Sequential Injection Ion Chromatography with Flow Injection Post Column Derivatization Capable of Using the Unstable Reagent Murexide to Determine Calcium and Magnesium in a Mixture

A hyphenated sequential injection ion chromatography–flow injection analysis (SIIC–FIA) system is proposed for post column derivatization capable of using murexide, an unstable but commonly available reagent, for the determination of calcium and magnesium in a mixture. A short ion exchange column was modified from a 4.6 mm × 10 mm C18 monolithic guard column. Calcium/magnesium mixture and murexide were used as model analytes and derivatizing agent, respectively. The FIA post column allows the use of unstable chromogenic reagents. The continuous flow of liquid also helped to stabilize the signal baseline during detection. A single concentration based calibration graph was demonstrated. The system requires low volumes of standard/sample (5–50 µL) and mobile phase (4.50 mL), and offers sample throughput at 8 h^?1 without the need for long column calibration. Detection limits were 0.5 and 0.1 µg for Ca²⁺ and Mg²⁺, respectively. Working ranges were 1–5 µg Ca²⁺ and 0.2–1 µg Mg²⁺. Analyses of well and drinking water samples were demonstrated and validated with the standard complexometric titration.     

Sequential injection-ELISA based system for online determination of hyaluronan

Sequential injection-bead-based immunoassay system has been developed. The main purpose is to make immunoassay process more automated by manipulating the precise delivery of micro-volumes of reagents and the precise timing of incubation and washing steps with a computer program that controls the bi-directional syringe pump. The manifold was designed with the aims of reducing back pressure from beads that act as solid surfaces for immobilization of the target substance, reducing dispersion and dilution of the reagent during incubation, and maximizing signal while minimizing incubation time. This was done by introducing air segment to separate the reagent zone from the carrier stream and by using a suitable sensitive detector which, in this case, was an amperometer. In this study, hyaluronan (HA) was used as a target analyte because of its clinical significance as a potential biomarker for liver, bone and cancer diseases. Amount of hyaluronan was determined using competitive enzyme linked immuno sorbent assay (ELISA) based technique where immobilized HA and HA in solution compete to bind with a fixed amount of biotinylated HA-binding proteins (b-HABPs). Upon separation of the two phases, anti-biotin conjugated with enzyme and a suitable substrate were introduced to follow the binding reaction of the immobilized HA and b-HABPs whose degree of binding is indirectly proportional to the amount of HA in solution. A calibration curve was constructed from a series of concentrations of HA standards. Lowest detectable concentration was found to be 1 ng/mL with the dynamic working range of 1-5000 ng/mL and R.S.D. of intra-assay (n = 7) and inter-assay (n = 3) of various HA concentrations were 4-10% and 9-12%, respectively. Used beads could be reused by washing with 2 M guanidine. Total analysis time for this automatic assay was about 30 min as compared to the 5-8 h used in conventional batch well ELISA. The system could be applied to assay HA in human serum.     

Novel approach for mono-segmented flow micro-titration with sequential injection using a lab-on-valve system: a model study for the assay of acidity in fruit juices

A new concept for micro-titration using a "lab-on-valve"(LOV) system with sequential injection of mono-segmented flow is proposed. The performance of the system was demonstrated by the assay of acidity in fruit juices which is based on acid-base neutralization. A standard/sample solution containing citric acid, indicator, sodium hydroxide, were sandwiched between air segments and were aspirated in microliter volumes through a selection valve into a holding coil. The acid, indicator, and base were mixed by flow reversal. After removing air segments, the solution was pushed to the detector for monitoring of the change in absorbance of the indicator color, which depended on the concentration of the remaining base. With LOV, microliter volumes of the solution can be detected without dispersion of the color zone. A calibration graph (plot of absorbance vs. acidity value) in the range of 0.2-1.2% (w/v) as citric acid was established. Sample throughput of 30 sample h(-1) and good reproducibility (RSD = 1.2%, n= 11 for 0.6% acidity) were achieved. The procedure has been applied to determine acidity in fruit juices.     

Simple lab-on-chip approach with time-based detection

A simple lab-on-chip approach with time-based detection is proposed. A platform is made from a piece of acrylic differently shaped channels for introducing sample and reagent(s) using flow manipulation. Time-based changes involving migration of the reaction zone are monitored. The changes can be visually monitored by using a stop-watch with naked eyes observation. Some applications for the determination of ascorbic acid, acetic acid and iron in real samples with different chemistries were demonstrated.     

Preparation and characterization of MgB2 superconductor

The MgB₂ superconductor, synthesized using solid-state and liquid-phase sintering methods, have been characterized for various properties. The upper critical field, irreversibility line and critical current density have been determined using magnetization data. The current-voltage characteristics recorded under an applied magnetic field revealed the existence of vortex glass transition. The surface analysis using X-ray photoelectron spectroscopy shows that MgB₂ is sensitive to atmospheric degradation.     

Gamma-ray spectrometry combined with acceptable knowledge (GSAK): A technique for characterization of certain remote-handled transuranic (RH-TRU) wastes

Gamma-ray spectrometry combined with acceptable knowledge (GSAK) is a technique for the characterization of certain remote-handled transuranic (RH-TRU) wastes. GSAK uses gamma-ray spectrometry to quantify a portion of the fission product inventory of RH-TRU wastes. These fission product results are then coupled with calculated inventories derived from acceptable process knowledge to characterize the radionuclide content of the assayed wastes. GSAK has been evaluated and tested through several test exercises. This paper describes the GSAK approach, while Part II presents the test results.     

Analysis of coupled conduction and radiation heat transfer in presence of participating medium- using a hybrid method

The current study addresses the mathematical modeling aspects of coupled conductive and radiative heat transfer in presence of absorbing, emitting and isotropic scattering gray medium within two-dimensional square enclosure. The walls of the enclosure are considered to be opaque, diffuse and gray. The enclosure comprised of isothermal vertical walls and insulated horizontal walls. A new hybrid method where the concepts of modified differential approximation employed by blending discrete ordinate method and spherical harmonics method, has been developed for modeling the radiative transport equation. The finite volume method has been adopted as the numerical technique. The effect of various influencing parameters i.e., radiation-conduction parameter, surface emissivity, single scattering albedo and optical thickness has been illustrated. The compatibility of the method with regard to solving coupled conduction and radiation has also been addressed.     

An alternative approach to determine the spot-size of a multi-mode laser beam and its application to diode laser beams

An alternative approach is suggested to determine the spot-size of a multi-mode laser beam. It has been shown by simulations that the suggested approach can give the beam quality factor and characteristic radius with less than 5% error. Unlike the power content method, the proposed method is applicable to the beams even with diameter one tenth of the CCD size. The new approach has been applied to a multi-mode diode laser output and it is shown that the ABCD matrix analysis can be used for beam propagation, with the measured parameters of the laser.