Mehr-Detektor-Anordnung für die Koinzidenzmessung von Positronenstrahlern

Procedures are given for the title compounds, which allow their preparation in high chemical purity and without any depletion of the ¹⁵N-content. A nitrogen isotope exchange between NOBF₄ and ¹⁵N₂O₃ was found, but it is too slow for preparative purposes.     

Isotopenverdünnungsanalytische Multielementanalyse mit der Funkenquellen-Massenspektrographie

Es wird ein Verfahren zur Isotopenverdünnungsanalyse mit stabilen Isotopen unter Verwendung einer Funkenionenquelle und einem doppelfokussierenden Massenspektrographen beschrieben, welches die gleichzeitige Analyse mehrerer Elemente in pulverförmigen Feststoffen erlaubt.

Die Leistungsfähigkeit des Analysenverfahrens wild am Beispiel der Spurenanalyse geologischer Standardproben demonstriert.

Das Analysenverfahren erlaubt die Bestimmung von Spurenkonzentrationen bis in den ppb-Bereich mit Standardabweichungen zwischen 2 und 10%.     

Funnel-type etched ion tracks in polymers

It is shown that conical track etching is a much more complicated process than generally assumed. The choice of the corresponding parameters (i.e. the ratios of concentrations and diffusion coefficients of both etchant (e.g. NaOH) and stopping solutions (e.g. HCl) and the etching temperature) determines the ratio of polymer dissolution to etchant penetration. The latter value controls the counterplay of diffusion, etching, ionic conductivity, field emission and capacitive effects, which is decisive for both the final track shapes and their electronic properties. The stages of track evolution during etching under different conditions are outlined in detail. Both transparent conical nanopores and “funnel-type” tracks can be obtained, the latter consisting of a shorter cone and a residual latent track. Depending on the internal structure of that latent track segment, such funnel-type tracks either allow smooth transmission of the rectified currents or they emit unipolar current spikes. Not only the study of electronic properties of single ion tracks, but also of a multitude of tracks makes sense. Depending on the applied parameters, the individual track properties may either just add up, or new effects may be found that emerge from the interaction of the tracks among each other. This is preferentially the case for spike-emitting tracks, where effects such as phase-locked spike synchronization can be found as described by neural network theory.     

Parametric study on a compound-drop spray flame

The introduction of compound-drop spray in a combustion system is a new concept. These droplets bear two gasification stages to cause an integral positive or negative effect on a premixed flame to raise or lower the local temperature of the gasification region. In this paper, we adopt a compound drop which contains a water core encased by a layer of shell fuel. A one-dimensional homogeneous lean or rich premixed flame with the dilute compound-drop spray was investigated by using large activation energy asymptotic analysis. The compound-drop spray burning mode was defined and divided into completely pre-vaporised burning (CPB), shell pre-vaporised burning (SPB) and shell partially pre-vaporised (SPP) burning modes by way of the gasification zones of the shell fuel and the core water relative to the flame position. The influences of the initial droplet radius, the shell-fuel mass fraction and the liquid loading of the compound-drop spray on the lean and rich flames were analysed. By means of the normalisation parameter of flame propagation mass flux (), enhancement, suppression or extinction of the compound-drop spray flame can be represented clearly. Furthermore, from the observation of extinction, the necessary conditions of extinction of a lean spray flame by the internal heat transfer are that the spray is a negative effect and causes a sufficient heat loss rate at flame sheet downstream side. For a rich spray flame, three extinction patterns were observed; they occur in SPP, SPB or at the critical SPB mode, but do not in CPB. The extinction maps of the compound-drop spray demarcate the patterns and also indicate the limitations and corresponding conditions of the flame extinction.     

A theoretical and numerical evaluation of the steady-state burning rate of vertically oriented PMMA slabs

The steady state burning rate of vertically oriented slabs of poly-methyl-methacrylate (PMMA) is numerically investigated. Model predictions are compared with measurements and results of the laminar boundary layer (LBL) theory. The numerical model provides a solution of the Favre-averaged Navier–Stokes equations coupled with sub-models for turbulence, combustion, soot production and radiation. The modelling of condensed phase processes is based on the one-dimensional heat transfer equation and pyrolysis is treated as a phase change using the latent heat approach. Results show that the pyrolysing region can be divided into three regions. In the laminar part of the flow (Gr _x < 4.3 × 10⁷), the predicted normalised burning rate, [mdot]″ _p x/μ_∞, is a power-law function of Gr _x with an exponent close to that of the LBL theory, surface re-radiation being the primary source of discrepancies. From the LBL theory for free flow, it is demonstrated that the local burning rate is inversely proportional to the shear velocity gradient. This is globally confirmed by numerical model results. At Gr _x = 4.3 × 10⁷ the change in slope of the burning rate observed experimentally, which indicates the end of the laminar flow region, is reproduced numerically. From Gr _x = 2.5 × 10⁹ model results show that the surface mass flux of pyrolyzate increases with x, in agreement with experimental data in literature.     

Sample Preparation for the Determination of Metals in Food Samples Using Spectroanalytical Methods—A Review

Abstract

The present article gives an overview of recent publications and modern techniques of sample preparation for food analysis employing atomic and inorganic mass spectrometric techniques, such as flame atomic absorption spectrometry, chemical vapor generation atomic absorption and atomic fluorescence spectrometry, graphite furnace atomic absorption spectrometry, inductively coupled plasma optical emission spectrometry, and inductively coupled plasma mass spectrometry. Among the most frequently applied sample preparation techniques for food analysis are dry ashing, usually with the addition of an ashing aid, and acid digestion, preferably with the assistance of microwave energy. Slurry preparation, particularly with the assistance of ultrasound, is increasingly used to reduce acid consumption and sample preparation time. Direct analysis of solid samples is gaining importance in the field of food analysis as it offers the highest sensitivity, avoids the use of acids and other aggressive reagents, makes possible the analysis of micro‐samples, and can be applied for fast screening analysis, e.g., of fresh meat.     

Recent Developments in Flow Injection/Sequential Injection Liquid-Liquid Extraction for Atomic Spectrometric Determination of Metals and Metalloids

Abstract

This review aims to provide a critical overview of automated flow injection and sequential injection liquid-liquid extraction for preconcentration and/or separation of ultra-trace metal and metalloid species hyphenated with atomic spectrometric detection systems, including some new trends and applications in the subbranches of cloud point extraction (CPE), wetting film extraction (WFE), supported liquid membrane extraction (SLME), extraction chromatography (EChr), and liquid-phase microextraction (LPME) techniques. The analytical performance of flow-injection/sequential injection liquid-liquid extraction methods is markedly affected by the components of the flow network such as segmentor, extraction coil, and phase separator. Thus, an overall presentation of system components along with some novel strategies for interface with atomic spectrometers is discussed and exemplified with selected applications.     

Microplasma Technology and Its Applications in Analytical Chemistry

Abstract

This review article describes some existing microplasma sources and their applications in analytical chemistry. These microplasmas mainly include direct current glow discharge (DC), microhollow-cathode discharge (MHCD) or microstructure electrode (MSE), dielectric barrier discharge (DBD), capacitively coupled microplasmas (CCμPs), miniature inductively coupled plasmas (mICPs), and microwave-induced plasmas (MIPs). The historical development and recent advances in these microplasma techniques are presented. Fundamental properties of the microplasmas, the unique features of the reduced size and volume, as well as the advantageous device structures for chemical analysis are discussed in detail, with the emphasis toward detection of gaseous samples. The analytical figures of merit obtained using these microplasmas as molecular/elemental-selective detectors for emission spectrometry and as ionization sources for mass spectrometry are also given in this review article.     

Mass Spectrometry,Review of the Basics: Ionization

Abstract: Mass spectrometry (MS) has become an integral tool in life sciences. The first step in MS analysis is ion formation (ionization). Many ionization methods currently exist; electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI) are the most commonly used. ESI relies on the formation of charged droplets releasing ions from the surface (ion evaporation model) or via complete solvent evaporation (charge residual model). MALDI ionization, however, is facilitated via laser energy and the use of a matrix. Despite wide use, ESI cannot efficiently ionize nonpolar compounds. Atmospheric pressure chemical ionization (APCI) and atmospheric pressure photo ionization (APPI) are better suited for such tasks. APPI requires photon energy and a dopant, whereas APCI is similar to chemical ionization. In 2004, ambient MS was introduced in which ionization occurs at the sample in its native form. Desorption electrospray ionization (DESI) and direct analysis in real time (DART) are the most widely used methods. In this mini-review, we provide an overview of the main ionization methods and the mechanisms of ion formation. This article is educational and intended for students/researchers who are not very familiar with MS and would like to learn the basics; it is not for MS experts.