This paper describes a procedure for the determination of antimony (III) by differential pulse anodic stripping voltammetry using a mercury film screen-printed electrode as the working electrode. The procedure has been optimized using experimental design methodology. Under these conditions, in terms of Residual Standard Deviation (RSD), the repeatability (3.81 %) and the reproducibility (5.07 %) of the constructed electrodes were both analyzed. The detection limit for Sb (III) was calculated at a value of 1.27×10−8 M. The linear range obtained was between 0.99 × 10−8 − 8.26 × 10−8 M. An analysis of possible effects due to the presence of foreign ions in the solution was performed and the procedure was successfully applied to the determination of antimony levels in pharmaceutical preparations and sea water samples.
A high-throughput Raman chemical imaging method was developed for direct inspection of benzoyl peroxide (BPO) mixed in wheat flour. A 5 W, 785 nm line laser (240 mm long and 1 mm wide) was used as a Raman excitation source in a push-broom Raman imaging system. Hyperspectral Raman images were collected in a wavenumber range of 103-2881 cm from dry wheat flour mixed with BPO at eight concentrations (w/w) from 50 to 6400 ppm. A sample holder with a sampling volume of 150 × 100 × 2 mm was used to present a thin layer (2 mm thick) of the powdered sample for line-scan image acquisition with a spatial resolution of 0.2 mm. A baseline correction method based on adaptive iteratively reweighted penalized least squares was used to remove the fluctuating fluorescence signals from the wheat flour. To isolate BPO particles from the flour background, a simple thresholding method was applied to the single-band fluorescence-free images at a unique Raman peak wavenumber (i.e., 1001 cm) preselected for the BPO detection. Chemical images were created to detect and map the BPO particles. Limit of detection for the BPO was estimated in the order of 50 ppm, which is on the same level with regulatory standards. Pixel concentrations were calculated from the percentages of the BPO pixels in the chemical images. High correlation was found between the pixel concentrations and the mass concentrations of the BPO, indicating that the Raman chemical imaging method can be used for quantitative detection of the BPO mixed in the wheat flour.
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