溶液酸度在线检测装置的研制

研制了酸度在线检测装置，并应用于溶液酸度在线检测，溶液酸度在线检测装置，设有防污过滤器，自动采样器，蠕动泵，小型管道ｐＨ传感器和控制电路等，其特点为防污除油，随机自动采样，定时检测，全部管道化，可单独使用和计算机控制系统联网，适用于溶液酸在线分析，测定精度〈ｐＨ０．０５。     

Heat-resistant polymers from melt-processable bisimido-bisphthalonitriles

Heat-resistant polymers which are processable into void-free components and suitable for composite applications have been synthesized by thermal/chemical polymerization of four newly developed bisimido-bisphthalonitriles containing silicon, ether, carbonyl, and hexafluoroisopropylidene groups. Thermal polymerization involving addition reactions was performed at 200–275°C for 2–10 h and then post-curing at 310°C for 10 h. Polymers VI, VII, VIII , and IX were obtained. The thermal polymerization was monitored using infrared spectroscopy. Thermal polymerization was also carried out in the presence of an aromatic diamine. A polyhexasocyclane ( V ) was synthesized by condensation polymerization of ether containing bisimido-bisphthalonitrile with 4,4′-diaminodiphenyl ether in solvent phenol. The synthesized polymers were evaluated for thermal stability using dynamic thermogravimetric analysis (TGA). Polymers VII, VIII, IX , and X showed thermal decomposition temperature in the range of 475–500°C in nitrogen and air atmosphere. The char yield of the polymers was in the range of 60–69% in nitrogen at 800°C. This study indicated that synthesized thermosetting polymers from ether and keto containing bisimido-bisphthalo-nitrile are potential candidates for development of graphite composites. © 1993 John Wiley & Sons, Inc.     

Simultaneous measurement of glucose and glutamine in aqueous solutions by near infrared spectroscopy

A method is described for measuring the concentrations of both glucose and glutamine in binary mixtures from near infrared (NIR) absorption spectra. Spectra are collected over the range from 5000–4000/cm (2.0–2.5μm) with a 1-mm optical path length. Glucose absorbance features at 4710, 4400, and 4300/cm and glutamine features at 4700, 4580, and 4390/cm provide the analytical information required for the measurement. Multivariate calibration models are generated by using partial least squares (PLS) regression alone and PLS regression combined with a preprocessing digital Fourier filtering step. The ideal number of PLS factors and spectral range are identified separately for each analyte. In addition, the optimum Fourier filter parameters are established for both compounds. The best overall analytical performance is obtained by combining Fourier filtering and PLS regression. Glucose measurements are established over the concentration range from 1.66–59.91 mM, with a standard error of prediction (SEP) of 0.32 mM and a mean percent error of 1.84%. Glutamine can be measured over the concentration range from 1.10–30.65 mM with a SEP of 0.75 mM and a mean percent error of 6.67%. These results demonstrate the analytical utility of NIR spectroscopy for monitoring glucose and glutamine levels in mammalian and insect cell cultures.     

Far infrared spectra of solid molecular nitrogen

This paper reports the observation of the far infrared absorption spectrum of a single crystal of N₂, measured over absorption paths of 4 cm (lengthwise) and 2 cm (across the crystal). The crystal chamber, with quartz windows, was immersed in a flow of cold helium gas. The spectrum from 20 to 120 cm^–1 was recorded in the liquid phase, the-phase, and over the full temperature range of the-phase (35.6–2.0 K) with a Fourier transform spectrometer. The spectral resolution, which was not instrument-limited, and the large path allowed the observation of more detailed multiphonon-transition structure in the spectrum of the-phase than has previously been observed.     

马来酸酐封端聚碳酸亚丙酯的大分子偶联反应

自从 1 969年井上祥平[1] 发现二氧化碳 (CO2 )可以同环氧化合物直接共聚合成脂肪族聚碳酸酯(APC)以来 ,这一学科领域受到科学家的广泛关注[2～ 8] .这是因为CO2 所产生的温室效应 ,成为使全球变暖的主要因素[9,10 ] .已经确定CO2 使气侯变暖占诸多因素中的 66% .目前大气中CO2 的体积浓度为 345ppmv,由于人类的各类活动每年以 1ppmv的速度递增 .因此 ,降低CO2 排放量已成为全人类共同关注的热点之一 .另一方面 ,CO2 的固定化以及消耗、利用显然是一个应积极鼓励的研究课题 .目前人们已经将CO2 同环氧乙烷 (EO)、环氧丙烷 (PO)、环…     

高频燃烧红外吸收光谱法测定钨钛合金中碳含量

建立高频燃烧红外吸收光谱法测定钨钛合金中碳含量的分析方法。在1980 W分析功率下,称取0.3 g样品,以2.0 g钨锡及0.5 g纯铁混合助熔,用高频红外分析仪测定碳。碳的含量在0.013%~0.050%范围内与红外吸收峰面积线性相关,相关系数为0.9993。碳的测定下限为3.6μg/g,方法检出限为1.08μg/g。该法测定结果的相对标准偏差为2.97%~4.11%(n=8),碳的加标回收率为96.2%~103.1%。该方法能够满足合金中碳含量的分析要求。     

Application of online near infrared spectroscopy to study the kinetics of anionic polymerization of butadiene

Online Fourier-transform near infrared (FT-NIR) spectroscopy in combination with a fiber optic probe was utilized to study the kinetics of the anionic polymerization of butadiene. The conversion of the butadiene to methylene protons in the polymer was monitored in solution polymerization conditions by monitoring the absorbance at 1632 nm. The off-line gel permeation chromatography, GPC, technique was used to validate the online FT-NIR spectroscopy method. Butadiene polymerization kinetics in cyclohexane initiated with n-butyllithium at different initiator concentrations and temperatures was studied. A phenomenological kinetic expression for the anionic polymerization of butadiene in cyclohexane initiated with n-butyllithium was determined. The predictions of the kinetic expression were in agreement with kinetic data reported in the literature.     

Selectivity enhancement of a metal-sensitive flame ionization detector for capillary gas chromatography

A novel modification of a hydrogen-atmosphere flamo ionization detector (HAFID) is presented which attenuates response to hydrocarbon compounds, significantly enhancing selectivity towards organometallic compounds by more than an order of magnitude. Chromatograms of an organometallic compound test mixture and regular leaded gasoline are presented to depict the specificity of the response.     

Development and validation of an analytical methodology for the determination of p,p′-DDT, p,p′-DDE and p,p′-DDD in fish oil pills

An analytical methodology was proposed and validated to be applied to the determination of p,p′-DDT and its metabolites p,p′-DDE and p,p′-DDD in fish oil. The analytical procedure presented in this paper involves a single-step clean up process prior to the analysis. A solution of 1,2,3,4-tetrachloronaphtalene was used as internal standard.The analytical technique used was gas chromatography coupled to an electron capture detector. Details on the validation process are provided.The limits of detection ranged from 2.6 to 4.7 pg μL^− 1. The BCR 598 standard reference material (cod liver oil) was used to evaluate the performance of the methodology with satisfactory recoveries for all the compounds.The analytes were determined in three different fish oil pills sold in Spain as a supplementary vitamin support. The sum of p,p′-DDT and metabolites was from 13.2 to 51.3 ng g^− 1, the dominant compound being p,p′-DDE.     

An Infrared Spectroscopic Study on the Hofmann-diam-type 1,12-Diaminododecanemetal(II) Tetracyanonickelate(II)-aromatic Guest Clathrates: M(H2N(CH2)12NH2)Ni(CN)4ċG(M=Co, Ni or Cd; G = Benzene, Naphthalene, Anthracene, Phenanthrene or Biphenyl)

Three Hofmann-diaminododecane-type clathrates of the form M(1,12-diaminododecane) Ni(CN)₄G (M = Co, Ni or Cd; G = benzene, naphthalene, anthracene, phenanthrene or biphenyl) have been prepared in powder form. The 1,12-diaminododecane molecules in the host lattice permit the inclusion of bulky guest molecules. The spectral features suggest that these compounds are similar in structure to the other Hofmann-diam-type clathrates.