simultaneous response (water sorption, crystallization, etc.) of the array of formulations to the environmental parameters was studied. Implications of the presented approach range from studies of smart polymeric materials and sensors to screening of pharmaceuticals and biomaterials.     

Compositional dynamics of a commercial wine fermentation using two-dimensional FTIR correlation analysis

We have demonstrated that compositional changes occurring during a commercial red wine fermentation can be effectively monitored using FTIR spectroscopy and modelled with the aid of two-dimensional correlation techniques. This study represents a novel application of two-dimensional spectroscopy and showed that the reaction rates for the conversion of fructose and glucose to alcohol were different, with the latter being more rapid. The use of a simple three-component model serves to aid interpretation of the data and the results obtained confirm the value of two-dimensional FTIR correlation spectroscopy as a chemometric tool which has considerable potential for process monitoring.     

导电高聚物聚2，5－二甲基苯胺的化学合成与特性

报道了聚２，５－二甲基苯胺（ＰＤＭｅＡｎ）的化学合成，并用标准四探针方法测定其电导率，以ＦＴＩＲ、ＵＶ－Ｖｉｓ吸收光谱、元素分析和ＣＶ法对其性质进行了研究，ＰＤＭｅＡｎ的结构与聚苯胺和聚２，５－二甲氧基苯胺的结构类似，是由其单元通过氮原子（Ｎ）在对位上键合而成，本征态的ＰＤＭｅＡｎ能溶于多种有机溶剂，如ＣＨ２Ｃｌ２、ＣＨＣｌ３、ＤＭＳＯ、ＤＭＦ等。     

Photoionization Detector for Portable Rapid GC

With the development of portable rapid gas chromatography (GC) for environmental monitoring the photoionization detector (PID) has potential application. The frequent calibration required and the relatively large dead volume have limited the use of the PID, however. An improved PID which resolves these problems is proposed in this paper. Compared with a commercial instrument, signal generation, the main aspect of the improved PID, has also been optimized. In the improved PID the sample is directed to flow across the lamp window, rather than toward the lamp, and a new, simple automatic self-cleaning technique, which effectively eliminates contaminants and substantially reduces drift, has also been adopted. Use of new electrodes has effectively reduced the background noise and dead volume of the PID. As a result of this new design the PID should be more compatible with rapid portable GC in environmental monitoring, because of elimination of most of the tedious cleaning and calibration previously necessary.     

Exploration of biomass waste as low cost adsorbents for removal of methylene blue dye: A review

Biomass waste, which is abundantly available has been studied as low cost biosorbent for dye sequestration from waste water. The present review reports on recent development for remediation of methylene blue dye by agricultural waste and fruit peel waste material. The aim of this study was to revise latest literature in the field of dye adsorption and discuss the dye adsorption capacity of different types of adsorbents. The activated carbon prepared from several types of biomass waste material enhances the adsorption efficiency after modification. The variety of activating agents, method of activation, characterization of biosorbent material like SEM, EDAX, BET surface area and FTIR analysis has been explored in the present review. The dye adsorption factors such as effect of pH, agitation time, temperature, adsorbate and adsorbent dose were discussed. The detailed investigation on applicability of isotherm model, kinetic model and thermodynamic parameters has also been presented. The adsorption kinetics and adsorption isotherm model focus on selectivity of adsorbent. Adsorption mechanism, Influence of surface area, influence of pH_pzc and comparative study of biomass waste adsorbent with other adsorbents have been carried out. The use of biomass waste adsorbents is economically feasible, environmental healthy and found to have outstanding removal capacity of dyes.     

Development of graphene-carbon nanotube-coated magnetic nanocomposite as an efficient sorbent for HPLC determination of organophosphorus pesticides in environmental water samples

A magnetic solid-phase extraction (MSPE) method coupled to high performance liquid chromatography with UV (HPLC-UV) was proposed for the determination of organophosphorus pesticides (OPPs) at trace levels in environmental water samples. The ternary nanocomposite of graphene-carbon nanotube-Fe₃O₄ (G-CNT-Fe₃O₄) has been synthesised via a simple solvothermal process and the resultant material was characterised by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy. Significant factors that affect the extraction efficiency, such as amount of magnetic nanocomposite, extraction time, ionic strength, solution pH and desorption conditions were carefully investigated. The results demonstrated that the proposed method had a wide dynamic linear range (0.005–200 ng mL^?1), good linearity (R² = 0.9955–0.9996) and low detection limits (1.4–11 pg mL^?1). High enrichment factors were achieved ranging from 930 to 1510. The results show that the developed method is suitable for trace level monitoring of OPPs in environmental water samples.