Proposals of a Procedure for Mass Recovery of Standard Materials: Comparison between Two Electrical Sensing Zone Instruments

Accurate mass balance is an important requirement, especially for mass calibration procedures. It has been observed that with high-resolution apparatus, some volume underestimation, probably due to dead times during channelization, may occur. In this paper, a procedure based on poly(styrene-divinylbenzene) latex standard suspensions is proposed to assess the accuracy of volume measurements. Such a procedure was followed to evaluate the volume measurement accuracy and precision of a Coulter Counter TAII, which is generally considered an accurate counter, and of a Coulter Multisizer II (software 2.1), a high-resolution apparatus. No differences in accuracy and precision were found between the two instruments. Both of them were found suitable for particulate volume measurements provided that an adequate number of replicates is performed.     

A study on the adhesion of anchoring groups to pigment surfaces

A method is described for the comparison of the adhesion of anchoring groups to pigment or filler surfaces, using simple model compounds. Energies of adsorption and the amount of anchoring groups per gram of pigment can be estimated.     

Development and evaluation of an interface for coupled capillary supercritical fluid chromatography/magnetic sector mass spectrometry. Application to thermally unstable and high molecular mass compounds

An interface for coupling supercritical fluid chromatography to a magnetic sector mass spectrometer was developed and evaluated. The interface is based on direct introduction of the mobile phase, carbon dioxide, into the ion-source of the mass spectrometer. The SFC-MS system was optimized with respect to the signal-to-noise ratio. Under optimized conditions, the estimated detection limit for n-pentadecane is approximately 30 ppm. Spectra obtained in the electron-impact ionization mode show a very good similarity with library spectra. The performance of the SFC-MS system was evaluated by the analysis of a number of test mixtures. A sample containing several low molecular mass, thermally unstable compounds, which could neither be analyzed by GC-MS nor by LC-MS, was analyzed. Also for the analysis of high molecular mass compounds, the coupled system showed a good performance.     

Compositional heterogeneity in pectic polysaccharides: NMR studies and statistical analysis

Pectins are a class of heterogeneous polysaccharides used in the food industry as a result of their ability to form gels. They are primarily composed of a (1ŕ4)-α-D-galactopyranosyluronic acid backbone where the carboxylic acid group is methyl esterified at a level which depends on the source of the pectin and processing conditions used to isolate the material. Of considerable interest is the distribution of the free acid and methyl ester groups along this polymer chain. NMR spectroscopy, coupled with statistical analysis, is a powerful technique for the study of sequence distribution of monomers. Experimental conditions (temperature, pD) are reported which are appropriate for the analysis of pectic polysaccharides. Results are presented from a study of sequence distribution in native, modified, and fractionated pectins using ¹H and ¹³C solution NMR methods. The triad sequence information was examined using Bernoullian and Markovian probability models in conjunction with continuous Gaussian distribution and discrete models. Intermolecular heterogeneity in pectins results in triad frequencies which reflect the distribution of acid and ester monomers for native and base saponified pectins. Fractionation of pectin through physicochemical methods and subsequent spectroscopic analysis provide insight into this heterogeneity. Segregation into discrete polymer populations shows a structural diversity best approximated by a 3-component statistical model.     

The effect of composition drift and copolymer microstructure on mechanical bulk properties of styrene-methyl acrylate emulsion copolymers

In order to determine the influence of composition drift and copolymer microstructure on the mechanical bulk properties of styrene -methyl acrylate copolymers, several copolymers were produced by emulsion copolymerization. Three different average compositions were used. By performing the copolymerizations under batch and semicontinuous conditions with two different monomer addition strategies (starved conditions and optimal addition) it was possible to control composition drift and to produce copolymers with different microstructures (chemical composition distributions). All these copolymers were processed in a way that ensured that the original particle structure was lost before the polymers were tested. It was found that composition drift had an influence on the mechanical properties (Young's modulus, maximum stress, elongation at break). This influence could be understood very well on the basis of present knowledge about structure-mechanical properties relationships. In the case of homogeneous copolymers maximum stress and elongation at break are dependent on the molecular weight, and only weakly dependent on the chemical composition, and Young's modulus is independent of chemical composition and molecular weight in the range of compositions investigated, as expected. In the case of heterogeneous copolymers, the influence of copolymer microstructure on Young's modulus, maximum stress and elongation at break is very large. Depending on the extent of control of composition drift during the polymerizations, phase separation was observed in the processed polymers, and the presence of a rubber phase affected the properties profoundly.