Search results for "Analytical"

Quantitative analysis of broad molecular weight distributions obtained by matrix-assisted laser desorption ionisation-time-of-flight mass spectrometry

1996

In order to quantify the error of matrix-assisted laser desorption ionisation (MALDI) time-of-flight (TOF) mass spectrometry in the determination of broad molecular weight distributions, different mixtures by weight of two poly(methyl methacrylate) standards were prepared. These mixtures, with well-defined bimodal molecular weight distributions were analysed by MALDI-TOF mass spectrometry using different matrices (2,4,6-trihydroxyacetophenone and 2,5-dihydroxybenzoic acid) and different cations (Li+, Na+, K+, Rb+ and Cs+) for doping the analyte. From the MALDI-TOF mass spectrometric data, the weight fractions of the two polymers of all mixtures were determined and compared to the values mea…

Rapid evaluation of oxidised fatty acid concentration in virgin olive oil using Fourier-transform infrared spectroscopy and multiple linear regression

2011

Abstract Fourier-transform infrared spectroscopy (FTIR), followed by multivariate treatment of spectral data, was used to evaluate the oxidised fatty acid (OFA) concentration in virgin olive oil samples characterised by different oxidative status. The entire FTIR spectra (4000–700 cm−1) of oils were divided in 25 wavelength regions. The normalised absorbances of the peak areas within these regions were used as predictors. In order to predict the OFA concentration, multiple linear regression (MLR) models were performed. After a cube root transformation of data, an MLR model constructed using eight predictors was able to predict OFA concentration with an average error of 17%. The main wavelen…

A model for polybutadiene coatings on porous silica

1993

Non-wetting viscous liquids such as oligobutadiene prefer “active” sites such as pores during the process of physisorption. Thus, polybutadiene (PBD) coatings on porous silica do not result in a homogeneous polymer film but in an inhomogeneous loading where the bulk polymer is mainly sited in the pores of the silica. An increasing polymer loading leads to increasingly filled pores instead of a thicker polymer film. We cannot exclude the possibility that most of the surface is covered at least with a thin polymer film since the chromatographic behaviour is relatively good for polypeptides, which are highly susceptible to the silanol groups of silica.

Anisotropic diffusion in etched particle tracks studied by field gradient NMR

1994

Etched particle tracks produced after heavy ion irradiation of polymer foils are used as model systems to test the performance of NMR in a newly developed ultrahigh magnetic field gradient system. The stimulated NMR echo decay of molecules diffusing in the channels, formulated in terms of the self part of the intermediate scattering function, is anisotropic and yields the form factor of the channels.

Synthesis of β-d-mannosides from β-d-glucosides via an intramolecular Sn2 reaction at C-2

1992

Abstract The selective synthesis of β- d -mannosides was achieved by first synthesizing β- d -glucosides that carry a N -phenylcarbamoyl protecting group at O-3. These derivatives were transformed into the corresponding β- d -mannosides by intramolecular nucleophilic substitution with inversion of configuration at C-2, the O -triflyl group being the leaving group. Subsequent intramolecular attack of the neighboring carbamoyl group resulted in the formation of the 2,3-carbonate of the desired β d -mannoside.

2020

Tristriazolotriazines (TTTs) with a threefold alkoxyphenyl substitution were prepared and studied by DSC, polarized optical microscopy (POM) and X-ray scattering. Six pentyloxy chains are sufficient to induce liquid-crystalline behavior in these star-shaped compounds. Thermotropic properties of TTTs with varying substitution patterns and a periphery of linear chains of different lengths, branching in the chain and swallow-tails, are compared. Generally, these disks display broad and stable thermotropic mesophases, with the tangential TTT being superior to the radial isomer. The structure–property relationships of the number of alkyl chains, their position, length and structure were studied.

Voltammetric Identification of Lead(II) and (IV) in Mediaeval Glazes in Abrasion-Modified Carbon Paste and Polymer Film Electrodes. Application to th…

2000

Direct identification of lead(II) and (IV) in glazed ceramics by cyclic voltammetry and differential pulse voltammetry is described. Characteristic cathodic and anodic profiles are obtained for microsample coatings in Paraloid B72-film electrodes immersed in NaCl and HAc/NaAc media. The electrochemical response of PbO, PbO2 and Pb3O4, and a series of test specimens of glaze is compared with that of microsamples extracted from the glaze of blue and white decorated ceramic produced in Manises (Spain) in the 15th century which have been buried in a damp place. Under abrasive conditions, striping peaks at –0.12 and –0.25 V (vs. SCE) appear for Pb(IV) centers and, at –0.55 and –0.75 V, for Pb(II…

Environment Humidity Effect on the Weight of Carbonized Na-Al-Si Glass Fabrics Recovery after Heating

2015

Na-Al-Si glass fabrics fibres contain Na+ ions that diffuse to its surface and along with CO2 and H2O from atmosphere create here the shell of carbonate hydrates. The heating of fabric leads to weight loss by evolving these substances. In this work the results of weight recovery study at room relative humidity (20% – 50%) and elevated humidity (near 70%) of fabrics after its heating at different temperatures (70°C – 150°C) are compared. The experiments shoved the different weight recovery kinetics. The initial exponential stages up to 0.3 h – 0.5 h of the both recoveries are associated with water absorption and differ by its levels. In a case of lower environment humidity the later weight i…

Infrared spectroscopy on lead silicate glass

1993

The reflectance spectra of some lead silicate glasses of general formula (PbO)x(SiO2)y have been measured in the infrared frequency range from 50 to 4000 cm−1. The dispersion and absorption spectra in the range 50–2000 cm−1 have been calculated from the reflectance data using the Kramers-Kronig relations. The band at ∼ 135 cm−1 is assigned to the stretching vibration of lead-oxygen bonds. The shoulder band of the silicon-oxygen stretching mode at ∼900 cm−1 shows a weak coupling of those bonds to the Pb2+ modifier. The vibration strength of those bands shows that the number of the Pb2+ modifier increases first up approximately to 50 Mol% with the increase of PbO content and then decreases ra…

β-Relaxation and low-temperature specific heat in (KBr)1?x(KCN)x

1990

The specific heat in (KBr)1−x(KCN)x has been measured for concentrations 0.00≦x≦0.93 and for temperatures 2 K≦T≦50 K. In addition, the dipolar relaxation phenomena were studied using dielectric spectroscopy. The relaxation behaviour was parametrized assuming a Gaussian distribution of energy barriers and the mean activation energies, the distribution widths, and the attempt frequencies have been determined as a function of the CN− concentration. With these parameters the linear and the excess specific heat contributions were calculated and compared to the calorimetric results.