简易型离子选择电极-流动注射分析仪的研制及卤水中氯、溴和碘的连续测定

本文设计研制了简单实用的流通池,组装了简易型离子选择电极—流动注射分析仪,对体系的分析特点和影响因素进行了考察。此装置性能可靠,能满足简单流注分析的需要,并建立了卤水中Cl~-、Br~-和I~-的连续测定方法。     

Chemical and thermal analysis of the biopolymers in thyme (Thymus vulgaris)

Thyme (Thymus vulgaris) has been known, long time ago, for its aromatic properties. It contains essential oils and polymers such as cellulose (mixture of hemicellulose and cellulose) and lignin. The thyme, studied in this work, was gathered from the same place, in the period from November 1999 to October 2000. The chemical analysis (water, total ash, essential oils, extractive substances, cellulose, holocellulose and lignin) can be used roughly in the characterisation of the four periods that correspond to the four seasons of the year. The cellulose level was found to be more than lignin level in the wet periods (growth of the plant). The opposite was found in the dry periods. The total ash and essential oil levels were found to be high during the period of high pluviometry. The thermal decomposition of cellulose and holocellulose was found to fit well with the first-order kinetics. The activation energy, under air flow, was 185 and 196 kJ mol⁻¹ for cellulose and holocellulose, respectively. The maximum decomposition rate and thermal analysis heating rate of lignin were found to have a direct linear relationship.     

Spectrophotometric determination of Fe(II) in milligram solid samples

The analytical procedure of determination of Fe(II) in the presence of Fe(III) in milligram samples is proposed. A solid sample is dissolved in hydrochloric acid in argon atmosphere. Subsequently, the pH-value of the solution is fixed and Fe(III) complexed by phosphoric buffer. At the next step Fe(II) is oxidized by -molybdosilicic acid. Finally, the intensity of colouring caused by the reduced form of the acid is measured at the wavelength 770 nm. The proper treatment of the sample during oxidation, and immediately before, is decisive for the accuracy of the analysis. The method was verified by means of the analysis of synthetic magnetite. The theoretical content of Fe(II) was 24.12%, the determined one was 24.02 ± 0.10%. The method was applied to the determination of the homogeneity of an iron catalyst for ammonia synthesis.     

Analysis of grid file algorithms

Grid file algorithms were suggested in [12] to provide multi-key access to records in a dynamically growing file. We specify here two algorithms and derive the average sizes of the corresponding directories. We provide an asymptotic analysis. The growth of the indexes appears to be non-linear for uniform distributions:O(v ^c ) orO(v ), wherec=1+b^–1, =1+(s-1)/(sb+1),s is the number of attributes being used,v the file size, andb the page capacity of the system. Finally we give corresponding results for biased distributions and compare transient phases.     

Sensitivity of sample values to parameter changes

The effect of small changes in parameter values on the sample values is investigated further. The concept of linearity with respect to parameters is introduced, and the linear and the nonlinear cases are treated separately. The relation with the sample-path analysis is discussed.     

Electron radiation effects on the structure of ultradisperse polytetrafluoroethylene

Electron radiation effects (40 mrad, 70 mrad, and 100 mrad) on the molecular and supramolecular structure and morphology of ultradisperse polytetrafluoroethylene obtained by the thermogas dynamic (TGD) method were studied by IR and EPR spectroscopy, X-ray phase analysis, and atomic force microscopy. Irradiation of ultradisperse powder in air leads to oxidized polymer forms due to the terminal carbonyl groups and stable peroxide radicals that appear in the structure. Fast electron radiation in doses of up to 100 mrad did not change the polymer crystallinity and particle entity, while thin films on the surface of ultradisperse polytetrafluoroethylene powder decomposed.     

Thermoanalytische Charakterisierung Strahlengehärteter Polymerfilme

Thermo-oxidative and thermo-mechanical stabilities of radiation-cured acrylates and epoxides were examined by TG, DMA and DSC.The polymeric trifunctional acrylates PETIA, TMPTA and THEIC displayed the highest temperatures of onset of degradation. The high crosslinking density of the films resulted in an almost temperature-independent complex E-modulus, as measured by DMA. With increasing degree of ethoxylation or propoxylation of the monomers, decreases in thermal stability and strength were found. For difunctional polymeric acrylates and epoxides, the glass transition temperature was measured.The average degree of curing of UV-cured epoxy films can be determined from the temperature of the maximum in the loss modulus (E_max.This revised version was published online in November 2005 with corrections to the Cover Date.     

纳米氧化锆的物相与尺寸效应

用溶胶凝胶法制得ＺｒＯ２粉体。通过控制晶体尺寸得到了室温下稳定的立方相、四方相和单斜相。用Ｘ射线衍射（ＸＲＤ）、透射电镜（ＴＥＭ）、激光拉曼谱（ＬＲＳ）、电子顺磁共振（ＥＳＲ）等技术研究了晶体结构和晶粒尺寸的相互关系。试验表明：单斜相、四方相、立方相ＺｒＯ２的比表面能依次递减。因而，当晶粒尺寸减小至纳米级时，四方相和立方相都可变为室温下的稳态或亚稳态。     

Correction procedure for the electron microprobe analysis of porous materials

A correction method is proposed for the quantitative determination of stoichiometric ratios in porous materials by electron microprobe analysis. Analysis of this kind of material is complicated by an imperfect surface that can only be improved to some extent. The correction is based on a linear dependence (different for each element) of the analyses on a sum of weight concentrations of oxides. With this correction it is possible to use analyses affected by the imperfection of the surface with much better confidence compared to common normalisation. An example is presented for a series of ceramic superconductors Bi_2.1(SrCa)_2.9Cu₂O₈₊.