In-house quality control material of nicarbazin and narasin in eggs: preparation and inter-laboratory evaluation

Coccidiostats are a group of pharmacologically active substances widely used in veterinary practice. Their residues are detected relatively often in poultry tissues and egg samples analyzed as part of official residue control programs in the European Union. Therefore, accuracy of quantitative results needs to be monitored through internal and external quality control studies. In addition, the use of materials containing incurred residues would be welcome to for ongoing monitoring of the method accuracy. Unfortunately, in the field of veterinary drug residues, certified reference materials are often unavailable. Therefore, in-house quality control material of incurred lyophilized eggs containing narasin and nicarbazin has been produced and characterized. The eggs originated from hens receiving feed with coccidiostat premix Maxiban were mixed to obtain presumed concentrations of residues and freeze-dried. Homogeneity of the material was verified by the duplicate analysis of ten random samples, and the results proved that the between samples variation was negligible in comparison with the method repeatability. No measurable loss of analytes was observed within 1 year; the slope of the regression line of the results of stability measurements was not significantly different from zero. The assigned values were expressed as medians of the results of inter-laboratory comparison performed in four different European laboratories; the uncertainty of the material was estimated, taken into consideration all above tests, resulting in (14.4 ± 2.53) µg/kg for nicarbazin and (7.91 ± 1.52) µg/kg for narasin.     

Conduction calorimetric studies of ternary binders based on Portland cement, calcium aluminate cement and calcium sulphate

Different binders of Portland cement, calcium aluminate cement and calcium sulphate (PC/CAC/C $ {\bar{\text{S}}} $ ) have been investigated to determinate the influence the CAC and C $ {\bar{\text{S}}} $ amount in the reactions mechanism. Several mixtures were studied, ratios of 100, 85/15 and 75/25 of PC/CAC with 0, 3 and 5 % of C $ {\bar{\text{S}}} $ . Conduction calorimetric technique was used to follow the hydration during 100 h. The XRD and FTIR techniques were used as support in the analysis of the hydration products. The results have shown that the studied ternary systems form an extra amount of ettringite, and changes in the reactions mechanism with respect to a PC. The reactions mechanism depends on the CAC and C $ {\bar{\text{S}}} $ amount present in the different binders.     

Monitoring and Evolution of the Pollution by Volatile Organic Compounds (Vocs) in the Groundwaters of The Najerilla River Basin (Spain)

VOCs were detected and identified in the water of several wells in the area of Nájera (La Rioja). The past uncontrolled spills from an important painting and varnishing industry and from other smaller ones devoted to the manufacture of furniture and varnishing activities were the sources of the VOCs plume detected in this aquifer. This article shows the results obtained in the monitoring and assessment of the pollution at 18 sampling points for more than a year. It has allowed us to study the evolution of the different pollutants and the influence of a remediation process applied by the company in the main pollution source. The analytical method is based on headspace-solid-phase microextraction (SPME) using a 75-μm carboxen-polydimethylsiloxane fibre. Quantification was carried out by gas chromatography with flame ionization detection. This method has allowed us to determine the 13 VOCs identified in the polluted underground samples providing good sensitivity (LOD between 0.1 and 6.0 ng/mL) and reproducibility (r.s.d. less than 10%).     

ITQ-12: a new microporous silica polymorph potentially useful for light hydrocarbon separations

The new synthetic form of microporous crystalline silica, denoted as ITQ-12, shows a high potential for the separation of propane and propene from its mixtures.     

Mathematical models of solute retention in gas chromatography as sources of thermodynamic data. Part III. Alkylbenzenes as the test analytes

Direct determination of thermodynamic data has always been a complicated and troublesome experimental task. Gas chromatography is among long-established working tools well suited to performing this particular task indirectly. Our own results were first presented in the papers by Ciazynska-Halarewicz and Kowalska (1,2), and this article is Part III in the series. Present experiments are carried out on low- and medium-polarity stationary phases at five different temperatures ranging from 323K to 423K. They enable determination of two thermodynamic properties of the alkylbenzenes, molar enthalpy of vaporization (DeltaH(vap)), and the chemical potential of partitioning of the methylene group between the two phases of the chromatographic system (Delta micro (p(-CH2-))). These properties are obtained from eight nonempirical models and, as is apparent from their derivation (3-7), the terms of the models have clearly defined physical meaning, which enables calculation of thermodynamic properties.     

Copper exchanged beta zeolites for the catalytic oxidation of ammonia

Copper exchanged on beta zeolites are extremely active and selective for the catalytic oxidation of ammonia to nitrogen and water and this activity correlates to the ease of reduction of the copper species.     

Colloidal liquid crystal type assemblies of spheroidal polystyrene core/polyglycidol‐rich shell particles (P[S/PGL]) formed at the liquid‐silicon‐air interface by a directed dewetting process

A method for the preparation of stripe‐like monolayers of microspheroids is described. The particles were obtained from polystyrene core/polyglycidol‐rich shell microspheres by stretching poly (vinyl alcohol) films that contain embedded particles. The stretching was performed under controlled conditions at temperatures above the T_g of the films and particles. The elongated films were dissolved in water, and the microspheroids were subsequently removed and purified from the poly (vinyl alcohol). The aspect ratio (AR) of the particles, which denotes the ratio of the lengths of the longer to shorter particle axes, was determined by the film elongation. The AR values were in the range of 2.9‐7.7. Spheroidal particles with various ARs were deposited onto silicon wafers from an ethanol (EtOH) suspension. The particle concentration and volume of the suspension were the same in each experiment. Evaporation of the EtOH yielded stripes of spherical particles packed into nematic‐type colloidal crystals and assembled into monolayers. The orientation of the stripes after ethanol evaporation was perpendicular to the triphasic (silicon‐ethanol‐air) interface along the silicon substrate. The adsorbed stripes on the wafers were characterized in terms of their interstripe distance (ID), stripe width, and crystal domain size. Nematic‐type spheroid arrangements in the stripes were the dominant structure, which enabled denser packing of the particles into colloidal crystals than that allowed by the smectic‐type arrangements. Furthermore, the number of spheroids adsorbed per surface unit of the silicon wafers was similar for all ARs, but the width and frequency of the spheroid stripes adsorbed on the wafers were different.     

Trapping of a Highly Reactive Oxoiron(IV) Complex in the Catalytic Epoxidation of Olefins by Hydrogen Peroxide

The generation of a nonheme oxoiron(IV) intermediate, [(cyclam)Fe^IV(O)(CH₃CN)]²⁺ ( 2 ; cyclam=1,4,8,11‐tetraazacyclotetradecane), is reported in the reactions of [(cyclam)Fe^II]²⁺ with aqueous hydrogen peroxide (H₂O₂) or a soluble iodosylbenzene (sPhIO) as a rare example of an oxoiron(IV) species that shows a preference for epoxidation over allylic oxidation in the oxidation of cyclohexene. Complex 2 is kinetically and catalytically competent to perform the epoxidation of olefins with high stereo‐ and regioselectivity. More importantly, 2 is likely to be the reactive intermediate involved in the catalytic epoxidation of olefins by [(cyclam)Fe^II]²⁺ and H₂O₂. In spite of the predominance of the oxoiron(IV) cores in biology, the present study is a rare example of high‐yield isolation and spectroscopic characterization of a catalytically relevant oxoiron(IV) intermediate in chemical oxidation reactions.     

Optimisation of a key cross-coupling reaction towards the synthesis of a promising antileishmanial compound

During the course of a research program aimed at identifying novel antileishmanial compounds, a multi-gram synthesis of N-(trans-4-((4-methoxy-3-((R)-3-methylmorpholino)-1H-pyrazolo[3,4-d]pyrimidin-6-yl)amino)cyclohexyl)-2-methylpropane-1-sulfonamide ((R)-1) was required. This letter describes optimisation of the reaction conditions and protecting group strategy for a key Buchwald-Hartwig coupling, delivering the required quantities of (R)-1, as well as further compounds in the series.     

Associative and segregative phase separations of poly(N-tert-butylacrylamide)/poly(acrylic acid) mixtures. Effect of solvent

Poly(N-tert-butylacrylamide) (PNtBAm) and poly(acrylic acid) (PAA) form interpolymer complexes in 1- and 2-propanol, blend in ethanol, whereas a segregative phase separation is observed when using methanol as solvent as shown by Fourier transform infrared (FTIR) spectrometry and elemental analysis studies. The composition of PNtBAm/PAA complexes has been determined. Thermal studies demonstrated that all complexes show unique glass transition temperatures, higher than those of the polymer components. Complexation of PAA with PNtBAm results in an improvement of its thermal stability. Solvent effects and specific interactions in the system PNtBAm/PAA have been studied by FTIR, revealing that differences in the polymer–solvent interactions are a decisive factor governing complex formation in solution.