We examine the application of an oscillating cell in combination with right-angle Raman scattered light collection geometry for quantitative Surface Enhanced (Resonance) Raman Scattering (SER(R)S) measurements from nano-colloidal noble metal solutions. This excitation/collection Raman configuration allows specific SERS and SERRS signatures of aqueous solutions of mitoxantrone, an antitumor drug, to be easily resolved at (sub)-ng/mL and (sub)-pg/mL concentration levels. A partial least-squares (PLS) chemometric algorithm was applied to predict the concentration of 25 microL of aqueous solutions of mitoxantrone added in 0.5 mL of a silver colloidal solution in a test tube attached to the oscillating cell. For SERS (514.5 nm) measurements, this was performed over the range from 0 to 13 ng/mL with a correlation coefficient R(2) of 98.5% and RMS error of prediction equal to 0.5 ng/mL. SERRS (632.8 nm) measurements performed over a range of 0 to 7 pg/mL gave R(2) = 98.92% and RMSE = 0.2 pg/mL.
Quantitative analysis of methylene blue (MB) has been performed with Surface Enhanced Raman Scattering, SERS, using citrate reduced silver colloid activated with NaCl. In this study, the combination of SERS occurring at the proximity of the plasmon surface and of resonance Raman with excitation wavelength matched to the maximum absorbance of the molecule being analyzed, was successfully applied to maximize the Raman scattering intensity. The surface‐enhanced resonance Raman scattering (SERRS) spectra of aqueous solutions of the dye at various concentrations were collected in right‐angle scattering geometry configuration which results favorable when nanocolloidal dispersions are used. The MB concentration was correlated with the intensity of the peak centered at 1,625 cm−1 in the SERRS spectrum and this correlation resulted in an extremely sensitive quantitative investigation of the MB with limit of detection in pM level. Among others, this method can be easily applied for the examination of both the selectivity of waste water purification membranes for relevant small molecular weight contaminants or/and the solar photocatalytic effectiveness of such membranes for the degradation of pertinent pollutants by their quantitative assessment in the permeate at very low concentration range.
The goal of this work is to model the nature of the chemical species [CdCl2(extractant)2] that are formed during the solvent (or liquid-liquid) extraction of the toxic cadmium(II) from chloride-containing aqueous media using hydrophobic 2-pyridyl ketoximes as extractants. Our coordination chemistry approach involves the study of the reactions between cadmium(II) chloride dihydrate and phenyl 2-pyridyl ketoxime (phpaoH) in water-containing acetone. The reactions have provided access to complexes [CdCl2(phpaoH)2]∙H2O (1∙H2O) and {[CdCl2(phpaoH)]}n (2); the solid-state structures of which have been determined by single-crystal X-ray crystallography. In both complexes, phpaoH behaves as an N,N’-bidentate chelating ligand. The complexes have been characterized by solid-state IR and Raman spectra, and by solution 1H NMR spectra. The preparation and characterization of 1∙H2O provide strong evidence for the existence of the species [CdCl2(extractant)2] that have been proposed to be formed during the liquid-liquid extraction process of Cd(II), allowing the efficient transfer of the toxic metal ion from the aqueous phase into the organic phase.
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