New aspects in cationization of lignocellulose materials. VII. Modification of spruce wood meal with quarternary ammonium groups

Trimethylammonium-2-hydroxypropyl (TMAHP) derivatives of spruce wood meal (SWM) and holocellulose of this specia were prepared by the reaction of wood meal with 3-chlor-2-hydroxy-propyltrimethylammoniumchloride (CHMAC) in alkaline medium. The TMAHP samples were fractionated and yields and exchange capacity (Q) of individual fractions were compared with beech and aspen fractions obtained under the same conditions. As it is evident from ¹³C-NMR spectroscopy and GPC analysis the water soluble fraction from TMAHP–SWM consists only of lignin–saccharide degradation products. The NaOH extracts of TMAHP–SWM and TMAHP–holocellulose as well as the water-soluble fraction from TMAHP–holocellulose are polymeric materials. From TMAHP–SWM only 3.1% of alkali-soluble material could be extracted, while from TMAHP–holocellulose 15.7% of water-soluble and 7.9% of alkali-soluble materials were obtained.     

Nonterminal unsaturated silane coupling agents for mineral-filled ethylene–propylene rubber

This paper describes the results of an experimental investigation concerning the effect of reactive organofunctional unsaturated silanes on mechanical properties of mineral-filled ethylene–propylene elastomers. The tested group of the unsaturated silanes was prepared by hydrosilylation syntheses. The experimental silanes, 2,6-octadienyltriethoxysilane, cis-2-butenyltriethoxysilane, 2-(3-cyclohexenylethyl)triethoxysilane, and 2-(3-cyclohexenylethyl)methyldiethoxysilane, led to a considerable improvement in mechanical and electrical properties of mineral-filled vulcanizates based on peroxide-cured ethylene–propylene elastomers. From the tested silanes, the 3-cyclohexenylethylsilanes impart an improvement comparable with the action of vinyltris(2-methoxyethoxy)silane, presently used as a standard coupling agent in mineral-filled peroxide-cured elastomers.     

Reactive polymers,XXXVII. An investigation of the internal structure of polymeric sorbents based on poly(2,3-epoxypropyl methacrylate-co-ethylene dimethacrylate)

The internal structure of polymeric sorbents based on 2,3-epoxypropyl methacrylateethylene dimethacrylate was investigated by means of mercury porosimetry and by employing the sorption method. The results were confronted with characteristic chromatographic data and helped to elucidate the relationships existing between the internal structure of copolymers and their chromatographic properties.     

Determination of phosphorus-, copper-, and zinc-containing human brain proteins by LA-ICPMS and MALDI-FTICR-MS

Human brain proteins containing phosphorus, copper, and zinc were detected directly in protein spots in gels of a human brain sample after separation by two-dimensional gel electrophoresis using laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS). A powerful laser ablation system with cooled laser ablation chamber was coupled to a double-focusing sector field ICPMS. The separated protein spots in 2D gels were fast screened using the optimized microanalytical LA-ICPMS technique measured at medium mass resolution with a focused laser beam (wavelength, 213 nm; diameter of laser crater, 50 mum; and laser power density, 3 x 10(9) W cm(-2)) with respect to selected three essential elements. Of 176 protein spots in 2D gel from a human brain sample, phosphorus, copper, and zinc were detected in 31, 43, and 49 protein spots, respectively. For the first time, uranium as a naturally occurring radioactive element was found in 20 selected protein spots. The detection limits for P, S, Cu, Zn and U were determined in singular protein spots with 0.0013, 1.29, 0.029, 0.063, and 0.000 01 mg g(-1), respectively. A combination of LA-ICPMS with matrix-assisted laser desorption/ionization Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FTICR-MS) was applied for the identification of selected protein spots from human brain protein separated by 2D gel electrophoresis. Combining MALDI-FTICR-MS for the structure analysis of metal- and phosphorus-containing human brain proteins with LA-ICPMS, the direct analysis of heteroelements on separated proteins in 2D gels can be performed. For quantification of analytical LA-ICPMS data, the number of sulfur atoms per protein (and following the sulfur concentration) determined by MALDI-FTICR-MS was used for internal standardization. From the known sulfur concentration in protein, the concentration of other heteroelements was calculated. In addition, the number of phosphorylation and the phosphorylation sites of phosphorylated proteins in the human brain sample detected by LA-ICPMS were determined by MALDI-FTICR-MS. This technique allows the study of posttranslational modifications in human brain proteins.     

Latex-coated polymeric monolithic ion-exchange stationary phases. 1. Anion-exchange capillary electrochromatography and in-line sample preconcentration in capillary electrophoresis

A sulfonated methacrylate monolithic polymer has been synthesized inside fused-silica capillaries of diameters 50-533-microm i.d. and coated with 65-nm-diameter fully functionalized quaternary ammonium latex particles (AS18, Dionex Corp.) to form an anion-exchange stationary phase. This stationary phase was used for ion-exchange capillary electrochromatography of inorganic anions in a 75-microm-i.d. capillary with Tris/perchlorate electrolyte and direct UV detection at 195 nm. Seven inorganic anions (bromide, nitrate, iodide, iodate, bromate, thiocyanate, chromate) could be separated over a period of 90 s, and the elution order indicated that both ion exchange and electrophoresis contributed to the separation mechanism. Separation efficiencies of up to 1.66 x 10(5) plates m(-1) were achieved, and the monoliths were stable under pressures of up to 62 MPa. Another latex-coated monolith in a 250-microm-i.d. capillary was used for in-line preconcentration by coupling it to a separation capillary in which the EOF had been reversed using a coating of either a cationic polymer or cationic latex particles. Several capillary volumes of sample were loaded onto the preconcentration monolith, and the analytes (inorganic anions) were then eluted from the monolith with a transient isotachophoretic gradient before being separated by electrophoresis in the separation capillary. Linear calibration curves were obtained for aqueous mixtures of bromide, nitrite, nitrate, and iodide. Recoveries of all analytes except iodide were reduced significantly when the sample matrix contained high levels of chloride. The preconcentration method was applied to the determination of iodide in open ocean water and provided a limit of detection of 75 pM (9.5 ng/L) calculated at a signal-to-noise ratio of 3. The relative standard deviation for migration time and peak area for iodide were 1.1 and 2.7%, respectively (n = 6). Iodide was eluted as an efficient peak, yielding a separation efficiency of 5.13 x 10(7) plates m(-1). This focusing was reproducible for repeated analyses of seawater.     

Extrahierbarkeit der Organozinnstabilisatoren aus Hart-Polyvinylehlorid-Folien

Zusammenfassung Wegen der biologischen Aktivität von Organozinnverbindungen, die als Stabilisatoren für PVC-Mischungen verwendet werden, und ihrer bewiesenen Auslaugung aus Folien scheint es erforderlich, deren Anwendung in der Lebensmittelindustrie einzuschränken. Ein endgültiges Ergebnis kann erst nach Abschluß der biologischen Versuche gefällt werden.Sollte ein Organozinnstabilisator untoxisch sein, so kann seine Verwendung erst dann erwogen werden, wenn eine verläßliche Methode seiner Erfassung im Kunststoff ausgearbeitet ist, d. h. eine Methode für die Bestimmung des organischen Radikals und nicht nur für die Bestimmung des Zinns.     

Detection of lead in Zea mays by dual‐energy X‐ray microtomography at the SYRMEP beamline of the ELETTRA synchrotron and by atomic absorption spectroscopy

This study is related to the application of the X‐ray dual‐energy microradiography technique together with the atomic absorption spectroscopy (AAS) for the detection of lead on Zea mays stem, ear, root, and leaf samples. To highlight the places with lead intake, the planar radiographs taken with monochromatic X‐ray radiation in absorption regime with photon energy below and above the absorption edge of a given chemical element, respectively, are analyzed and processed. To recognize the biological structures involved in the intake, the dual‐energy images with the lead signal have been compared with the optical images of the same Z. mays stem. The ear, stem, root, and leaf samples have also been analyzed with the AAS technique to measure the exact amount of the hyperaccumulated lead. The AAS measurement revealed that the highest intake occurred in the roots while the lowest in the maize ears and in the leaf. It seems there is a particular mechanism that protects the seeds and the leaves in the intake process. Microsc. Res. Tech., 2010. © 2009 Wiley‐Liss, Inc. This article was published online on 1 December 2009. An error was subsequently identified. This notice is included in the online and print version to indicate that both have been corrected 19 February 2010.     

Wear Behavior of Composites Based on ZA-27 Alloy Reinforced by Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Particles Under Dry Sliding Condition

In present study, the effect of Al₂O₃ particle reinforcement on the sliding behavior of ZA-27 alloy composites was investigated. The composites with 3, 5, and 10 wt% of Al₂O₃ particles were produced by the compocasting procedure. Tribological properties of unreinforced alloy and composite were studied, using block-on-disk tribometer under unlubricated sliding conditions at different specific loads and sliding speeds. The worn surfaces of samples were examined by the scanning electron microscopy (SEM). The test results revealed that those composite specimens exhibited significantly lower wear rate than the ZA-27 matrix alloy specimens in all combinations of applied loads and sliding speeds. The difference in the wear resistance of composite with respect to the matrix alloy, increased with the increase of the applied load/sliding speed and Al₂O₃ particle content. The highest degree of improvement of the ZA-27 alloy tribological behavior corresponded with change of the Al₂O₃ particles content from 3 to 5 wt%. At low sliding speed, moderate lower wear rate of the composites over that of the matrix alloy was noticed. This has been attributed to micro cracking tendency of the composites. Significantly reduced wear rate, experienced by the composite over that of the matrix alloy at the higher sliding speeds and loads, could be explained due to enhanced compatibility of matrix alloy with dispersoid phase and greater thermal stability of the composite in view of the presence of the dispersoid. Level of wear rate of tested ZA-27/Al₂O₃ samples pointed to the process of mild wear, which was primarily controlled by the formation and destruction of mechanical mixed layers (MMLs).