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Steven A Steiner

Publications and source records attributed to Steven A Steiner.

5 recordsLinked to original sources

Ultrafast concentration and speciation of chromium(III) and (VI).

There is an increasing need to know the concentrations of chromium(III) and (VI) separately rather than only the total chromium content. A method is described for accomplishing this very quickly using only low-cost, portable equipment. Two small, resin-loaded extraction disks are placed one on top of the other in a plastic holder. Then a syringe containing the aqueous sample is attached to the holder and the sample is pushed through the disks. In a matter of seconds, all of the chromium(VI) is retained on the top anion-exchange disk and chromium(III) is extracted by the second cation-exchange disk. The concentrations on each disk are several hundredfold higher than they were in the original sample. The amounts of chromium(III) and (VI) extracted are measured directly on the surface of the respective disks by diffuse reflectance spectroscopy (DRS). Despite the low molar absorptivity of chromium(III) in aqueous solution, the concentration on the upper most layer on the extraction disk is high enough to permit the determination of chromium(III) in samples at the low mg/L range. Chromium(VI) can also be determined at low to sub-mg/L concentrations. A study of the cation-exchange disks was undertaken to compare the performance characteristics of disks containing sulfonated resins and those with iminodiacetate functionality. In addition, data are presented to show the effects of heating the iminodiacetate disks after the initial extraction. The disks were heated in hot water for 15-30 min to complete the slow complexation reaction on the surface.

Anion Exchange Resins↗

Metathesis polymerization-derived monolithic membranes for solid-phase extraction coupled with diffuse reflectance spectroscopy.

Novel monolithic disks were prepared via ring opening metathesis polymerization (ROMP) from norborn-2-ene (NBE), a crosslinker, i.e., 1,4,5,8,8a-hexahydro-1,4,4,5,8, exo, endo-dimethanonaphthalene (DMN-H6) and tris(norborn-5-ene-2-ylmethylenoxy)methylsilane, respectively, 2-propanol and toluene (25:25:41:9, all %, w/w) using RuCl2(PCy3)2(CHPh) (Cy=cyclohexyl) as initiator and triphenylphosphine (PPh3) as modulator. Disks 1-2 mm thick were prepared by polymerization in a mold, disks thinner than 1mm were prepared by impregnation of nylon or other porous filters prior to the polymerization step. These disks were evaluated for the preconcentration of iodine and selected organic solutes from dilute aqueous samples by solid-phase extraction (SPE). Quantitative measurement of the extracted solutes was achieved by diffuse-reflectance spectroscopy (DRS) directly on the surface of the disk.

Bridged Bicyclo Compounds↗

Ion association with alkylammonium cations for separation of anions by capillary electrophoresis.

A background electrolyte (BGE) containing a 100 mM concentration of an alkylammonium cation with ethyl, propyl or butyl groups provides an excellent medium for separation of anions by capillary electrophoresis (CE). Two major effects were noted. Use of one of a series of alkylammonium cations in the BGE at a selected pH provides a simple and effective way to vary and control electroosmotic flow (EOF) over a broad range. It is believed that the alkylammonium cations are coated onto the capillary surface through a reversible dynamic equilibrium. Secondly, alkylammonium cations modify the electrophoretic migration of sample anions and the electroosmotic migration of neutral organic analytes by association interaction. This selective interaction results in improved anion separations and permits the simultaneous separation of neutral analytes. The degree of association interaction varies with the bulk and hydrophobicity of the alkylammonium cations. Incorporation of an aliphatic amine salt of moderate molecular weight in the running electrolyte provides a valuable new way to vary the migration times of sample anions and to optimize their resolution. The interactions between alkylammonium cations and sample anions or neutral organics appear to take place entirely within the liquid phase and do not require a polymeric or micellar pseudo phase.

Anions↗

Capillary electrophoresis of organic cations at high salt concentrations.

At concentrations of 100 mM or higher the chemical nature of both the cation and anion in the background electrolyte (BGE) can be varied to manipulate the migration times of protonated aniline cations. Significant differences were noted with Li+, Na+ and K+ for capillary electrophoretic runs carried out at pH 3. However, much greater differences in migration times were observed at acidic pH values when the BGE contained protonated cations of aliphatic amines. Analyte migration became progressively slower in the series: methylamine, diethylamine, diethylamino ethanol and triethylamine. A major part of this effect was attributed to an opposing electroosmotic flow (EOF) resulting from a positively-charged coating of the capillary surface with the amine cations in the BGE via a dynamic equilibrium. The amine cations also interact in solution with the analyte ions to reduce their electrophoretic mobilities. Migration times of anilines could be varied systematically over a broad range according to the BGE amine cation selected. Excellent separations of seven closely-related anilines were obtained with the new system.

Cations↗

Rapid determination of ions by combined solid-phase extraction--diffuse reflectance spectroscopy.

We introduce colorimetric solid-phase extraction (C-SPE) for the rapid determination of selected ions. This new technique links the exhaustive concentration of an analyte by SPE onto a membrane disk surface for quantitative measurement with a hand-held diffuse reflectance spectrometer. The concentration/measurement procedure is complete in approximately 1 min and can be performed almost anywhere. This method has been used to monitor iodine and iodide in spacecraft water in the 0.1-5.0 ppm range and silver(I) in the range of 5.0-1000 microg/l. Applications to the trace analysis of copper(II), nickel(II), iron(III) and chromium(VI) are described. Studies on the mechanism of extraction showed that impregnation of the disk with a surfactant as well as a complexing reagent results in uptake of additional water, which markedly improves the extraction efficiency.

Cations↗