Rapid method for radiostrontium determination in milk in emergency situations using PS resin

This study describes a new and rapid procedure for radiostrontium determination in milk samples based on the use of plastic scintillation resins (PS resins). The proposed method reduces the time of analysis by at least 2 h by combining separation and measurement preparation into a single step and optimizing the pre-treatment steps. The method is robust and reproducible, with good total recoveries (65% on average) and a relative bias for total radiostrontium activity (⁸⁹Sr + ⁹⁰Sr) below 7%. The minimum detectable activity for 100 mL of milk sample measured for 60 min is about 0.34 Bq L^?1. The proposed method can quantify radiostrontium content in 5 h, which makes it suitable for use in emergency situations.     

Gravimetric determination of palladium with quinolinimide as a reagent

Summary Quinolinimide which is found to be a selective reagent for palladium forms a complex of the composition Pd(C₇H₃O₂N₂)₂. The reagent quantitatively precipitates palladium from solutions of p_H 0.5 to 2.5 in presence of common ions as well as platinium metals, except tin which, however, can be kept in solution by complexing with citric acid. The palladium complex being stable up to 307° C can be directly weighed.

---

Zusammenfassung Chinolinimid wird als selektives Reagens für Palladium vorgeschlagen. Bei p_H-Werten zwischen 0,5 und 2,5 kann Palladium quantitativ in Form des Komplexes Pd(C₇H₃O₂N₂)₂ gefällt werden, wobei die meisten anderen Ionen, auch die der Platinmetalle, in Lösung bleiben. Zinn stört, kann aber mit Citronensäure maskiert werden. Der Palladiumkomplex ist bis 307° C stabil und kann direkt ausgewogen werden.

     

DBU-CH3I,a Potential Substitute for CH2N2 in the Preparation of Methyl Esters and Methyl Aryl Ethers: Studies with Assorted Acids

DBU-CH₃I has been poised to be a substitute for diazomethane in the preparation of methyl esters from carboxylic acids. The reactions can be carried out in commercial untreated acetone and acetonitrile, which have been exemplified with several methyl esters, otherwise it is difficult to prepare. Bis-esterification using diiodomethane can also be achieved in a similar fashion. Sufficiently acidic phenols are also conveniently O-methylated by the method.     

Ultra-performance liquid chromatography-tandem mass spectrometry for the analysis of heterocyclic amines in food

A new ultra-performance liquid chromatography-electrospray tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed to perform the determination of 16 mutagenic heterocyclic amines (HAs) in complex food samples in less than 2 min. The UPLC separation was carried out using an Acquity BEH C18 column (50 mm x 2.1 mm i.d., 1.7 microm particle size) that provided high efficiency and resolution in combination with high linear velocities. The UPLC system was coupled to the triple quadrupole Waters Micromass Quattro Premier. This system permits high-speed data acquisition without peak intensity degradation which is required to monitor the narrow chromatographic peaks (1-2 s) of HAs. The determination was performed in selected reaction monitoring (SRM) mode. The quality parameters of the developed method were established, obtaining instrumental LODs lower than 0.23 pg injected and a repeatability at low concentration level lower than 9.1% CV (n = 6). To evaluate the performance of the method in high throughput analysis of complex samples, the UPLC-MS/MS method was applied to the analysis of HAs in two meat extracts.     

Solid‐Phase Incorporation of an ATRP Initiator for Polymer–DNA Biohybrids

The combination of polymers with nucleic acids leads to materials with significantly advanced properties. To obviate the necessity and complexity of conjugating two macromolecules, a polymer initiator is described that can be directly covalently linked to DNA during solid‐phase synthesis. Polymer can then be grown from the DNA bound initiator, both in solution after the DNA‐initiator is released from the solid support as well as directly on the solid support, simplifying purification. The resulting polymer‐DNA hybrids were examined by chromatography and fluorescence methods that attested to the integrity of hybrids and the DNA. The ability to use DNA‐based supports expands the range of readily available molecules that can be used with the initiator, as exemplified by direct synthesis of a biotin polymer hybrid on solid‐support. This method expands the accessibility and range of advanced polymer biohybrid materials.     

Iodine/CuI-mediated alkyne–carbonyl metathesis reaction: synthesis of 1-aryl-1,2-dihydrochromeno[2,3-b]azepine-3,6-dione

Iodine/cuprous iodide-mediated intramolecular alkyne–carbonyl metathesis reaction has been developed using 2-(N-aryl-N-propargyl)aminochromone-3-carbaldehyde as the substrate. It led to the synthesis of hitherto unreported chromeno[2,3-b]azepine-3,6-dione. The special features of this methodology are mild reaction conditions, 100% atom economy and use of inexpensive reagents. This is the first example of I₂/CuI-mediated alkyne–carbonyl metathesis reaction.     

Indium trichloride catalyzed sp C–H bond functionalization of 2-alkyl azaarenes under microwave irradiation

Microwave promoted indium trichloride (10 mol %) catalyzed sp³ C–H bond functionalization of 2-alkyl azaarenes 1 or 4 has been observed to construct C–C bond either with but-2-ene-1,4-diones 2 or (E)-3-(2-oxo-2-phenylethylidene)indolin-2-one (6) giving access to 2-((quinolin-2-yl)methyl)butane-1,4-diones 3, 2-((pyridin-2-yl)methyl)butane-1,4-diones 5, or 3-(quinolin-2-yl)propan-2-yl)indolin-2-ones 7 in good yields using 1,4-dioxane as solvent.     

Biomimetic multifunctional porous chalcogels as solar fuel catalysts

Biological systems that can capture and store solar energy are rich in a variety of chemical functionalities, incorporating light-harvesting components, electron-transfer cofactors, and redox-active catalysts into one supramolecule. Any artificial mimic of such systems designed for solar fuels production will require the integration of complex subunits into a larger architecture. We present porous chalcogenide frameworks that can contain both immobilized redox-active Fe(4)S(4) clusters and light-harvesting photoredox dye molecules in close proximity. These multifunctional gels are shown to electrocatalytically reduce protons and carbon disulfide. In addition, incorporation of a photoredox agent into the chalcogels is shown to photochemically produce hydrogen. The gels have a high degree of synthetic flexibility, which should allow for a wide range of light-driven processes relevant to the production of solar fuels.