Stability-indicating comparative methods using mekc and lc for determination of olmesartan medoxomil

A stability-indicating method using MEKC was validated for the analysis of olmesartan medoxomil in tablets. Successful separation was achieved using a fused silica capillary (40 cm x 50 µm i.d.); background electrolyte consisted of a combination of 10 mmol L-1 borate buffer and 5 mmol L-1 anionic detergent sodium dodecyl sulfate (95:5; v/v) pH 6.5; hydrodynamic mode at 50 mBar for 5 s; 25 kV separation voltage at 25 ºC; and column temperature 25 ºC with detection at 257 nm. The proposed method, validated following ICH guidelines, was applied to the determination of this antihypertensive with good results compared with an LC method.

Decaimento de íons cianato e a formação de carbamato de etila

Cyanate ion stability was studied in aqueous/ethanolic solutions, pH = 4.5 (CH3COOH/NaCH3COO), at different temperatures. Following the decay [(OCN)-] versus time, in the presence of excess C2H5OH, the rate constant for this reaction (k1) was calculated as (2.5 ± 0.3) x 10-4 s-1 at 25 ºC, for 0 < [C2H5OH] < 13.7 x 10-1 mol L-1. For [C2H5OH] > 2.0 mol L-1 a decrease in the numerical value of k1 was observed, reaching 5.2 x 10-5 s-1 when [CH3CH2OH] = 13.7 mol L-1. Variations in the kinetic parameter values ΔH1‡, ΔS1‡ and ΔG1‡ for the cyanate ion decay reaction were observed for solutions at different ethanol concentrations.

Stability of a nanofiltration membrane after contact with a low-level liquid radioactive waste

This study investigated the treatment of a liquid radioactive waste containing uranium (235U + 238U) using nanofiltration membranes. The membranes were immersed in the waste for 24-5000 h, and their transport properties were evaluated before and after the immersion. Surface of the membranes changed after immersion in the waste. The SW5000 h specimen lost its coating layer of polyvinyl alcohol, and its rejection of sulfate ions and uranium decreased by about 35% and 30%, respectively. After immersion in the waste, the polyamide selective layer of the membranes became less thermally stable than that before immersion.

Stability-indicating RP-HPLC method for simultaneous determination of gatifloxacin and flurbiprofen in binary combination

A stability-indicating RP-HPLC method is presented for determination of gatifloxacin and flurbiprofen in binary combination. Gatifloxacin, flurbiprofen and their degradation products were detected at 254 nm using a BDS Hypersil C8 (250 X 4.6 mm, 5 µm) column and mixture of 20 mM phosphate buffer (pH 3.0) and methanol 30:70 v/v as mobile phase. Response was linear over the range of 15-105 mg mL-1 for gatifloxacin (r² > 0.998) and of 1.5-10.5 mg mL-1 for flurbiprofen (r² > 0.999). The developed method efficiently separated the analytical peaks from degradation products (peak purity index > 0.9999). The method developed can be applied successfully for determination of gatifloxacin and flurbiprofen in human serum, urine, pharmaceutical formulations, and their stability studies.

Evaluation of phenotypic stability of resistance to Phytophthora spp. in cacao clones

Resistance of fourteen Theobroma cacao clones to Phytophthora spp. was evaluated using stem inoculations on grafted seedlings. Concepts of phenotypic stability were used to interpret the results and to express horizontality of the resistance. The linear regression coefficient 'b', the determination coefficient (R²) and average lesion size were used to determine the level of horizontal resistance, the phenotypic stability and the predictability of all clones. The results indicated that clones P 7 and MA 15 present highest levels of horizontal resistance and stability, but with moderate predictability. Clones CAS 1 and CEPEC 13 were classified as those with high horizontal resistance, stability and predictability, while clones PA 30, UF 650 and SIAL 88 and EET 59 showed intermediate resistance and stability and high predictability. Clones SPA 17, OC 61, PA 150, SIAL 505, ICS 1 and R 41 presented high susceptibility and intermediate or low stability and moderate or high predictability.

Thermal decomposition and stability in a series of heterobimetallic carbonyl compounds of the type [Fe(CO)4(HgX)2] (X=Cl, Br, I)

Heterobimetallic carbonyl compounds of the type [Fe(CO)4(HgX)2] (X= Cl, Br, I), which have metal-metal bonds, have been prepared in order to study their thermal stabilities as a function of the halogen coordinated to mercury atoms. The characterization of the above complexes was carried out by elemental analysis, IR and NMR spectroscopies. Their thermal behaviour has been investigated and the final product was identified by IR spectroscopy and by X-ray powder diffractogram.

Numerical modelling of small supersonic axial flow turbines

Supersonic axial turbine stages typically exhibit lower efficiencies than subsonic axial turbine stages. One reason for the lower efficiency is the occurrence of shock waves. With higher pressure ratios the flow inside the turbine becomes relatively easily supersonic if there is only one turbine stage. Supersonic axial turbines can be designed in smaller physical size compared to subsonic axial turbines of same power. This makes them good candidates for turbochargers in large diesel engines, where space can be a limiting factor. Also the production costs are lower for a supersonic axial turbine stage than for two subsonic stages. Since supersonic axial turbines are typically low reaction turbines, they also create lower axial forces to be compensated with bearings compared to high reaction turbines. The effect of changing the stator-rotor axial gap in a small high (rotational) speed supersonic axial flow turbine is studied in design and off-design conditions. Also the effect of using pulsatile mass flow at the supersonic stator inlet is studied. Five axial gaps (axial space between stator and rotor) are modeled using threedimensional computational fluid dynamics at the design and three axial gaps at the off-design conditions. Numerical reliability is studied in three independent studies. An additional measurement is made with the design turbine geometry at intermediate off-design conditions and is used to increase the reliability of the modelling. All numerical modelling is made with the Navier-Stokes solver Finflo employing Chien’s k ¡ ² turbulence model. The modelling of the turbine at the design and off-design conditions shows that the total-to-static efficiency of the turbine decreases when the axial gap is increased in both design and off-design conditions. The efficiency drops almost linearily at the off-design conditions, whereas the efficiency drop accelerates with increasing axial gap at the design conditions. The modelling of the turbine stator with pulsatile inlet flow reveals that the mass flow pulsation amplitude is decreased at the stator throat. The stator efficiency and pressure ratio have sinusoidal shapes as a function of time. A hysteresis-like behaviour is detected for stator efficiency and pressure ratio as a function of inlet mass flow, over one pulse period. This behaviour arises from the pulsatile inlet flow. It is important to have the smallest possible axial gap in the studied turbine type in order to maximize the efficiency. The results for the whole turbine can also be applied to some extent in similar turbines operating for example in space rocket engines. The use of a supersonic stator in a pulsatile inlet flow is shown to be possible.

Stability constants and thermodynamic parameters of cadmium complexes with sulfonamides and cephapirin

Stability constant (log beta) and thermodynamic parameters of Cd2+ complexes with sulfonamide and cephapirin were determined by Polarographic technique at pH = 7.30 ± 0.01 and µ = 1.0 M KNO3 at 250°C. The sulfonamides were sulfadiazine, sulfisoxazole, sulfamethaxazole, sulfamethazine, sulfathiazole, sulfacetamide and sulfanilamide used as primary ligands and cephapirin as secondary ligand. Cd2+ formed 1:1:1, 1:2:1 and 1:1:2 complexes. The nature of electrode processes were reversible and diffusion controlled. The stability constants and thermodynamic parameters (deltaG, deltaH and deltaS) were determined. The formation of the metal complexes has been found to be spontaneous, exothermic in nature, and entropically unfavourable at higher temperature.

Numerical Investigation of Flow Past a Circular Cylinder and in a Staggered Tube Bundle Using Various Turbulence Models

Transitional flow past a three-dimensional circular cylinder is a widely studied phenomenon since this problem is of interest with respect to many technical applications. In the present work, the numerical simulation of flow past a circular cylinder, performed by using a commercial CFD code (ANSYS Fluent 12.1) with large eddy simulation (LES) and RANS (κ - ε and Shear-Stress Transport (SST) κ - ω! model) approaches. The turbulent flow for ReD = 1000 & 3900 is simulated to investigate the force coefficient, Strouhal number, flow separation angle, pressure distribution on cylinder and the complex three dimensional vortex shedding of the cylinder wake region. The numerical results extracted from these simulations have good agreement with the experimental data (Zdravkovich, 1997). Moreover, grid refinement and time-step influence have been examined. Numerical calculations of turbulent cross-flow in a staggered tube bundle continues to attract interest due to its importance in the engineering application as well as the fact that this complex flow represents a challenging problem for CFD. In the present work a time dependent simulation using κ – ε, κ - ω! and SST models are performed in two dimensional for a subcritical flow through a staggered tube bundle. The predicted turbulence statistics (mean and r.m.s velocities) have good agreement with the experimental data (S. Balabani, 1996). Turbulent quantities such as turbulent kinetic energy and dissipation rate are predicted using RANS models and compared with each other. The sensitivity of grid and time-step size have been analyzed. Model constants sensitivity study have been carried out by adopting κ – ε model. It has been observed that model constants are very sensitive to turbulence statistics and turbulent quantities.

Thermal stability and thermal decomposition of sucralose

Several papers have been described on the thermal stability of the sweetener, C12H19Cl3O8 (Sucralose). Nevertheless no study using thermoanalytical techniques was found in the literature. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC) and infrared spectroscopy, have been used to study the thermal stability and thermal decomposition of sweetener.

Analysis and Control of Excitation, Field Weakening and Stability in Direct Torque Controlled Electrically Excited Synchronous Motor Drives

Direct torque control (DTC) is a new control method for rotating field electrical machines. DTC controls directly the motor stator flux linkage with the stator voltage, and no stator current controllers are used. With the DTC method very good torque dynamics can be achieved. Until now, DTC has been applied to asynchronous motor drives. The purpose of this work is to analyse the applicability of DTC to electrically excited synchronous motor drives. Compared with asynchronous motor drives, electrically excited synchronous motor drives require an additional control for the rotor field current. The field current control is called excitation control in this study. The dependence of the static and dynamic performance of DTC synchronous motor drives on the excitation control has been analysed and a straightforward excitation control method has been developed and tested. In the field weakening range the stator flux linkage modulus must be reduced in order to keep the electro motive force of the synchronous motor smaller than the stator voltage and in order to maintain a sufficient voltage reserve. The dynamic performance of the DTC synchronous motor drive depends on the stator flux linkage modulus. Another important factor for the dynamic performance in the field weakening range is the excitation control. The field weakening analysis considers both dependencies. A modified excitation control method, which maximises the dynamic performance in the field weakening range, has been developed. In synchronous motor drives the load angle must be kept in a stabile working area in order to avoid loss of synchronism. The traditional vector control methods allow to adjust the load angle of the synchronous motor directly by the stator current control. In the DTC synchronous motor drive the load angle is not a directly controllable variable, but it is formed freely according to the motor’s electromagnetic state and load. The load angle can be limited indirectly by limiting the torque reference. This method is however parameter sensitive and requires a safety margin between the theoretical torque maximum and the actual torque limit. The DTC modulation principle allows however a direct load angle adjustment without any current control. In this work a direct load angle control method has been developed. The method keeps the drive stabile and allows the maximal utilisation of the drive without a safety margin in the torque limitation.

Microscopic simulation of pigment coating consolidation

The control of coating layer properties is becoming increasingly important as a result of an emerging demand for novel coated paper-based products and an increasing popularity of new coating application methods. The governing mechanisms of microstructure formation dynamics during consolidation and drying are nevertheless, still poorly understood. Some of the difficulties encountered by experimental methods can be overcome by the utilisation of numerical modelling and simulation-based studies of the consolidation process. The objective of this study was to improve the fundamental understanding of pigment coating consolidation and structure formation mechanisms taking place on the microscopic level. Furthermore, it is aimed to relate the impact of process and suspension properties to the microstructure of the coating layer. A mathematical model based on a modified Stokesian dynamics particle simulation technique was developed and applied in several studies of consolidation-related phenomena. The model includes particle-particle and particle-boundary hydrodynamics, colloidal interactions, Born repulsion, and a steric repulsion model. The Brownian motion and a free surface model were incorporated to enable the specific investigation of consolidation and drying. Filter cake stability was simulated in various particle systems, and subjected to a range of base substrate absorption rates and system temperatures. The stability of the filter cake was primarily affected by the absorption rate and size of particles. Temperature was also shown to have an influence. The consolidation of polydisperse systems, with varying wet coating thicknesses, was studied using imposed pilot trial and model-based drying conditions. The results show that drying methods have a clear influence on the microstructure development, on small particle distributions in the coating layer and also on the mobility of particles during consolidation. It is concluded that colloidal properties can significantly impact coating layer shrinkage as well as the internal solids concentration profile. Visualisations of particle system development in time and comparison of systems at different conditions are useful in illustrating coating layer structure formation mechanisms. The results aid in understanding the underlying mechanisms of pigment coating layer consolidation. Guidance is given regarding the relationship between coating process conditions and internal coating slurry properties and their effects on the microstructure of the coating.

Some defects in two-dimensional spin-1/2 Heisenberg antiferromagnets: a numerical study of magnetic effects

En del av de intressantaste fenomenen inom dagens materialfysik uppstår ur ett intrikat samspel mellan myriader av elektroner. Högtemperatursupraledare är det mest berömda exemplet. Varken klassiska teorier eller modeller där elektronerna är oberoende av varandra kan förklara de häpnadsväckande effekterna i de starkt korrelerade elektronsystemen. I vissa kopparoxider, till exempel La2CuO4, är det känt att valenselektronerna till följd av en stark ömsesidig växelverkan lokaliseras en och en till kopparatomerna i föreningens CuO2 plan. Laddningarnas inneboende magnetiska moment—spinnet—får då en avgörande roll för materialets elektriska och magnetiska egenskaper, vilka i exemplets fall kan beskrivas med Heisenbergmodellen som är den grundläggande teoretiska modellen för mikroskopisk magnetism. Men exakt varför föreningarna kan bli supraledande då de dopas med överskottsladdningar är än så länge en obesvarad fråga. Min avhandling undersöker orenheters inverkan på Heisenbergmodellens magnetiska egenskaper—ett problem av både experimentell och teoretisk relevans. En etablerad numerisk metod har använts—en kvantmekanisk Monte Carlo teknik—för att utföra omfattande datorsimuleringar av den matematiska modellen på två dedikerade Linux datorkluster. Arbetet hör till området beräkningsfysik. De teoretiska modellerna för starkt korrelerade elektronsystem, däribland Heisenbergmodellen, är ytterst invecklade matematiskt sett och de kan inte lösas exakt. Analytiska utredningar bygger för det mesta på antaganden och förenklingar vars inverkningar på slutresultatet är ofta oklara. I det avseende kan numeriska studier vara exakta, det vill säga de kan behandla modellerna som de är. Oftast behövs bägge tillvägagångssätten. Den röda tråden i arbetet har varit att numeriskt testa vissa högaktuella analytiska förutsägelser rörande effekterna av orenheter i Heisenbergmodellen. En del av dem har vi på basen av mycket noggranna data kunnat bekräfta. Men våra resultat har också påvisat felaktigheter i de analytiska prognoserna som sedermera delvis reviderats. En del av avhandlingens numeriska upptäckter har i sin tur stimulerat till helt nya teoretiska studier.

Stability of Citrus tristeza virus protective isolate 'Pêra IAC' according to SSCP analysis of old and new lines of three sweet orange varieties

Clonal cleaning, followed by pre-immunization with protective complexes of Citrus tristeza virus(CTV), allowed the commercial cultivation of Pêra sweet orange, a variety that has great importance for Brazilian citriculture but is sensitive to the virus. The use of mild protective isolates in other citrus varieties, even those more tolerant to CTV, can also be of interest to prevent the spread of severe isolates. The aim of this study was to characterize, by means of SSCP (Single Strand Conformational Polymorphism) analysis of the coat protein gene, CTV isolates present in plants of the sweet orange cultivars Pêra, Hamlin and Valencia propagated from four budwood sources: 1) old lines, 2) nucellar lines, 3) shoot-tip-grafted lines, and 4) shoot-tip-grafted lines pre-immunized with the mild CTV protective isolate 'PIAC'. We also evaluated the correlation of the obtained SSCP patterns to stem pitting intensity, tree vigor and fruit yield. SSCP results showed low genetic diversity among the isolates present in different trees of the same variety and same budwood source and, in some cases, in different budwood sources and varieties. Considering tristeza symptoms, lower intensity was noted for plants of new, shoot-tip-grafted and pre-immunized shoot-tip-grafted lines, compared to old lines of the three varieties. The observed SSCP patterns and symptomatology suggested that more severe CTV complexes infect the plants of old lines of all three varieties. The protective complex stability was observed in the SSCP patterns of CTV isolates of some shoot-tip-grafted and pre-immunized clones. It was concluded that the changes detected in other electrophoretic profiles of this treatment did not cause loss of the protective capacity of CTV isolate 'PIAC' inoculated in the pre-immunization.