Simple, inexpensive mass spectrometric analyzer for thermogravimetry

A low-cost mass spectrometer attachment for thermogravimetric analysis has been constructed from readily available commercial instruments and components. The benefits of this set-up include excellent mass-flow repeatability, simple design, and significantly lower adoption cost as opposed to ready-built commercial solutions. The inclusion of an open source software package allows semi-automated, highly simplified data analysis. The results from the instrument show excellent sensitivity for small volumes of evolved gas, as well as highly reproducible signal strengths. The GUI-based software package provides data analysis in a way that is very intuitive and that can be easily modified to work with a broad range of TG instruments.     

Quantitative and pharmacokinetic analysis of naloxone in plasma using high-performance liquid chromatography with electrochemical detection and solid-phase extraction

In this study we present a method for measuring naloxone in plasma after intravenous and oral administration of naloxone to humans, in order to study its pharmacokinetic profile. The method consists of a solid-phase extraction step followed by detection on a high-performance liquid chromatographic (HPLC) system equipped with an electrochemical dual-electrode detector. The extraction step employs cyanopropyl columns optimized for naloxone extraction to allow for elution of naloxone by the HPLC mobile phase; this eluate is then directly injected in the HPLC instrument. The HPLC system employs a radial compression phenyl column with a mobile phase containing 18% (v/v) acetonitrile and pentanesulfonic acid as ion-pairing agent; this system shows extraordinary high plate counts for naloxone. The detection limit is 3 ng (signal-to-noise ratio = 3) free naloxone per ml plasma. Following intravenous injection of 30 mg naloxone hydrochloride in two subjects, it was possible to determine the free naloxone concentration in the plasma for 8 h, more than four times the half-life of naloxone in plasma in humans.     

Bayesian nonparametric estimation of first passage distributions in semi‐Markov processes

Bayesian nonparametric (BNP) models provide a flexible tool in modeling many processes. One area that has not yet utilized BNP estimation is semi‐Markov processes (SMPs). SMPs require a significant amount of computation; this, coupled with the computation requirements for BNP models, has hampered any applications of SMPs using BNP estimation. This paper presents a modeling and computational approach for BNP estimation in semi‐Markov models, which includes a simulation study and an application of asthma patients' first passage from one state of control to another.     

Visible Light Cross‐Linking of Gelatin Hydrogels Offers an Enhanced Cell Microenvironment with Improved Light Penetration Depth

In this study, the cyto‐compatibility and cellular functionality of cell‐laden gelatin‐methacryloyl (Gel‐MA) hydrogels fabricated using a set of photo‐initiators which absorb in 400–450 nm of the visible light range are investigated. Gel‐MA hydrogels cross‐linked using ruthenium (Ru) and sodium persulfate (SPS), are characterized to have comparable physico‐mechanical properties as Gel‐MA gels photo‐polymerized using more conventionally adopted photo‐initiators, such as 1‐[4‐(2‐hydroxyethoxy)‐phenyl]‐2‐hydroxy‐2‐methyl‐1‐propan‐1‐one (Irgacure 2959) and lithium phenyl(2,4,6‐trimethylbenzoyl) phosphinate (LAP). It is demonstrated that the Ru/SPS system has a less adverse effect on the viability and metabolic activity of human articular chondrocytes encapsulated in Gel‐MA hydrogels for up to 35 days. Furthermore, cell‐laden constructs cross‐linked using the Ru/SPS system have significantly higher glycosaminoglycan content and re‐differentiation capacity as compared to cells encapsulated using I2959 and LAP. Moreover, the Ru/SPS system offers significantly greater light penetration depth as compared to the I2959 system, allowing thick (10 mm) Gel‐MA hydrogels to be fabricated with homogenous cross‐linking density throughout the construct. These results demonstrate the considerable advantages of the Ru/SPS system over traditional UV polymerizing systems in terms of clinical relevance and practicability for applications such as cell encapsulation, biofabrication, and in situ cross‐linking of injectable hydrogels.     

A simple strategy for constructing bounded convection schemes for unstructured grids

Due to the great geometrical flexibility, popularity for unstructured grid methods in fluid dynamics has been increasing in recent years. In parallel with this interest there is a need for bounded second or higher order convection schemes which can be implemented easily in the unstructured setting. In the present work a simple strategy for achieving convective boundedness in the context of a vertex‐centered unstructured finite volume algorithm is demonstrated. Testing is carried out on an inviscid oblique step problem using both structured and unstructured grid arrangements. Further testing for numerical diffusion is done using a distorted grid in a two dimensional channel. The proposed scheme is straightforward to implement and is found to perform well for the cases considered. The overall algorithm converges well and the limiter appears to introduce little extra numerical diffusion beyond that inherently present in the base scheme. Copyright © 2004 John Wiley & Sons, Ltd.     

Novel synthesis and structural analysis of ferrihydrite

Naturally occurring ferrihydrite is both impure and difficult to isolate, so the numerous applications and interesting properties of ferrihydrite have spurred the development of various synthetic techniques. Nearly all techniques are based on the hydrolysis of an iron salt and require careful control of temperature, pH, and concentration. In this Article, we report a new synthetic method which does not require such control and is perhaps the fastest and simplest route to synthesizing ferrhydrite. XRD, TEM, BET, and chemical purity characterizations show that the chemically pure, 2-line ferrihydrite product consists of crystallites 2-6 nm in diameter which aggregate to form mesoporous, high surface area agglomerates that are attractive candidates for the many adsorption applications of ferrihydrite. X-ray PDF data were also collected for the ferrihydrite product and refined against the hexagonal structural model recently proposed by Michel et al. These analyses suggest that ferrihydrite has a consistent, repeatable structure independent of variation in the synthetic method, water content of the sample, or particle size of the crystallites, and this structure can be adequately described by the proposed hexagonal model.     

Thermal Conductivity Measurement of Gases by the Transient Short-Hot-Wire Method

Measurements of the thermal conductivity of helium and hydrogen are performed using the transient short-hot-wire method. The short hot wire is made of platinum and has a diameter of about 10 μm and a length of about 15 mm. It is attached by spot welding to platinum terminals with a diameter of 1.5 mm. The probe is inserted into the sample vessel that has a volume of 35 cm³ and an inner diameter of 30 mm. The thermal conductivity is evaluated by comparing a numerical solution of the heat conduction in and around the short wire with the experimentally obtained temperature rise of the wire. The measured thermal conductivities show good reproducibility. Also, the measured thermal conductivities agree with the reference equations within a deviation of ± 1%.     

Size-dependence of the heat capacity and thermodynamic properties of hematite (α-Fe2O3)

The heat capacity of a 13 nm hematite (α-Fe₂O₃) sample was measured from T = (1.5 to 350) K using a combination of semi-adiabatic and adiabatic calorimetry. The heat capacity was higher than that of the bulk which can be attributed to the presence of water on the surface of the nanoparticles. No anomaly was observed in the heat capacity due to the Morin transition and theoretical fits of the heat capacity below T = 15 K show a small T³ dependence (due to lattice contributions) with no T^3/2 dependence. This suggests that there are no magnetic spin-wave contributions to the heat capacity of 13 nm hematite. The use of a large linear term to fit the heat capacity below T = 15 K is most likely due to superparamagnetic contributions. A small anomaly within the temperature range (4 to 8) K was attributed to the presence of uncompensated surface spins.     

Estimation of Uncertainty in an Analytical Inverse Heat Conduction Solution

The method of sequential perturbations is applied to find the uncertainty in estimated surface temperature and heat flux from a two-dimensional analytical inverse heat conduction problem related to impinging jet quenching experiments. It is shown that for meaningful uncertainty estimates, the inverse solution itself must be formulated such that it can be interpreted as giving average surface conditions over a small period of time and space. A procedure for estimating the time and space resolution limits of the solution is proposed.     

On techniques for the measurement of the mass fractal dimension of aggregates

A review is presented of a number of techniques available for the characterisation of the structure of aggregates formed from suspensions of sub-micron particles. Amongst the experimental techniques that have been commonly used are scattering (light, X-ray or neutron), settling and imaging and these are the focus of this work. The theoretical basis for the application of fractal geometry to characterisation of flocs and aggregates is followed by a discussion of the strengths and limitations of the above techniques. Of the scattering techniques available, light scattering provides the greatest potential for use as a tool for structure characterisation even though interpretation of the scattered intensity pattern is complicated by the strong interaction of light and matter. Restructuring further complicates the analysis. Although settling has long been used to characterise particle behaviour, the absence of an accurate permeability model limits the technique as a means of determining the porosity of fractal aggregates. However, it can be argued that the determination of fractal dimension is relatively unaffected. The strength of image analysis lies in its ability to provide a great deal of information about particle morphology and the weaknesses lie in the difficulties with image processing and sample size as this is a particle counting technique. There are very few papers which compare the fractal dimension measured by more than one technique. Light scattering potentially provides a useful tool for checking settling results. However, further work is required to develop proper models for aggregate permeability and flow-through effects.