ALBERT

Notes: Summary A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC systems to enable the determination of microcontaminants at the 0.02–1 μg L−1 level in 7–50 mL of aqueous sample. The screening was limited to compounds present in at least one heteroatom-selective GC-AED trace above a predetermined concentration level. These compounds were identified by their partial formulae (AED) and the corresponding mass spectra, which were obtained from the GC-MS chromatogram via the retention index concept. The potential of the approach was demonstrated by the identification of target compounds as well as all unknowns present in tap and waste water above the predetermined threshold of 0.05 μg L−1 (tap water) or 0.5 μg L−1 (waste water).

Notes: Summary An on-line, solid-phase extraction gas chromatography atomic-emission detection (SPE-GC-AED) system has been set up using an on-column interface to transfer 100 μl of desorbing solvent to the GC part of the system. Analytical characteristics such as recovery, precision and linearity of calibration plots were comparable with those of the off-line combination of SPE-GC-AED using organophosphorus pesticides as test compounds. The fully on-line set-up causes a marked improvement in detection because of the quantitative transfer of the analytes from the SPE module to the GC: detection limits are as low as 5–20 ng l−1 for the analysis of 10 ml raw and spiked surface water samples using the phosphorus channel. Detection levels can be further enhanced by processing up to 100 ml samples. The integrated analytical system is robust. The potential of the on-line set up has been demonstrated for the analysis of surface water and waste water.

Notes: One of the basic prerequisites for rational and high quality production of plastic parts is a tool layout tailored to the production process. To date, both design and construction have generally been based on values acquired by experience. This first, necessitates highly qualified personnel and second, involves what is frequently time consuming and costly finishing work. Experience acquired so far with computer-aided layout of injection molds shows that even a designer with little experience reaches the target more quickly and more reliably. At the same time he is able to draw on the results of intricate calculation and simulation methods which he was unable to apply in the past for reasons of time alone. This paper thus sets out the possibilities currently open and the experience available for computer-aided mold layout. The chief point of focus here is a system for the layout of injection molds. Working on from this system, however, the potentials for computer application are presented for blow mold- and foaming mold-design. After finding the mold principle, mold layout essentially divides up into two major areas, namely dimensioning calculations (CAE) and compilation of production documents (CAD). In dimensioning, the different functional elements of the mold are calculated. The aids that have been developed and the potentials of computer-aided dimensioning are presented with examples from the fields of rheological, thermal, and mechanical mold layout. Computer-aided rheological layout divides up into two steps. The first gives information on qualitative filling behavior (filling picture, flow paths) and the second provides quantitative results (pressures, shear stresses, temperatures). Computer-aided thermal layout similarly divides up into part steps. These are a rough overall energy balance, a rough layout of the tempering system, a segmented layout, and a homogeneity check, which involves simulating the temperature conditions in the mold by means of difference methods. When it comes to mechanical layout of the mold, programs are available for deformation calculations on basic cases and these will frequently be sufficient. For more complex cases of loading and deformation, a finite element program is used. Graphic data processing units can be used to supply extra facilities - first, to provide an aid for the simulation programs in dimensioning and second, to rationalize the compilation of the production documents. An illustration of a CAD workplace is given, incorporating the necessary computer configuration and peripherals. Compiling production documents is essentially a problem of variant design. The variants in this case are the individual components of the mold and a number of standardized accessories that can be called up as “standardized components.” The mold cavity, however, always has to be a free design. All programs are dialogue driven and are in a standardized manner so that even designers with no data processing experience can use the computer as an aid. The CAD/CAE system presented duly fulfils all these requirements. It allows the designer, at a single computer work station, to carry out both simulation and dimensioning calculations, to obtain information on material data, and to compile production documents on the basis of variant and free design. This provides the designer with a readily manageable aid and makes a considerable contribution towards improving the design result. Finally, the capacity of different computer concepts and the CAE/CAD/CAM systems on the market are discussed. For the future it will be possible to establish a computer-aided link between the different areas of design, from development of the molded part, via mold design and production, through setting the processing parameters of the injection molding machine.

Notes: Summary A method is described for the rapid catalytic hydrolysis of phenylurea herbicides on silica gel at elevated temperatures. After derivatisation of the anilines produced with heptafluorobutyric acid anhydride final analysis is done on a gas chromatograph equipped with an electroncapture detector. Detection limits are in the 1–5 picogram range. The method has successfully been applied to residue analysis of water samples at the 1 ppb level. The determination of free anilines present in water samples and the potential of various techniques to be used to discriminate between free anilines and parent herbicides are also discussed.

Notes: Summary Phosphine, alkylated phosphines and monophosphinate esters are detected with high sensitivity in capillary gas chromatography (GC) by their chemiluminescent reactions with molecular fluorine. Detection limits are estimated to be 1.3 pg, 0.5 pg, 8 pg, and 17 pg for phosphine, trimethyl phosphine, trimethyl phosphinate ester, and triethyl phosphine, respectively. As found earlier with alkylated sulfur, selenium and tellurium compounds, the detector exhibits a linear response. For triethyl phosphine, a linear range of greater than three orders of magnitude was demonstrated. Emission spectra were obtained for the trimethyl phosphine and triethyl phosphine systems. Chemiluminescence emitters include electronically excited HCF, vibrationally excited HF, and an unknown species in the trimethyl phosphine system. Banded emission from vibrationally excited HF and a broad continuum were observed for both trimethyl phosphine and triethyl phosphine; however, HCF emission was observed only for TMP. Under the conditions employed, the principal emitter is HCF for trimethyl phosphine and HF and the unknown emitter for triethyl phosphine. This detector may have important applications in investigations of the biogeochemical cycling of phosphorus.

Notes: Summary The usefulness of several grades of carbon dioxide for online supercritical fluid extraction/capillary gas chromatography has been studied. If trace-level work has to be performed, no single grade can be recommended for all modes of detection studied. Good-quality carbon dioxide is available for use with flame ionization and thermionic detectors. With electron-capture detection, however, distinct problems still exist.

Notes: Summary An indirect GC method is described for the determination of Ethephon in drinking water on the basis of the headspace analysis of the ethylene formed from Ethephon. In order to reach the necessary detection limit, the entire volume of the static headspace distribution is transferred into a cold injection system (CIS). There, the ethylene is adsorbed on Carbosieve SIII at 10°C and, subsequently, desorbed at 300 °C. The water vapour included in the headspace is completely eliminated through the splitting system. By means of this technique, a detection limit of 0.05 μg/l water was reached.

Notes: The reaction of 2-methylene-1,3-dioxolanes and 2-methylene-1,3-oxazolidines with benzoyl peroxide (acceptor radical) and with N-ethylmaleimide (acceptor) was investigated. It was shown that benzoyl peroxide adds to monomers 1a and 1b, giving the corresponding linear diester amides 1a and 1b respectively. The oxazolidine 1c adds benzoyl peroxide, without ring opening, by addition to the exomethylene group. Together with N-ethylmaleimide the oxazolidines 1a or 1b produce deep-colored charge transfer complexes, resulting in high molecular poly-N-ethylmaleimides probably via a radical mechanism. The 1,3-dioxolanes 2a and 2b were radically polymerized to produce polyacetals by vinyl polymerization. 2c was polymerized to produce randomly containing acetal units and ester units. The mechanism of polymerization of 2e is complex, affording polymers of nonuniform character. 2-Methylene-4-phenyl-1,3-dioxolane polymerization leads to polyester as the main structure, and to a lesser degree polyacetal structures. The chemical structures of the polymers were confirmed by NMR spectra and elemental analysis. © 1996 John Wiley & Sons, Inc.

Notes: Sodium hypochlorite solutions are used to treat membranes prepared from a polymeric blend containing poly(vinyl pyrrolidone) (PVP) to increase their water permeability. Sodium hypochlorite affects the membrane material in such a way that PVP is selectively removed from the membrane matrix. The mechanism of the reaction between hypochlorite and PVP is investigated by several chemical analysis techniques of the reaction products. Strong indications are found that the reaction involves chain scission of PVP according to a radical mechanism. © 1995 John Wiley & Sons, Inc.

Notes: Die Kenntnis der Grenztemperatur organischer Isolierstoffe ist für deren Anwendung in der Elektrotechnik von großer Wichtigkeit. Die Änderung von Eigenschaftswerten auf Grund einer Wärmebehandlung wird theoretisch beschrieben unter der Annahme, daß ein linearer Zusammenhang mit den Gesetzen der Reaktionskinetik besteht. Unter den getroffenen Voraussetzungen können. Alterungs- und Lebensdauerfunktionen angegeben werden, die sich bei geeigenten Koordinaten als Geradendarstellen lassen. Meßergebnisse können auf diese Weise besser ausgewertet werden als nach herkömmlichen Verfahren.