The ales laboratory automation system

A systenm for the automation of the analytical activities of a chemical laboratory is described. The system dieals with investigations of physical and chemical characteristics of telecommunication materials for prototype development and quality control. The architecture, software development and interfacing of different analytical instruments (mainly for calorimetry, spectroscopy, electrochemistry, chromatography and mechanics) for the ALES (Automatzione del Laboratorio Elettrochimico SIP) system are discussed in terms of analytical and management performance.     

Monte Carlo simulation of crystal-fluid coexistence states in the hard-sphere system under gravity with stepwise control

Monte Carlo (MC) simulations were performed for hard spheres (with diameter sigma and mass m) placed between well-separated upper and lower hard walls. A periodic boundary condition was imposed in the horizontal direction. The system was exposed to the gravitational field with the acceleration due to gravity g. After preparing a melt as the initial state, g was increased stepwise up to mgsigma/k(B)T(identical with g(*))=1.5 or 2.0 with an increment Deltag(*) = 0.1; k(B)T is the temperature multiplied by Boltzmann's constant. We maintained g(*) at each value for 2.0 x 10(5) MC cycles. The transition of the system into a metastable state such as a polycrystalline state due to trapping phenomena was successfully avoided. A monotonic increase and subsequent saturation were observed for the development of the crystalline region formed at the bottom of the system. The development of this region accompanied a shrinkage of the defective (or less ordered) crystalline region that was formed between the bottom region and the fluid phase. As the development of the bottom region almost saturated, the defective region grew upward again.     

A modular microfluidic system for deoxyribonucleic acid identification by short tandem repeat analysis

Microfluidic technology has been utilized in the development of a modular system for DNA identification through STR (short tandem repeat) analysis, reducing the total analysis time from the ∼6 h required with conventional approaches to less than 3 h. Results demonstrate the utilization of microfluidic devices for the purification, amplification, separation and detection of 9 loci associated with a commercially-available miniSTR amplification kit commonly used in the forensic community. First, DNA from buccal swabs purified in a microdevice was proven amplifiable for the 9 miniSTR loci via infrared (IR)-mediated PCR (polymerase chain reaction) on a microdevice. Microchip electrophoresis (ME) was then demonstrated as an effective method for the separation and detection of the chip-purified and chip-amplified DNA with results equivalent to those obtained using conventional separation methods on an ABI 310 Genetic Analyzer. The 3-chip system presented here demonstrates development of a modular, microfluidic system for STR analysis, allowing for user-discretion as to how to proceed after each process during the analysis of forensic casework samples.     

An Improved System for the Aqueous Lipshutz–Negishi Cross‐Coupling of Alkyl Halides with Aryl Electrophiles

The development of a palladacyclic precatalyst supported by a new biaryl(dialkyl)phosphine ligand (VPhos) in combination with octanoic acid/sodium octanoate as a simple and effective surfactant system provided an improved catalyst system for the rapid construction of a broad spectrum of alkylated scaffolds from alkyl zinc reagents generated in situ.     

Effect of UV radiation on the neonatal skin immune system- implications for melanoma

The neonatal immune environment and the events that occur during this time have profound effects for the adult period. While protective immune responses can develop, the neonatal immune system, particularly the skin immune system (SIS), tends to promote tolerance. With this information we undertook a number of studies to identify unique aspects of skin during the neonatal period. Proteomics revealed proteins uniquely expressed in neonatal, but not adult, skin (e.g. Stefin A, peroxiredoxins) and these may have implications in the development of SIS. Vitamin D was found to have a modulating role on SIS and this was apparent from the early neonatal period. Exposure of the neonatal skin to UV radiation altered the microenvironment resulting in the generation of regulatory T cells, which persisted in adult life. As the development of UV radiation-induced melanoma can occur following a single high dose (equivalent to burning in adults) to transgenic mice (hepatocyte growth factor/scatter factor or TPras) during the neonatal period, the early modulating events which lead to suppression may be relevant for the development of UV radiation-induced human melanoma. Any attempt to produce effective melanoma immunotherapy has to accommodate and overcome these barriers. Margaret Kripke's pioneering work on UV-induced immunosuppression still remains central to the understanding of the development of melanoma and how it frequently escapes the immune system.     

Automatic mass spectrometry method development for drug discovery: application in metabolic stability assays

High-throughput metabolic screening has been requested routinely to keep pace with high-throughput organic synthesis. Liquid chromatography/tandem mass spectrometry (LC/MS/MS) with a fast gradient has become the method of choice for the task due to its sensitivity and selectivity. We have developed an automated system that consists of a robotic system for in vitro incubation and a commercially available software package for automatic MS/MS method development. A short, generic LC gradient and MS conditions that are applicable to most compounds have been developed to minimize the method development time and data analysis. This system has been used to support a number of in vitro screening assays in early drug discovery phase including microsomal stability and protein binding.     

Integration of computer-assisted statistical scanning optimization system in HPLC

Three computer-assisted statistical scanning methods, the monofactor optimization system (MOS), multicomponent solvent optimization system (MSOS), and difactor optimization system (DOS) for optimizing HPLC separations, have been integrated to produce the optimization system of HPLC (OS-L). The method proposes the complementary use of these techniques, maximizing their strengths while compensating for their weaknesses. The result of OS-L is a method development strategy which obtains simple solutions for simple separation problems and reserves the more complex solutions for difficult separations.     

Environmental certification: a scientific tool for sustainability. Evaluation of possible indicators for the environmental performance evaluation (EPE) of Ravenna province (Italy)

Environmental certification is becoming the main tool for application of sustainable development principles. The European Regulation Emas and the international standard ISO 14001 both require for certification, to perform an environmental management system to prevent environmental impacts and to continuously improve environmental performance. For a good environmental performance evaluation (EPE), certification needs to use scientific methodologies and to interface with scientific research; here we proposed emergy analysis as a valid method for EPE and emergetic environmental performance and condition indicators (EPIs, ECIs) to monitor a territorial system: Ravenna province (Italy). Together with emergy indicators were selected other indicators for a deeper EPE: emitted/adsorbed CO2, energy consumptions, air and water pollution measures. The paper showed that Ravenna system has a good environmental performance and demonstrated how different indicators from the most advanced chemical research (chemical-physical, analytical, etc.) contribute to a complete EPE of a complex territorial system and are useful for environmental certification and sustainable development.     

Development of an Automatic Electrochemical System for Differential Pulse Amperometry and Its Application for Se(IV) Determination

This work presents the development of an automatic system for differential pulse amperometry (DPA) with electrochemical deposition. The system consists of a microcomputer, running a home‐made software, connected to a commercial potentiostat through a data acquisition board. The system was applied for selenium determination using gold electrode and flow injection analysis (FIA). Analytical curves were obtained in the concentration range of 20 to 400 μg L^?1 for Se(IV), with a calculated detection limit of 6 μg L^?1. The analysis results for fish samples doped with Se(IV) and digested in a microwave oven showed recoveries above 93%.     

Further progress in atom transfer radical polymerizations conducted in a waterborne system

An improved atom transfer radical polymerization (ATRP) process was developed for use in a waterborne miniemulsion system. To conduct a successful ATRP in a heterogeneous waterborne system, it is of great importance to ensure control over the polymerization process while preserving colloidal stability. Efforts devoted to optimization of reaction conditions and improvement in the overall productivity of the process allowed the development of a novel, practical initiation system for ATRP suitable for use in a miniemulsion procedure that can provide copolymers of well-defined composition (e.g., block copolymers) and topologies (e.g., multiarm polymer). © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 3606–3614, 2003     

High-speed analysis of multiplexed short tandem repeats with an electrophoretic microdevice

We report the development of a robust and effective method for multiplexed short tandem repeat (STR) analysis within a chip-based microdevice. The method uses a laser-induced fluorescence detection system and simultaneously detects three- and four-color multiplexed polymerase chain reaction (PCR) samples. Analyses of the eight combined DNA index system (CODIS) STR loci were performed in 20 min with single-base-pair resolution ranging from 0.75 to 1. A simultaneous analysis of fifteen loci-ladders and a gender marker Amelogenin based on the PowerPlexTM 16 System was achieved in less than 35 min. The system is capable of repetitive operation and may be extended to high-throughput multilane devices that could be readily interfaced to an automated sample loading system.     

A Compton suppression gamma-ray spectrometer for low level counting

A Compton suppression gamma-ray spectrometry system has been evaluated for its use as a low level radioactivity counting facility. The system consists of a premium quality Ge(Li) detector surrounded by a shield of NaI(T1) detector material. Compton suppression is obtained by operating the two detector systems in anti-coincidence. Spectrum collection hardware consists of a NP11-A (DEC) interface for two ADC's and a PDP 11/T 10 minicomputer with 64 K byte core memory. Software development and system operation modes are described. System performance as a function of physical characteristics of the sample, scattering angle and gamma-photon energy, is discussed. Continum reduction for cascaded gamma-transitions and natural backgorund are considered separately.     

Recent progress of photo‐resin for rapid prototyping, “resin for stereolithography”

A main goal for manufacturing systems is to shorten lead‐time for the development of new products. An important challenge is to make sound decisions at early stages of product development where committed costs are low which leads us to obtain a lower total cost. This could mean that incurred costs are higher in the beginning where more work has to be done in terms of learning the market, developing the product and the production system. An important feature is to avoid changes at later stages where the incurred costs are high. The stereolithography using photo curable liquid resin is important for the manufacturing. The technology based on the stereolithography has been widely accepted due to the phenomena of spreading “Information Technology (IT)” and three‐dimensional computer aided design (3D CAD) system. The stereolithography technique has become very popular in the field of automotive, home‐electronics industries. In this paper the photo curable liquid resins for the stereolithography system are reviewed.     

Development and applications of a microfluidic reactor with multiple analytical probes

We report the development of a versatile microfluidic (MF) reactor with multiple analytical probes, which can be used for (i) quantitative characterisation of molecular vibrational signatures of reactants or products, (ii) the localised real-time monitoring of temperature and (iii) site-specific measurements of pH of the reaction system. The analytical probes utilised for in situ reaction analysis include an ATR-FTIR probe, a temperature probe, and a pH probe. We demonstrate the applications of the MF reactor with integrated probes for the parallel monitoring of multiple variables in acid/base neutralisation reaction, of changes in buffer pH, temperature, and vibrational absorption bands, and for monitoring the kinetics of the reaction between CO(2) and a buffer system with therapeutic applications.     

Novel three-dimensional capillary electrophoresis system for complex and trace analysis

A novel triple column capillary electrophoresis system is described. Design specifications facilitate method development and analyses by providing on-line, selective, pre-concentration and clean-up of both high (ml) and low (microl) volumes of specific analytes in two dimensions and separation via an additional third dimension. The system described additionally provides four distinct detection capabilities via both contactless conductivity and UV. The addition of a third dimension to the previously reported "coupled-column" systems, and further modifications made, has allowed for optimal identification, separation, and quantitation of micro-components in complex mixtures. The ability to perform both capillary zone electrophoretic and isotachophoretic separations on-line and in any combination enhances the scope for rapid analytical method development and analysis of complex or trace sample components.     

Microwave assisted reduction of Se(VI) to Se(IV) and determination by HG/FI-ICP/MS for inorganic selenium speciation

Speciation of inorganic selenium using hydride generation method is a widespread analytical method nowadays. However, a reduction step of Se(VI) to Se(IV) is necessary as the hydride-forming species is HSeO(3)(-) (oxydation state+IV). This paper describes the development of a batch assisted microwave system allowing a rapid (<5 min) conversion of Se(VI) to Se(IV). Hydride generation is performed by a flow injection system and detection by ICP/MS. Detection limits of 6 and 8 pg for Se(IV) and for Se(VI) (by using a sample loop of 200 mul) respectively have been achieved. This method has been validated by participating in a European certification exercise for inorganic Se speciation in aqueous solutions.     

Practical solvent system selection for counter-current separation of pharmaceutical compounds

Counter-current chromatography (CCC) is a technique that shows a lot of potential for large scale purification. Its usefulness in a "research and development" pharmaceutical environment has been investigated, and the conclusions are shown in this article. The use of CCC requires the development of an appropriate solvent system (a parameter of critical importance), a process which can be tedious. This article presents a novel strategy, combining a statistical approach and fast HPLC to generate a three-dimensional partition coefficient map and rapidly predict an optimal solvent system. This screen is performed in half a day and involves 9 experiments per solvent mixture. Test separations were performed using that screen to ensure the validity of the method.     

A PET imaging system dedicated to mammography

The imaging system Clear-PEM for positron emission mammography, under development within the framework of the Crystal Clear Collaboration at CERN, is presented. The detector is based on pixelized LYSO crystals optically coupled to avalanche photodiodes (APD) and readout by a fast low-noise electronic system. A dedicated digital trigger and data acquisition system is used for on-line selection of coincidence events with high efficiency, large bandwidth and negligible dead-time. The detector module performance was characterized in detail.     

Development of a trace gas stable isotope capture system in a mobile laboratory for temporal and spatial sampling of field and laboratory experiments

We describe the development of a novel mobile field laboratory, purposely designed for the automated capture and subsequent stable isotopic analyses of multiple gas samples. The multiple capture system is integrated into a mobile laboratory that is fully capable of measuring the concentration of carbon dioxide, methane and nitrous oxide trace gases in a flow-through system connected to a gas chromatograph fitted with both electron capture and flame ionisation detectors. The capture of gases is achieved by routing samples through a series of 135 mL gas flasks that are sealed by micro-solenoid valves triggered by a timing system. Trace gas light stable isotope ratio mass spectrometry can then be carried out on gas samples collected by the system (NERC (15)N Stable Isotope Facility). The excitingly unique potential of the system to the ecological research field is that it will allow the collection of cyclical data for three different trace gases both in real-time and in situ. We present data arising from the validation of this mobile system as well as a preliminary experimental assessment of this technique. This technique was used to measure delta(13)C in CO(2) and CH(4) in soil gases released from waterlogged cores and delta(13)C-CH(4) values were significantly depleted in wet cores compared with dry ones (p < 0.001).     

Hybrid electro-optical nanosystem for neurons investigation

The scope of this paper is development of a new laboratory-on-a-chip (LOC) device for biomedical studies consisting of a microfluidic system coupled to microelectronic/optical transducers with nanometric features, commonly called biosensors. The proposed device is a hybrid system with sensing element on silicon (Si) chip and microfluidic system on polydimethylsiloxane (PDMS) substrates, taking into accounts their particular advantages. Different types of nanoelectrode arrays, positioned in the reactor, have been investigated as sensitive elements for electrical detection and the recording of neuron extracellular electric activity has been monitorized in parallel with whole-cell patch-clamp membrane current. Moreover, using an additional porosification process the sensing element became efficient for optical detection also. The preliminary test results demonstrate the functionality of the proposed design and also the fabrication technology, the devices bringing advantages in terms enhancement of sensitivity in both optoelectronic detection schemes.