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QUANTIFICATION OF IRON IN SEAWATER AT THE LOW PICOMOLAR RANGE BASED ON THE OPTIMIZATION OF THE BROMATE-AMMONIA-DIHYDROXYNAPHTALENE SYSTEM BY CATALYTIC ADSORPTIVE CATHODIC STRIPPING VOLTAMMETRY.
MedLine Citation:
PMID:  23339679     Owner:  NLM     Status:  Publisher    
Abstract/OtherAbstract:
A new analytical protocol for the challenging analysis of total dissolved iron at the low picomolar level in oceanic waters suitable for onboard analysis is presented. The method is based on the revision of the adsorptive properties of the iron-2,3-dihydroxynaphthalene (DHN) complexes on the Hanging Mercury Drop Electrode with catalytic enhancement by bromate ions. Although based on a previously proposed reagent combination, we show here that the addition of an acidification/alkalinisation step is essential in order to cancel any organic complexation and that an extra increment of the pH to 8.6-8.8 leads to the definition of a preconcentration free procedure with the lowest detection limit described up to now. For total dissolved iron analysis, samples were acidified to pH 2.0 in the presence of 30 M DHN and left to equilibrate overnight. A 10 mL sample was subsequently buffered to pH~8.7 in the presence of 20 mM bromate: a 60 seconds deposition at 0V led to a sensitivity of 34 nAnM-1min-1, a 4 fold improvement over previous methods, that translated in a limit of detection of 5 pM (2-20 fold improvement). Several tests proved that a non reversible reaction in the time scale of the analysis, triggered by the acidification/alkalinisation step, was behind the signal magnification. The new method was validated onboard via the analysis of reference material and via intercalibration against FIA-chemiluminescence on Southern Ocean surface samples.
Authors:
Luis Miguel Laglera; Juan Santos-Echeandia; Salvatore Caprara; Damiano Monticelli
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Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2013-1-23
Journal Detail:
Title:  Analytical chemistry     Volume:  -     ISSN:  1520-6882     ISO Abbreviation:  Anal. Chem.     Publication Date:  2013 Jan 
Date Detail:
Created Date:  2013-1-23     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  0370536     Medline TA:  Anal Chem     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
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