Showing papers by "Purnendu K. Dasgupta published in 2000"

Luminescence detector with liquid-core waveguide

Abstract: A luminescence detector with a liquid-core waveguide. For detecting photoluminescence, the exciting radiation is provided transversely instead of axially, thus eliminating the need for monochromators and focusing optics. For detecting chemiluminescence, the chemiluminescent reagents are mixed in situ in the detector, thus eliminating time loss which results in loss of chemiluminescence. A further aspect of the invention is the electrogeneration of an unstable reagent for the production of chemiluminescence. The unstable reagent is generated in such a way that there is complete separation of anodic and cathodic products without the use of a physical barrier.

Measurement of Atmospheric Hydrogen Peroxide and Hydroxymethyl Hydroperoxide with a Diffusion Scrubber and Light Emitting Diode−Liquid Core Waveguide-Based Fluorometry

Abstract: We describe a new automated instrument for measuring gas- and aqueous-phase H2O2. The chemistry relies on the hematin-catalyzed oxidation of nonfluorescent thiamine to fluorescent thiochrome by H2O2; this reaction is 25-fold more selective for hydrogen peroxide than its nearest alkyl hydroperoxide congener, CH3HO2. The optical characteristics of the fluorescent product are such that it is ideally excited by newly available GaN-based light emitting diodes emitting in the near-UV. A stable long-life miniature flow-through fluorescence detector based on a transversely illuminated liquid core waveguide is thus used for this purpose. The limit of detection (LOD, S/N = 3) for liquid-phase H2O2 is 11 nM. A temperature-controlled high-efficiency Nafion membrane diffusion scrubber is used to collect gaseous hydrogen peroxide with near-quantitative efficiency with an S/N = 3 LOD of 13.5 pptv. The system responds to hydrogen peroxide and hydroxymethyl hydroperoxide but not to methyl hydroperoxide. The use of very in...

Gas sensor with phased heaters for increased sensitivity

Abstract: A concentrator and sensor assembly are disclosed that use phased heaters to multiply the concentration levels that can be eluted, relative to operation with a single interactive element having a sorbent material to increase the concentration of desired gas constituents at a detector. This is accomplished here by providing two or more interactive concentrator elements that are selectively heated in a time phased sequence so that each of the interactive elements becomes heated and desorbs gas constituents into the sample fluid stream at substantially the same time that an upstream concentration pulse, produced by heating one or more upstream interactive elements, reaches the interactive element. This produces a multiplication effect that significantly increases the concentration of the gas constituents at the detector, thereby increasing the effective sensitivity of the detector.

Continuous on-line true titrations by feedback-based flow ratiometry. The principle of compensating errors

Abstract: We introduce a new concept for continuous on-line titrations based on feedback-controlled flow ratiometry and the principle of compensating errors. The system has been thoroughly tested by applying it to acid−base neutralization titrations with indicator-based end point detection. In a typical case, the total flow (FT, consisting of the sample and the titrant flows) is held constant while the titrant (e.g., a standard base containing an indicator) flow FB varies linearly in response to a controller output voltage. The sample (e.g., an acidic solution to be titrated) flow FA constitutes the makeup and thus also varies (FA = FT − FB). The status of the indicator color in the mixed stream is monitored by an optical detector and used either for governing the controller output or for interpreting the results of the titration. Three methods (PID based control, fixed triangular wave control, and feedback-based triangular wave control implemented on a PC) were examined. In the last and the most successful approac...

A continuous film-recirculable drop gas-liquid equilibration device. Measurement of trace gaseous ammonia

Abstract: A miniature gas−liquid equilibrator or a gas collector, intended as a low-volume interface between a soluble gaseous sample and a liquid phase analyzer or between a liquid phase sample and a detector designed for use with gas samples, is described. This paper addresses the application of the device for the measurement of trace atmospheric ammonia. Gas collection occurs solely by diffusive sampling such that aerosol particles are not collected. The device essentially consists of a tube surrounded externally by a jacket. Gas flows through the jacket and contacts a liquid film flowing on the surface of the tube. The flowing film forms a drop at the tube terminus and is aspirated off through the inner bore of the tube. The collected analyte can be (a) directly sent to an analysis system or (b) preconcentrated on a suitable stationary phase; the preconcentrator effluent can be recycled, if desired. With a fluorometric flow injection analysis system harnessed to measure ammonia with such a collector, the limit ...

Ion chromatographic determination of acidity.

Abstract: The practice of determining acid concentrations by titrations has remained unchanged for more than a century. We introduce a new approach to the determination of acid concentrations based on cation exchange chromatography. We demonstrate the ability of sulfonated styrene-divinylbenzene based stationary phases to separate the hydrogen ion from other monovalent cations. The eluent is a dilute solution of a neutral salt, sometimes containing a small concentration of the corresponding acid, e.g., sodium ethanesulfonate, pH adjusted with ethanesulfonic acid. The high equivalent conductance (approximately 350 S.cm2/equiv) of H+ and relatively low eluent concentration allows sensitive conductometric detection of H+, down to the 50 microM level under favorable conditions. The conductometric response to H+ can be linear over a wide range of H+ concentrations, from sub-millimolar to several molar concentrations. The system allows the rapid quantitation of strong acids; weak acids can also be determined depending on pKa and injected concentration. The determinations of several strong and weak acids are presented along with factors that govern their chromatographic analysis.

Determination of oxidative stability of lipids in solid samples

Abstract: A gas-phase flow injection analysis (FIA) method for the direct determination of the oxidative stability of solid fat/oil samples is described. Samples are confined with a low level of oxygen in a reactor of adjustable temperature. The oxygen consumption by the sample is automatically monitored after a preset period. The temperature-dependent data exhibit Arrhenius behavior. Normally, it is difficult to directly determine the stability at ambient temperatures because of inordinately long time requirements. The close correspondence to Arrhenius behavior makes it possible to use the results obtained at higher temperature to calculate the stability of samples at lower temperature conditions, such as at ambient storage temperature. The effects of sample size, sample particle size, sample fat content and the reproducibility of the method over time were studied using synthetic and bone meal samples. The oxygen consumption was found to be linearly dependent on the amount of sample taken, inversely dependent on the particle diameter, and independent of the exact lipid content, given some minimum lipid content. The results exhibited high day-to-day reproducibility. The gasphase FIA system developed in this work is easy to operate. Compared with the currently used method, the sample throughput rate is much faster (2–3h for complete multitemperature characterization of a sample) and the sample requirement is much lower (∼1 g). Furthermore, it eliminates the need to extract and recover the fat from the sample for further processing as is required by the other methods commonly used to measure oxidative stability.

A simple instrument for ultraviolet-visible absorption spectrophotometry in high temperature molten salt media

Abstract: An inexpensive (

Methods and apparatus for estimating the oxidative stability of an oxidizable material

Abstract: The method comprises determining the oxygen consumption by a sample of the material at a first temperature, determining the oxygen consumption by a sample of the material at a second temperature, and estimating the oxidative stability of the material at a third temperature by extrapolating the temperature-dependent data obtained at the first temperature and the second temperature to the third temperature.