Towards real-time understanding of processes in pharmaceutical powder technology

There is a need for better understanding of the processes and new ideas to develop traditional pharmaceutical powder manufacturing procedures. Process analytical technology (PAT) has been developed to improve understanding of the processes and establish methods to monitor and control processes. The interest is in maintaining and even improving the whole manufacturing process and the final products at real-time. Process understanding can be a foundation for innovation and continuous improvement in pharmaceutical development and manufacturing. New methods are craved for to increase the quality and safety of the final products faster and more efficiently than ever before. The real-time process monitoring demands tools, which enable fast and noninvasive measurements with sufficient accuracy. Traditional quality control methods have been laborious and time consuming and they are performed off line i.e. the analysis has been removed from process area. Vibrational spectroscopic methods are responding this challenge and their utilisation have increased a lot during the past few years. In addition, other methods such as colour analysis can be utilised in noninvasive real-time process monitoring. In this study three pharmaceutical processes were investigated: drying, mixing and tabletting. In addition tablet properties were evaluated. Real-time monitoring was performed with NIR and Raman spectroscopies, colour analysis, particle size analysis and compression data during tabletting was evaluated using mathematical modelling. These methods were suitable for real-time monitoring of pharmaceutical unit operations and increase the knowledge of the critical parameters in the processes and the phenomena occurring during operations. They can improve our process understanding and therefore, finally, enhance the quality of final products.

Time dependence of effective slip on textured hydrophobic surfaces

In this paper, we present results on water flow past randomly textured hydrophobic surfaces with relatively large surface features of the order of 50 µm. Direct shear stress measurements are made on these surfaces in a channel configuration. The measurements indicate that the flow rates required to maintain a shear stress value vary substantially with water immersion time. At small times after filling the channel with water, the flow rates are up to 30% higher compared with the reference hydrophilic surface. With time, the flow rate gradually decreases and in a few hours reaches a value that is nearly the same as the hydrophilic case. Calculations of the effective slip lengths indicate that it varies from about 50 µm at small times to nearly zero or “no slip” after a few hours. Large effective slip lengths on such hydrophobic surfaces are known to be caused by trapped air pockets in the crevices of the surface. In order to understand the time dependent effective slip length, direct visualization of trapped air pockets is made in stationary water using the principle of total internal reflection of light at the water-air interface of the air pockets. These visualizations indicate that the number of bright spots corresponding to the air pockets decreases with time. This type of gradual disappearance of the trapped air pockets is possibly the reason for the decrease in effective slip length with time in the flow experiments. From the practical point of usage of such surfaces to reduce pressure drop, say, in microchannels, this time scale of the order of 1 h for the reduction in slip length would be very crucial. It would ultimately decide the time over which the surface can usefully provide pressure drop reductions. ©2009 American Institute of Physics

Estimating crop area using seasonal time series of enhanced vegetation index from MODIS satellite imagery

Cereal grain is one of the main export commodities of Australian agriculture. Over the past decade, crop yield forecasts for wheat and sorghum have shown appreciable utility for industry planning at shire, state, and national scales. There is now an increasing drive from industry for more accurate and cost-effective crop production forecasts. In order to generate production estimates, accurate crop area estimates are needed by the end of the cropping season. Multivariate methods for analysing remotely sensed Enhanced Vegetation Index (EVI) from 16-day Moderate Resolution Imaging Spectroradiometer (MODIS) satellite imagery within the cropping period (i.e. April-November) were investigated to estimate crop area for wheat, barley, chickpea, and total winter cropped area for a case study region in NE Australia. Each pixel classification method was trained on ground truth data collected from the study region. Three approaches to pixel classification were examined: (i) cluster analysis of trajectories of EVI values from consecutive multi-date imagery during the crop growth period; (ii) harmonic analysis of the time series (HANTS) of the EVI values; and (iii) principal component analysis (PCA) of the time series of EVI values. Images classified using these three approaches were compared with each other, and with a classification based on the single MODIS image taken at peak EVI. Imagery for the 2003 and 2004 seasons was used to assess the ability of the methods to determine wheat, barley, chickpea, and total cropped area estimates. The accuracy at pixel scale was determined by the percent correct classification metric by contrasting all pixel scale samples with independent pixel observations. At a shire level, aggregated total crop area estimates were compared with surveyed estimates. All multi-temporal methods showed significant overall capability to estimate total winter crop area. There was high accuracy at pixel scale (>98% correct classification) for identifying overall winter cropping. However, discrimination among crops was less accurate. Although the use of single-date EVI data produced high accuracy for estimates of wheat area at shire scale, the result contradicted the poor pixel-scale accuracy associated with this approach, due to fortuitous compensating errors. Further studies are needed to extrapolate the multi-temporal approaches to other geographical areas and to improve the lead time for deriving cropped-area estimates before harvest.

Multi-time scale analysis applied to long time simulation of power systems

The results are presented of applying multi-time scale analysis using the singular perturbation technique for long time simulation of power system problems. A linear system represented in state-space form can be decoupled into slow and fast subsystems. These subsystems can be simulated with different time steps and then recombined to obtain the system response. Simulation results with a two-time scale analysis of a power system show a large saving in computational costs.

Time evolution of graphene growth on SiC as a function of annealing temperature

We followed by X-ray Photoelectron Spectroscopy (XPS) the time evolution of graphene layers obtained by annealing 3C SiC(111)/Si(111) crystals at different temperatures. The intensity of the carbon signal provides a quantification of the graphene thickness as a function of the annealing time, which follows a power law with exponent 0.5. We show that a kinetic model, based on a bottom-up growth mechanism, provides a full explanation to the evolution of the graphene thickness as a function of time, allowing to calculate the effective activation energy of the process and the energy barriers, in excellent agreement with previous theoretical results. Our study provides a complete and exhaustive picture of Si diffusion into the SiC matrix, establishing the conditions for a perfect control of the graphene growth by Si sublimation.

Separation of 5-methylcytosine-rich DNA using immobilized antibody

Anti-(5-methylcytosine) antibodies were immobilized on glutaraldehyde-activated Indion 48-R, a polystyrene resin with amino groups. Immobilized antibody was very stable and could be used several times without any apparent change in the initial binding capacity of the antibody-matrix. Fractions of total DNA from various animal and plant sources were retained on this column and could be eluted quantitatively with 1.0 m NaCl. The bound fraction was further characterized for its 5-methylcytosine content by restriction enzyme digestion patterns.

Past-day recall of sedentary time: Validity of a self-reported measure of sedentary time in a university population

Background Sedentary behaviour is associated with several deleterious health consequences. Although device-based measures of sedentary time are available, they are costly and do not provide a measure of domain specific sedentary time. High quality self-report measures are necessary to accurately capture domain specific sedentary time, and to provide an alternative to devices when cost is an issue. In this study, the Past-day Adults’ Sedentary Time (PAST) questionnaire, previously shown to have acceptable validity and reliability in a sample of breast cancer survivors, was modified for a university sample and validity of the modified questionnaire was examined compared with activPAL. Methods Participants (n = 58, age = 18–55 years, 48% female, 66% students) were recruited from the University of Queensland (students and staff). They answered the PAST questionnaire, which asked about time spent sitting or lying down for work, study, travel, television viewing, leisure-time computer use, reading, eating, socialising and other purposes, during the previous day. Time reported for these questions was summed to provide a measure of total sedentary time. Participants also wore an activPAL device for the full day prior to completing the questionnaire and recorded their wake and sleep times in an activity log. Total waking sedentary time derived from the activPAL was used as the criterion measure. Correlation (Pearson's r) and agreement (Bland–Altman plots) between PAST and activPAL sedentary time were examined. Results Participants were sedentary (activPAL-determined) for approximately 66% of waking hours. The correlation between PAST and activPAL sedentary time for the whole sample was r = 0.50 [95% confidence interval (CI) = 0.28–0.67]; and higher for non-students (r = 0.63, 95% CI = 0.26–0.84) than students (r = 0.46, 95% CI = 0.16–0.68). Bland–Altman plots revealed that the mean difference between the two measures was 19 min although limits of agreement were wide (95% limits of agreement −4.1 to 4.7 h). Discussion The PAST questionnaire provides an acceptable measure of sedentary time in this population, which included students and adults with high workplace sitting. These findings support earlier research that questionnaires employing past-day recall of sedentary time provide a viable alternative to existing sedentary behaviour questionnaires.

Development of analytical methods for the separation of plutonium, americium, curium and neptunium from environmental samples

In this work, separation methods have been developed for the analysis of anthropogenic transuranium elements plutonium, americium, curium and neptunium from environmental samples contaminated by global nuclear weapons testing and the Chernobyl accident. The analytical methods utilized in this study are based on extraction chromatography. Highly varying atmospheric plutonium isotope concentrations and activity ratios were found at both Kurchatov (Kazakhstan), near the former Semipalatinsk test site, and Sodankylä (Finland). The origin of plutonium is almost impossible to identify at Kurchatov, since hundreds of nuclear tests were performed at the Semipalatinsk test site. In Sodankylä, plutonium in the surface air originated from nuclear weapons testing, conducted mostly by USSR and USA before the sampling year 1963. The variation in americium, curium and neptunium concentrations was great as well in peat samples collected in southern and central Finland in 1986 immediately after the Chernobyl accident. The main source of transuranium contamination in peats was from global nuclear test fallout, although there are wide regional differences in the fraction of Chernobyl-originated activity (of the total activity) for americium, curium and neptunium.

Separation of 35S-Labeled thionucleosides of Escherichia coli and Pseudomonas aeruginosa transfer RNAs on a phosphocellulose column

35S-Labeled thionucleosides prepared from Escherichia coli and Pseudomonas aeruginosa tRNAs were chromatographed separately on a phosphocellulose column with a linear salt gradient of 0.005–0.1 M ammonium formate (pH 3.9). The thionucleosides of E. coli tRNA were quantitatively separated into four peaks which were identified using authentic samples as 4-thiouridine (78 %), 2-methylthio-N6-isopentenyladenosine (8 %), 2-thiocytidine (2.5 %) and 5-methylaminomethyl-2-thiouridine (11.5 %). In the case of P. aeruginosa tRNA four radioactive thionucleoside peaks were also observed. One major difference was the almost complete absence of 2-methylthio-N6-isopentenyladenosine and the presence of a new peak of radioactivity in the nucleosides of P. aeruginosa. The relative proportions of the various thionucleosides were found to be different in E. coli and P. aeruginosa tRNAs.

Open-circuit potential-time transient of the magnesium anode

On interrupting polarisation, the magnesium anode exhibits a negative overshoot in potential followed by a slow recovery to a steady state value. A model has been proposed to explain the opencircuit potential-time transient in terms of a spontaneous passivation of the metal and the consequent changes in the corrosion potential. Theoretical expressions have been derived for the timedependence of the open-circuit electrode potential. Calculated, potential-time curves thus obtained are in qualitative agreement with experimental data. A possible application of this phenomenon to develop non-destructive quality control tests of Mg, Li and Al-based dry cells has been pointed out.

Calendar of events taken from the Occident, Asmonean, and Stein's Chronological Handbuch

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Separation of sulfur-containing components of transfer ribonucleic acid on Bio-Gel P-2 and Sephadex G-10 columns

S-Labeled nucleosides of E. coli tRNA and some of the derivatives of thionucleosides were separated on Bio-Gel P-2 and Sephadex G-10 columns employing buffers of low salt concentration and high pH.

A numerical method for separation of stresses in photo-orthotropic elasticity

A numerical method is suggested for separation of stresses in photo-orthotropic elasticity using the numerical solution of compatibility equation for orthotropic case. The compatibility equation is written in terms of a stress parameter S analogous to the sum of principal stresses in two-dimensional isotropic case. The solution of this equation provides a relation between the normal stresses. The photoelastic data give the shear stress and another relation between the two normal stresses. The accuracy of the numerical method and its application to practical problems are illustrated with examples.

A method for separation of stresses in Two- and three-dimensional photoelasticity

A method for separation of stresses in two and three-dimensional photo elasticity using the harmonisation ofjrst stress invariant along a straight section is deve- ,dped. For two-dimensions, the equations of equilibrium are reformulated in terms ojsum and difference of normal stresses and relations are obtained which can be used for harmonisation of the first invariant of stress along a straight section. A similar procedure is adopted for three-dimensions by making use of the Beltrmi-MicheN equations. The new relations are used in finite d~yerencefo rm to evaluate the sum of normal stresses along straight sections in a three-dimensional body. The method requires photoelastic data along the section as well ~rra djacent sections. This method could be used as an alternative to the shear d@erence method for separation of stresses in photoelasticity. 7he accuracy and reliability of the method is ver$ed by applying the method to problems whose solutions are known.