Contact Info
Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf
IEC
Citations 3
"Sensitivity Enhancement In The Determination Of Silicate By Ion-exclusion Chromatography Using Luminol Chemiluminescence Detection"
Anal. Chim. Acta
1995 Volume 302, Issue 2-3 Pages 173-177
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Abstract:
An increased chemiluminescence (CL) emission, produced upon mixing an acidified silicate solution with an alkaline luminol solution even in the absence of hydrogen peroxide, provided an effective post-column detection system to enhance sensitivity in the selective determination of silicate by ion-exclusion chromatography. The detection limit of 0.1 ng mL-1 silicon(IV) obtained under the optimum conditions was much lower than that obtained by using the CL reaction in the presence of hydrogen peroxide. The working range was linear from 1.0 ng mL-1 to 10 µg mL-1. Using the experimental conditions optimized for silicate, a comparative study of the CL behavior of other anions such as carbonate, phosphate, sulfate and sulfide ions showed that the CL intensity with the silicate ion was the greatest among these anions.
Silicate
Post-column derivatization
"Determination Of Boron By Ion-exclusion Chromatography With Post-column Derivatization"
Bunseki Kagaku
1994 Volume 43, Issue 5 Pages 365-370
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Abstract:
Borate was separated on an Excelpak ICS-R3G/ICS-R35 column (5 cm/15 cm x 7.8 mm; H+ form; 3.5 milliequivalents per g dry wt.) with 1 mM H2SO4 as mobile phase (1 ml/min) and detection at 420 nm after post-column reaction in a coil (5 m x 0.5 mm i.d.) at 40°C with a stream (0.8 ml/min) of 0.5% azomethine H/1% ascorbic acid/1% diammonium EDTA solution in 1.5 M ammonium acetate. The calibration graph was linear for 0.01-10 mg/l of B (injection volume 0.05 ml) and the detection limit was 0.008 mg/l. The RSD (n = 10) at 0.02 mg/l of B was 5.5%. Results correlated well with those by ICP-MS.
Boron
Method comparison
Post-column derivatization
"Cytosolic Metal Speciation Studies By Sequential, Online, SE-IE/HPLC-ICP-MS"
Mar. Environ. Res.
1998 Volume 46, Issue 1-5 Pages 573-577
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Abstract:
A procedure involving directly coupled HPLC-ICP-MS is described for the quantification of metals associated with cytosolic proteins. Selectivity is achieved by sequential fractionation by size exclusion (TSK SW2000) followed by ion exchange chromatography (Showdex DEAE). Spectra on up to 11 masses for six elements were acquired simultaneously by scanning the quadrapole in the peak hopping mode. A flow injection loop inserted downstream of the columns was used to monitor analyte recovery and quantify the ion intensity profiles from the MS. Reproducibility of analysis was approximately 2-5% and absolute detection limits were typically between 10 and 60 pg of analyte. The utility of the technique for: (i) detecting abnormal distributions in cytosolic metals due to metal exposure; and (ii) determining the biological turnover of Cu and other metals associated with proteins is demonstrated using the marine shellfish Littorina littorea exposed to elevated concentrations of Cd and 65Cu.
Metals
Marine
Speciation