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1.
Talanta ; 82(2): 675-80, 2010 Jul 15.
Article in English | MEDLINE | ID: mdl-20602953

ABSTRACT

A bismuth bulk electrode (BiBE) has been investigated as an alternative electrode for the anodic stripping voltammetric (ASV) analysis of Pb(II), Cd(II), and Zn(II). The BiBE, which is fabricated in-house, shows results comparable to those of similar analyses at other Bi-based electrodes. Metal accumulation is achieved by holding the electrode potential at -1.4V (vs. Ag/AgCl) for 180 s followed by a square wave voltammetric stripping scan from -1.4 to -0.35 V. Calibration plots are obtained for all three metals, individually and simultaneously, in the 10-100 microg L(-1) range, with a detection limit of 93, 54, and 396 ng L(-1) for Pb(II), Cd(II), Zn(II), respectively. A slight reduction in slope is observed for Cd(II) and Pb(II) when the three metals are calibrated simultaneously vs. individually. Comparing the sensitivities of the metals when calibrated individually vs. in a mixture reveals that Zn(II) is not affected by stripping in a mixture. However, Pb(II) and Cd(II) have decreasing sensitivities in a mixture. The optimized method has been successfully used to test contaminated river water by standard addition. The results demonstrate the ability of the BiBE as an alternative electrode material in heavy metal analysis.


Subject(s)
Bismuth/chemistry , Cadmium/analysis , Lead/analysis , Zinc/analysis , Electrochemistry/methods , Electrodes , Limit of Detection , Potentiometry , Spectrophotometry/methods
2.
Anal Chem ; 82(2): 593-600, 2010 Jan 15.
Article in English | MEDLINE | ID: mdl-20038093

ABSTRACT

Optical fluorescence sol-gel sensors have been developed for the detection of carbon dioxide gas in the 0.03-30% range with a detection limit of 0.008% (or 80 ppm) and a quantitation limit of 0.02% (or 200 ppm) CO(2). Sol-gels were spin-coated on glass slides to create an organically modified silica-doped matrix with the 1-hydroxypyrene-3,6,8-trisulfonate (HPTS) fluorescent indicator. The luminescence intensity of the HPTS indicator (513 nm) is quenched by CO(2), which protonates the anionic form of HPTS. An ion pair technique was used to incorporate the lipophilic dye into the hydrophilic sol-gel matrix. TiO(2) particles (<5 microm diameter) were added to induce Mie scattering and increase the incident light interaction with the sensing film, thus increasing the signal-to-noise ratio. Moisture-proof overcoatings have been used to maintain a constant level of water inside the sensor films. The optical sensors are inexpensive to prepare and can be easily coupled to fiber optics for remote sensing capabilities. A fiber-optic bundle was used for the gas detection and shown to work as part of a multianalyte platform for simultaneous detection of multiple analytes. The studies reported here resulted in the development of sol-gel optical fluorescent sensors for CO(2) gas with sensitivity below that in the atmosphere (ca. 387 ppm). These sensors are a complementary approach to current FT-IR measurements for real-time carbon dioxide detection in environmental applications.

3.
Anal Chem ; 78(21): 7582-7, 2006 Nov 01.
Article in English | MEDLINE | ID: mdl-17073430

ABSTRACT

A new method for pretreating blood samples for trace Cr analysis is described. The advanced oxidation process (AOP with H2O2 and 5.5-W UV irradiation for 60 min) is used to remove biological/organic species for subsequent analysis. Prior to the AOP pretreatment, acid (HNO3) is used at pH 3.0 to inhibit the enzyme catalase in the blood samples. Catalytic adsorptive stripping voltammetry at a bismuth film electrode gives a Cr concentration of 6.0 +/- 0.3 ppb in the blood samples. This concentration was confirmed by dry-ashing the blood samples and subsequent analysis by atomic absorption spectroscopy. This current method may be used to monitor chromium, a trace metal in humans, and the efficacy and safety of chromium supplements as adjuvant therapy for diabetes.


Subject(s)
Chromium/blood , Electrochemistry/methods , Adsorption , Calibration , Catalysis , Hydrogen Peroxide , Oxidation-Reduction
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