Linking Simultaneous In Situ WAXS/SAXS/Raman with Raman/ATR/UV–vis Spectroscopy: Comprehensive Insight into the Synthesis of Molybdate Catalyst Precursors

A new setup is presented which enables simultaneous wide- and small-angle X-ray scattering (WAXS/SAXS) and Raman spectroscopic experiments during the synthesis of Mo-based mixed oxide catalyst precursors at the μ-spot beamline at the Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung (BESSY). Furthermore, we report about the separate monitoring of the same reactions under comparable conditions by simultaneous combined ATR/UV–vis/Raman spectroscopic measurements. For testing the performance of both experimental setups two syntheses were described comprising the precipitation of metal molybdates by mixing solutions of metal nitrates and ammonium heptamolybdate. Additionally, the effect of H₃PO₄ admixture on precipitation was investigated. The combined evaluation of spectroscopic and WAXS/SAXS data allows the discrimination between different molybdate species appearing in solution and precipitate. Furthermore, these molybdate species could be assigned to separate phases of different crystallinity.     

A consistent flamelet formulation for a reacting char particle considering curvature effects

In the present work, the combustion of a single char particle in quiescent and convective environments is investigated numerically. Fully resolved CFD calculations are carried out considering heterogeneous reactions at the particle surface and detailed homogeneous reactions in the gas phase. Unity and non-unity Lewis number diffusion modeling approaches are employed and compared to each other. The flame shape of the particle in a quiescent atmosphere shows full symmetry whereas the particle in the convective environment exhibits a stagnation region upstream of the particle and a wake region downstream of the particle. The detailed CFD results are used to analyze the flame structure around the char particle and corresponding flamelet simulations are carried out. For the presently investigated case, curvature effects of mixture fraction, species and temperature are found to be significant in almost all the cases. These curvature effects correspond to diffusion tangential to iso-surfaces of mixture fraction. To describe these processes, new extended flamelet equations are derived. The individual terms in the flamelet equations are analyzed for both the quiescent and the convective environment based on the CFD data and the results confirm the importance of tangential diffusion. Except for the quiescent environment and unity Lewis numbers, curvature cannot be neglected for the investigated char combustion case. For all other cases, significant differences between the standard flamelet model and the detailed CFD results are found. On the other hand, applying the extended flamelet equations yields very good agreement with the CFD results.     

Detection of 4-aminocarminic acid in beverages and cake glaze from the German market: a food additive not approved in the EU

In the European Union, carminic acid and its ammonium, calcium, potassium or sodium salts and its aluminium lakes are approved as food additive E120. In beverages obtained from the German market 4-aminocarminic acid (“acid-stable carmine”) was detected by HPLC–PDA and LC–MS/MS. Isolation of the colorant from a liquid dye preparation used for the production of a beverage sample and subsequent NMR analysis confirmed the presence of 4-aminocarminic acid. Synthesis of ¹⁵N-4-aminocarminic acid clearly demonstrated that “acid-stable carmine” is not the ammonium salt of carminic acid, which is approved as food additive in the European Union. In fact, nitrogen in “acid-stable carmine” is covalently bound. The molecular structure of carminic acid is chemically modified and 4-aminocarminic acid does not comply with the specifications laid down for E120 in Commission Regulation (EU) No 231/2012. 4-Aminocarminic acid was also detected in the red-colored glaze of a raspberry cake and in the liquid dye preparation used for coloring this glaze.     

Protective effects of various preservation solutions on cultured endothelial cells

Vascular endothelium represents the first target in organ preservation and plays an important role in reperfusion injury. Bovine aortic endothelial cells were cultivated and the most commonly used preservation solutions, such as University of Wisconsin HTK (Brettschneider's histidine-tryptophane-ketoglutarate), and Euro-Collins solutions were tested on the endothelial monolayer. In addition, one group of cultivated cells was preserved with cold saline solution, and endothelial monolayers grown in culture medium were used as controls. The quality of preservation was assessed after 24, 48, and 72 hours of cold storage. Reperfusion was simulated and its effects were observed by reincubation in culture medium at 37 degrees C for 6 hours. The total number of cells, cell viability (determined using trypan blue exclusion), and morphologic alterations were determined. Prostacyclin release was evaluated as a biochemical marker. University of Wisconsin solution maintains more than 99% cell viability after rewarming after both 24 and 48 hours of cold storage. After 72 hours, 86.7% of cells were still viable. Preservation with HTK and Euro-Collins solution allowed cell survival for only 24 hours (96.7%, HTK; 49.9%, Euro-Collins), with no viable cells seen after 48 hours. The cold saline-preserved sample showed 57.8% viable cells after 24 hours and 29.7% after 48 hours. No viable cells were detectable after 72 hours. Light microscopy revealed several patterns of both structural damage and intracellular change (nucleus and cytoplasm) in the endothelial monolayer after preservation with HTK, Euro-Collins solution, and cold saline solution. No morphologic alterations were seen in the University of Wisconsin solution group for as long as 72 hours.(ABSTRACT TRUNCATED AT 250 WORDS)     

Effects of scatter and attenuation correction on quantitative assessment of regional cerebral blood flow with SPECT

The pyruvate dehydrogenase complex (PDC) plays a key role in the anaerobic mitochondrial metabolism of the parasitic nematode Ascaris suum. A cDNA coding for an A. suum pyruvate dehydrogenase kinase (APDK) has been cloned and sequenced from poly(A)+ RNA isolated from adult A. suum muscle.2 APDK exhibited significant sequence identity to mammalian PDKs. Nucleotide sequence analysis of the APDK cDNA revealed a 22-nucleotide spliced leader, characteristic of many nematode mRNAs, a 5'-UTR of 6 nucleotides, an open reading frame of 1197 nucleotides, and a 3'-UTR of 101 nucleotides that included a putative polyadenylation signal. The open reading frame predicted a protein of 399 amino acids with a molecular weight of 45,402 that included a putative 18-aminoacid leader peptide. Recombinant APDK (rAPDK) was functionally expressed in Escherichia coli with a his tag at its N-terminus and purified to apparent homogeneity on Ni-NTA-agarose. Recombinant APDK was a dimer and was not autophosphorylated and its activity was stimulated in the presence of APDK-deficient adult A. suum muscle PDC presumably by the binding of APDK to the dihydrolipoyl transacetylase (E2) core of the complex. After binding to the core, rAPDK activity was stimulated by elevated NADH/NAD+ and acetyl CoA/CoA ratios within the same ranges as observed for the native APDK. Immunoblotting suggested that native APDK focused as a series of 43-kDa spots (pI 6.1-6.8) on two-dimensional gels of the purified adult A. suum muscle PDC.