Effect of milled fluidised bed cracking catalyst waste on hydration of calcium aluminate cement and formation of binder structure

The effect of Bi addition on precipitation and dissolution, in Cu–9at% In and Cu–5at% Sb supersaturated solid solutions, has been studied by several complementary techniques. Differential Dilatometry and Differential Scanning Calorimetry permit only the analysis of the δ phase dissolution kinetic in sufficiently aged samples. Delayed spheroidization due to Bi segregation around the precipitated lamellae, observed by Transmission Electron Microscopies in the first alloy, gives a residual interfacial energy leading to accelerated δ phase dissolution with decreased activation energy. Kinetics parameters evolution indicates a progressive δ phase continuous dissolution which makes available a small chemical driving force at high temperatures and leads to an increasing activation energy during dissolution. However, Bi dispersed particles in the second alloy haven’t effect on the dissolution but they cause a contraction above 833 K. Kinetics parameters evolution indicates rapid δ phase dissolution that shifted to high temperatures where an important chemical driving force for solution treatment is available. It leads to almost constant activation energy.

     

Use of slag (GBFS) generated in charcoal blast furnace as raw material in alkali-activated cement

Journal of Thermal Analysis and Calorimetry - Alkali-activated cements are low-environmental-impact binders and can be obtained from the alkaline activation of wastes such as slags and fly ashes,...     

NMR Characterization of Lanthanide(3+) Complexes of Tetraazatetrakisphosphinato and Tetraazatetra­kisphosphonato Ligands

The three‐dimensional structures in aqueous solution of the entire series of the Ln³⁺ complexes [Ln(DOTP*‐Et)]^? (formed from the free ligand P,P′,P″,P′′′‐[1,4,7,10‐tetraazacyclododecane‐1,4,7,10‐tetrayltetrakis(methylene)]tetrakis[P‐ethylphosphinic acid] (H₄DOTP*‐Et) were studied by NMR techniques to rationalize the parameters governing the relaxivity of the Gd³⁺ complex and evaluate its potential as MRI contrast agent. From the ¹H‐ and ³¹P‐NMR lanthanide‐induced‐shift (LIS) values, especially of the [Yb(DOTP*‐Et)]^? complex, it was concluded that the [Ln(DOTP*‐Et)]^? complexes adopt in solution twisted square antiprismatic coordination geometries which change gradually their coordination‐cage structure along the lanthanide series. These complexes have no inner‐sphere‐H₂O coordination, and preferentially have the (R,R,R,R) configuration of the P‐atoms in the pendant arms. Self‐association was observed in aqueous solution for the tetraazatetrakisphosphonic acid ester complexes [Ln(DOTP*‐OEt)]^? (=[Ln(DOTP‐Et)]^?) and [Ln(DOTP*‐OBu)]^? (=[Ln(DOTP‐Bu)]^?) at and above 5 mM concentration, through analysis of ³¹P‐NMR, EPR, vapor‐pressure‐osmometry, and luminescence‐spectroscopic data. The presence of the cationic detergent cetylpyridinium chloride (CPC; but not of neutral surfactants) shifts the isomer equilibrium of [Eu(DOTP*‐OBu)]^? to the (S,S,S,S) form which selectively binds to the cationic micelle surface.     

Statistical mixture design selective extraction of compounds with antioxidant activity and total polyphenol content from Trichilia catigua

Statistical design mixtures of water, methanol, acetone and ethanol were used to extract material from Trichilia catigua (Meliaceae) barks to study the effects of different solvents and their mixtures on its yield, total polyphenol content and antioxidant activity. The experimental results and their response surface models showed that quaternary mixtures with approximately equal proportions of all four solvents provided the highest yields, total polyphenol contents and antioxidant activities of the crude extracts followed by ternary design mixtures. Principal component and hierarchical clustering analysis of the HPLC–DAD spectra of the chromatographic peaks of 1:1:1:1 water–methanol–acetone–ethanol mixture extracts indicate the presence of cinchonains, gallic acid derivatives, natural polyphenols, flavanoids, catechins, and epicatechins.     

Preparation and characterization of bilayer carbon/polymer membranes

The objective of the present research work was to develop a membrane with a high H₂O/alcohol selectivity for pervaporation and for use in direct alcohol fuel cells. Sulfonated poly (ether ether ketone) (SPEEK) was coated with a thin continuous carbon molecular sieve (CMS) layer. The membranes obtained had 180- and 400-nm thick CMS layers that led to a clear reduction of alcohol crossover. The water/alcohol selectivity increased with the size of the alcohol molecules as follows: methanol < ethanol < n-propanol < iso-propanol. A water/n-propanol selectivity of up to 34,000 was obtained, confirming the molecular sieving effect. The system was tested in a direct methanol fuel cell using standard electrodes, and demonstrated a better performance than with plain membranes. In a later stage Pt was introduced in the CMS layer during the preparation of the membrane electrode assemblies, this had the advantage that the CMS layer not only acted as an alcohol barrier but also as a catalyst support.     

Differentiation of two main ammunition brands in Chile by Regularized Discriminant Analysis (RDA) of metals in gunshot residues

Conventionally, chemical patterns of gunshot residues (GSR) can be used for identification of a suspect involved in criminal fire arm incidents. Furthermore, metals composition in GSR is well related with the ammunition brand. In Chile the two main ammunition brands used are FAMAE and CBC. Metals, such as Pb, Ba, Sb, Cu, Zn and Ca are common elements detected in both brands. This work describes the application of both conventional and chemometric analysis of data (Regularized Discriminant Analysis, RDA) for differentiation of ammunition brands according to the metal patterns of GSR collected from shooter individuals. Real samples of GSR were collected from hands (dorsal region) of both shooters and non-shooters. Metals were analyzed using the techniques Atomic Absorption Spectrometry (AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-OES). By means of conventional plotting techniques for differentiation, such as binary and ternary plots, differences between the two brands are observed although without quantitative certainty. For the first time, applying chemometric analysis, such as regularized discriminant analysis (RDA), the investigated ammunition brands can be classified and differentiated correctly with 100% certainty.     

Synthesis of porphyrin indolin-2-one conjugates via palladium-catalyzed amination reactions

New porphyrin indolin-2-one conjugates were synthesized via palladium-catalyzed amination reactions of iodinated and dibrominated indolin-2-one derivatives with (2-amino-5,10,15,20-tetraphenylporphyrinato)nickel(II). The combination of palladium catalysts and the phosphine ligand dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl (XPhos) is an effective methodology for catalyzing the coupling of 5-iodo-, 5,7-dibromo- and 4,6-dibromo-1,3,3-trimethylindolin-2-one with 2-aminoporphyrin to give the corresponding mono-(2-aminoporphyrinyl)- and di-(2-aminoporphyrinyl)-substituted indolin-2-ones in satisfactory yields under mild conditions. The mono brominated porphyrinic derivatives also underwent cross-coupling reactions under similar catalytic conditions. The studies also demonstrated that the course of the coupling process depends on factors, such as the catalytic system, number and position of the halogen substituents and the heating condition. Insights into the reactivity trends of the 5-iodo; 4,6- and 5,7-dibrominated indolin-2-one derivatives was carried out using theoretical calculations performed using density-functional theory with the B3LYP functional.     

Implementation of the quality management system at the Laboratory of Radiological Protection and Safety (LPSR) in Portugal

The paper describes the activities carried out for the implementation of the quality management system (QMS) at the Laboratory of Radiological Protection and Safety (LPSR) in Portugal in order to achieve the management and technical requirements of ISO/IEC 17025:2005 and to get the accreditation for ten tests. The implementation of the QMS based on this international standard allowed LPSR to improve the methods, to identify problems, to implement preventive and corrective actions, to generate valid results and to achieve a stable level of high-quality output recognized by an independent body in the scope of waters, metrology, radiation and radiochemistry.