Quantitative Medium-Resolution NMR Spectroscopy Under Non-Equilibrium Conditions,Studied on the Example of an Esterification Reaction

Medium-resolution nuclear magnetic resonance spectroscopy is a promising tool for the monitoring of liquid reactions. For process analytical applications, the requirements of robustness and insensitivity of the spectrometer in relation to high temperatures and pressures are challenging. Within this study, a flow probe using a glass dewar is presented. Temperatures of flowing samples up to 130 °C and pressures up to 40 bar were successfully applied, and the corresponding temperature loss of the flowing sample at 2 ml min^?1 was <2.4 °C at 130 °C. Furthermore, if the process requires a measurement in a non-equilibrium state of magnetization, a comprehensive data treatment is given. For this purpose, the influences of the flow and T ₁ of the substances under investigation are studied in detail on the example of a homogeneously catalyzed esterification. In addition, data analysis schemes were designed such that the experiments directly revealed mole fractions from the spectra. Limited spectral resolutions and low signal-to-noise ratio still did not obstruct quantitative interpretation of the experiments.     

Neutron dosimetry device using PADC nuclear track detectors

A device consisting of poly allyl diglycol carbonate (PADC) foils with a polyethylene and polyvinyl chloride (PVC) radiator was calibrated in order to perform the dosimetry of an ²⁴¹Am-Be source covering a dose range from 0 to 3.1 mSv. Working conditions were established for a good visualization and counting of tracks: chemical attack was made in two steps with different solutions and etching times. A good fit was obtained for the dose as a function of the number of tracks per unit surface area. The calculated decision threshold was 0.12 mSv.     

Topochemical acetylation of cellulose nanopaper structures for biocomposites: mechanisms for reduced water vapour sorption

Moisture sorption decreases dimensional stability and mechanical properties of polymer matrix biocomposites based on plant fibers. Cellulose nanofiber reinforcement may offer advantages in this respect. Here, wood-based nanofibrillated cellulose (NFC) and bacterial cellulose (BC) nanopaper structures, with different specific surface area (SSA), ranging from 0.03 to 173.3 m²/g, were topochemically acetylated and characterized by ATR-FTIR, XRD, solid-state CP/MAS ¹³C-NMR and moisture sorption studies. Polymer matrix nanocomposites based on NFC were also prepared as demonstrators. The surface degree of substitution (surface-DS) of the acetylated cellulose nanofibers is a key parameter, which increased with increasing SSA. Successful topochemical acetylation was confirmed and significantly reduced the moisture sorption in nanopaper structures, especially at RH = 53 %. BC nanopaper sorbed less moisture than the NFC counterpart, and mechanisms are discussed. Topochemical NFC nanopaper acetylation can be used to prepare moisture-stable nanocellulose biocomposites.     

Die Selivanov‐Probe auf Fructose

The Seliwanoff's test is a useful tool in biochemistry and food chemistry as test for fructose and other hexoketoses. This article depicts the life and work of Russian chemist named F. F. Selivanov, who was born in aristocratic family, was affected by revolutionary Narodniki movement, and attended the universities in Russia, Switzerland and Germany. His life is a good example of connections between Russian and German agrochemical centres in XIX century. His major achievements are the test for fructose and the first synthesis of N‐Bromosuccinimide. He is also known as a doctoral supervisor of A.E. Arbuzov, the discoverer of Michaelis‐Arbuzov reaction.     

Die quantitative chemische Bestimmung von Vitamin D

Zusammenfassung Die zur Vitamin D₂-Bestimmung bekannten spezifischen Farbreaktionen nachHalden und H.Brockmann werden durch die Unbeständigkeit des erhaltenen Farbtones und dieser durch Fettbegleitsubstanzen empfindlich gestört. Es gelingt, eine für Vitamin D spezifische, im Farbton beständige Reaktion bei Verwendung einer 20%igen Antimontrichloridund 5%igen Guajakol-Lösung in Chloroform. Die Empfindlichkeit der Reaktion ist 1200000. Es können quantitativ 15 in 2,8 ml Chloroform nachgewiesen werden bei tunlichster Einhaltung der beschriebenen Versuchsbedingungen.Der Einfluß der Sterine auf die Reaktion ist sehr gering, doch werden die Empfindlichkeit und die Spezifität dann vermindert, wenn sehr große Mengen dieser Begleitstoffe vorhanden sind. Mit Hilfe der Adsorption an frisch behandeltes, bei 120 erhitztes Aluminiumoxyd können störende Begleitstoffe abgetrennt werden. Das Vitamin D₂ wird dabei in einer scharf umrissenen Zone festgehalten, die im UV.-Licht weiß aufleuchtet.Die vorliegende Methode ist geeignet zur mengenmäßigen Bestimmung von Vitamin D in tierischen und pflanzlichen Fetten, in Milch und Milcherzeugnissen, in Kindernährmitteln, bestrahlten Hefen und pharmazeutischen Präparaten. Um die hier auftretenden, störenden Begleitstoffe auszuschalten, werden die Präparate nach der Extraktion des Vitamins D verseift, und der unverseifbare Anteil wird an Aluminiumoxyd adsorbiert. Dabei wird das Vitamin D bei Einhaltung der Arbeitsvorschrift immer in einer charakteristischen schmalen Zone festgehalten, die im Tageslicht gelb bis rosafarben erscheint. Durch die Anwesenheit von Vitamin A, Provitamin A und anderen. Carotinoiden kann die Reaktion gestört werden, so daß auch hier eine chromatographische Auftrennung erforderlich ist, die sich aber leicht durchführen läßt.