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Earth and Environmental Science Department, University of Texas at San Antonio, USA
E-mail: konstantinos.makris@utsa.edu
; Fax: +1-210-458-4469
; Tel: +1-210-458-5745
Analyst, 2008,133, 191-196
DOI:
10.1039/B714389C
Received
18 Sep 2007,
Accepted
26 Nov 2007
First published online
20 Dec 2007
A sensitive (method detection limit, 2.0 µg As L−1) colorimetric determination of trace As(V) and As(III) concentrations in the presence of soluble phosphorus (P) concentrations in soil/water extracts is presented. The proposed method modifies the malachite green method (MG) originally developed for P in soil and water. Our method relies upon the finding that As(III) and As(V) do not develop the green color during P analysis using the MG method. When an optimum concentration of ascorbic acid (AA) is added to a sample containing up to 15 times P > As (µM) concentrations, the final sample absorbance due to P will be equal to that of As(V) molecules. The soluble As concentration can then be quantified by the concentration difference between the mixed oxyanion (As + P) absorbance (proposed method) and the MG method absorbance that measures only P. Our method is miniaturized using a 96-well microplate UV-VIS reader that utilizes minute reagent and sample volumes (120 and 200 µL sample−1, respectively), thus, minimizing waste and offering flexibility in the field. Our method was tested in a suite of As-contaminated soils that successfully measured both As and P in soil water extracts and total digests. Mean% As recoveries ranged between 84 and 117%, corroborating data obtained with high-resolution inductively-coupled plasma mass-spectrometry. The performance of the proposed colorimetric As method was unaffected by the presence of Cu, Zn, Pb, Ni, Fe, Al, Si, and Cr in both neutral and highly-acidic (ca. pH 2) soil extracts. Data from this study provide the proof of concept towards creating a field-deployable, portable As kit.
A sensitive (method detection limit, 2.0 µg As L–1) colorimetric determination of trace As(V) and As(III) concentrations in the presence of soluble phosphorus (P) concentrations in soil/water extracts is presented. The proposed method modifies the malachite green method (MG) originally developed for P in soil and water. Our method relies upon the finding that As(III) and As(V) do not develop the green color during P analysis using the MG method. When an optimum concentration of ascorbic acid (AA) is added to a sample containing up to 15 times P > As (µM) concentrations, the final sample absorbance due to P will be equal to that of As(V) molecules. The soluble As concentration can then be quantified by the concentration difference between the mixed oxyanion (As + P) absorbance (proposed method) and the MG method absorbance that measures only P. Our method is miniaturized using a 96-well microplate UV-VIS reader that utilizes minute reagent and sample volumes (120 and 200 µL sample–1, respectively), thus, minimizing waste and offering flexibility in the field. Our method was tested in a suite of As-contaminated soils that successfully measured both As and P in soil water extracts and total digests. Mean% As recoveries ranged between 84 and 117%, corroborating data obtained with high-resolution inductively-coupled plasma mass-spectrometry. The performance of the proposed colorimetric As method was unaffected by the presence of Cu, Zn, Pb, Ni, Fe, Al, Si, and Cr in both neutral and highly-acidic (ca. pH 2) soil extracts. Data from this study provide the proof of concept towards creating a field-deployable, portable As kit.
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