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Clifton P Calloway

Publications and source records attributed to Clifton P Calloway.

2 recordsLinked to original sources

Fraunhofer effect atomic absorption spectrometry.

The dark lines in the solar spectrum were discovered by Wollaston and cataloged by Fraunhofer in the early days of the 19th century. Some years later, Kirchhoff explained the appearance of the dark lines: the sun was acting as a continuum light source and metals in the ground state in its atmosphere were absorbing characteristic narrow regions of the spectrum. This discovery eventually spawned atomic absorption spectrometry, which became a routine technique for chemical analysis in the mid-20th century. Laboratory-based atomic absorption spectrometers differ from the original observation of the Fraunhofer lines because they have always employed a separate light source and atomizer. This article describes a novel atomic absorption device that employs a single source, the tungsten coil, as both the generator of continuum radiation and the atomizer of the analytes. A 25-microL aliquot of sample is placed on the tungsten filament removed from a commercially available 150-W light bulb. The solution is dried and ashed by applying low currents to the coil in a three-step procedure. Full power is then applied to the coil for a brief period. During this time, the coil produces white light, which may be absorbed by any metals present in the atomization cloud produced by the sample. A high-resolution spectrometer with a charge-coupled device detector monitors the emission spectrum of the coil, which includes the dark lines from the metals. Detection limits are reported for seven elements: 5 pg of Ca (422.7 nm); 2 ng of Co (352.7 nm); 200 pg of Cr (425.4 nm); 7 pg of Sr (460.7 nm); 100 pg of Yb (398.8 nm); 500 pg of Mn (403.1 nm); and 500 pg of K (404.4 nm). Simultaneous multielement analyses are possible within a 4-nm spectral window. The relative standard deviations for the seven metals are below 8% for all metals except for Ca (10.7%), which was present in the blank at measurable levels. Analysis of a standard reference material (drinking water) resulted in a mean percent recovery of 91%. This report attempts to give an historical perspective on the development of a novel atomic spectrometer based on the Fraunhofer effect.

Journal Article↗

Analytical characteristics of a continuum-source tungsten coil atomic absorption spectrometer.

A continuum-source tungsten coil electrothermal atomic absorption spectrometer has been assembled, evaluated, and employed in four different applications. The instrument consists of a xenon arc lamp light source, a tungsten coil atomizer, a Czerny-Turner high resolution monochromator, and a linear photodiode array detector. This instrument provides simultaneous multi-element analyses across a 4 nm spectral window with a resolution of 0.024 nm. Such a device might be useful in many different types of analyses. To demonstrate this broad appeal, four very different applications have been evaluated. First of all, the temperature of the gas phase was measured during the atomization cycle of the tungsten coil, using tin as a thermometric element. Secondly, a summation approach for two absorption lines for aluminum falling within the same spectral window (305.5-309.5 nm) was evaluated. This approach improves the sensitivity without requiring any additional preconcentration steps. The third application describes a background subtraction technique, as it is applied to the analysis of an oil emulsion sample. Finally, interference effects caused by Na on the atomization of Pb were studied. The simultaneous measurements of Pb and Na suggests that negative interference arises at least partially from competition between Pb and Na atoms for H2 in the gas phase.

Journal Article↗