University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Website: @unf

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Classification: Marine -> shellfish -> shrimp

Citations 4

"On-line Preconcentration System For Lead Determination In Seafood Samples By Flame Atomic Absorption Spectrometry Using Polyurethane Foam Loaded With 2-(2-benzothiazolylazo)-2-p-cresol"
Anal. Chim. Acta 2001 Volume 441, Issue 2 Pages 281-289
Valfredo A. Lemos and Sérgio L. C. Ferreira

Abstract: In the present paper, an on-line system for enrichment and determination of lead is proposed. It is based on the chemical sorption of lead(II) ions on a minicolumn packed with polyurethane foam loaded with 2-(2-benzothiazolylazo)-2-p-cresol (BTAC) reagent. After pre-concentration, lead(II) ions are eluted by 0.10 mol L-1 hydrochloric acid solution and determined directly by flame atomic absorption spectrometry (FAAS). Chemical and flow variables as well as effect of other ions were studied. The results demonstrated that lead could be determinate with an enrichment factor of 26 for a sample volume of 7.0 mL and pre-concentration time of 1 min. The detection limit (3 s) was 1.0 µg L-1 and the precision (assessed as the relative standard deviation) reached values of 6.0-0.7% in lead solutions of 10^-500 µg L-1 concentration, respectively. The enrichment factor and the detection limit can be further improved by increasing pre-concentration time without degradation in the efficiency due to the favorable kinetics and low hydrodynamic impedance of the present system. Achieved sampling frequency was 48 samples per hour. The effect of another ions in concentrations agreeing with biological samples was studied. It was found that the proposed procedure has necessary selectivity for lead determination in seafood and other biological samples. The accuracy was confirmed by analysis of the followings certified reference materials: fish tissue IAEA, lobster hepatopancreas NRCC TORT-1 and citrus leaves NIST 1572. Recoveries of spike additions (0.2 or 1.0 µg g-1) to several seafood samples were quantitative (90-107%). These results proved also that the procedure is not affected by matrix interferences and can be applied satisfactorily for lead determination in samples of shrimp, oyster, crab, fish and mussel contaminated by it.
Lead Spectrophotometry Preconcentration Interferences Amberlite Polyurethane foam Solid phase extraction

"Determination Of Sulfite In Food By Flow Injection Analysis"
J. AOAC Int. 1986 Volume 69, Issue 3 Pages 542-546
Sullivan JJ, Hollingworth TA, Wekell MM, Newton RT, Larose JE

Abstract: A method is described for the determination of sulfite levels in food products by flow injection analysis (FIA). The method is based on the decolorization of malachite green by SO2, which is isolated from the flowing sample stream by means of a gas diffusion cell. The FIA method has a detection limit in food sample extracts of 0.1 ppm SO2 (3 times peak height of blank), which corresponds to 1-10 ppm SO2 in a food product, depending on the extraction procedure used. At the 5 ppm SO2 level in a food extract, the precision of replicate injections is±1-2%. The method was tested on a variety of both sulfite-treated and untreated food products and the results compared favorably with those obtained by the Monier-Williams, colorimetric (pararosaniline), and enzymatic (sulfite oxidase) methods. The average differences from the FIA results were 19, 11, and 12%, respectively, for those samples (n = 12) above 50 ppm SO2. At lower levels the results were somewhat more erratic due to inaccuracies of the various methods at low concentrations. The method is based on the decolorization of malachite green (C. I. Basic Green 4) by SO2, which is isolated from the flowing sample stream by a gas diffusion cell; the decrease in absorbance is measured at 615 nm. The detection limit is 0.1 ppm, which corresponds to 1 to 10 ppm in a food product, depending on the extraction procedure used, which itself depends on the type of food being analyzed. For 5 ppm of SO2 in a food extract, the precision of replicate injections is ~1 to 2%. The proposed method was tested on sulfite-treated and untreated wine, apple juice, dried apricots, potatoes, pickled onions, shrimps, lettuce, dried apples and cabbage to give results in good agreement with those obtained by the Monier-Williams, pararosaniline colorimetric and sulfite oxidase methods. The mean differences from the proposed method were 19, 11 and 12%, respectively for the 12 samples with SO2 contents >50 ppm. At lower levels the results were somewhat more erratic. The construction of the flow injection apparatus is described in detail.
Sulfite Spectrophotometry Sample preparation Gas diffusion Extraction Method comparison

"Determination Of Total Sulfite In Shrimp, Potatoes, Dried Pineapple, And White Wine By Flow Injection Analysis: Collaborative Study"
J. AOAC Int. 1990 Volume 73, Issue 1 Pages 35-42
Sullivan JJ, Hollingworth TA, Wekell MM, Meo VA, Saba HH, Etemad-Moghadam A, Eklund C, Phillips JG, Gump BH

Abstract: A method for the determination of total sulfite in shrimp, potatoes, dried pineapple, and white wine by flow injection analysis (FIA) was collaboratively studied by 8 laboratories. In the method, the sample solution is reacted with sodium hydroxide to liberate aldehyde-bound sulfite. The sample stream is acidified to produce SO2 gas, which diffuses across a Teflon membrane in the gas diffusion cell into a flowing stream of malachite green. The degree of discoloration of the malachite green is proportional to the amount of sulfite in the sample solution. Red wine was included in the study but interlaboratory precision for these samples was not satisfactory and correlation with Monier-Williams results was poor. The present method is not recommended for use with these samples. For shrimp, potatoes, dried pineapple, and white wine, average reproducibility (RSDR) of results was 25% for samples at 10 ppm SO2 and 10% for samples at greater than 50 ppm. Overall average reproducibility was 14%. Recoveries of sulfite added to samples averaged 80%. Comparison of FIA with the Monier-Williams method indicated comparable results by the 2 methods. The FIA method has been adopted official first action for determination of greater than or equal to 5 ppm total sulfite in shrimp, potatoes, dried pineapple, and white wine.
Sulfite Spectrophotometry Diffusion Teflon membrane Method comparison Gas diffusion

"FAAS Determination Of Calcium And Magnesium In Gelatin Using The FIA Online Automatic Dilution Technique"
Lihua Jianyan, Huaxue Fence 1996 Volume 32, Issue 2 Pages 82-91
Zhang Min, Chen Shuyu, Lin Shuqin and Cheng Lin

Abstract: Sample (1.2 g) was soaked in 15 mL water for 15 min and digested with 1 mL concentrated HCl, 1 mL concentrated HNO3 and 4 mL H2O2. The digest was diluted with to 25 mL with water for FIA with flame AAS detection of Ca and Mg. Test solution was injected and carried to two sampling loops with a stream of water for alternating feeding, primary and secondary injection volumes being 21 and 70 µL, respectively. The solution was allowed to mix with a stream of 0.3% La solution prior to splitting into two streams by passing through two dilution tubes of 50 and 150 cm in length, respectively, with dilution of 87 to 233-fold, and detection. The peak B of the sets of signals was employed for measurement of Ca whereas the trough E for Mg. Determination was at µg/g level. RSD were 1.3-2.1%. The method was applied to the analysis of wheat, shrimp, pig liver and shrub leaves. Interference from phosphate was overcome. Sampling frequency was 96 runs/h.
Calcium Magnesium Sample preparation Spectrophotometry Interferences Dual injector Sample splitting