Reliability of background current subtraction in anodic stripping voltammetry at mercury film electrodes

The effectiveness and accuracy of the correction for background current in subtractive anodic stripping voltammetry at rotating mercury film electrodes are discussed. The effects of different experimental parameters on the subtracted baseline are examined. Long deposition periods, at extreme potentials, result in large errors in the background correction. The incomplete background correction is attributed mainly to changes in the morphology of the working electrode. Different approaches for obtaining the subtractive stripping response are compared. Errors are reduced when subtractive differential pulse stripping is used at different convection rates, resulting in a detection limit of 2 × 10^-9 M cadmium with 1-min deposition. Cadmium, lead, and zinc ions at nano molar concentrations were used as test ions.     

Raman scattering from crystalline and amorphous (GaSb)1-xGex semiconducting films

The first reported Raman scattering experiments have been performed on single crystal and amorphous films of the metastable alloy (GaSb)_1-xGe_x with compositions across the pseudobinary phase diagram. In crystalline films, the optical phonons exhibit a “one-two” type mode behavior. Broadening and softening of the Raman peaks with increasing alloy concentrations are attributed to a relaxation of q-vector selection rules due to substitutional disorder on both the cation and anion sublattices. Additionally, disorder induced scattering from the zone-edge acoustic phonons was observed. In amorphous alloy films, the reduced Raman spectra were compared to the one-phonon densities of states of the end-member crystals. The resulting apparent lack of polarization dependence indicated that the amorphous films were of the random network type.     

A comparison of 2-D chromatography separations using UV and (18)O quantification of proteins in similar proteomes

Proteins present in two mitochondria preparations were separated by 2-D chromatography using the ProteomeLab PF-2D Protein Fractional System, protein fractionation in two dimensions (PF-2D). The proteins in each first-dimension fraction were determined by trypsinization and LC-MS/MS. Chromatography peaks were quantified by UV detection using the "Mapping Tools" software (Beckman). The proteins present in UV detected peaks were trypsinized and identified by automated MS/MS sequencing. Relative amounts of the proteins present in the equivalent peak for each sample were assessed by comparison of the intensities of the constituent peptides and a predicted PF-2D value was calculated from the total ion count (TIC) for each peptide. Relative quantification for (18)O labeled peptides was performed using the ZoomQuant (v1.43b) software [1, 2]. We found that the chromatography peaks detected by UV generally contained several proteins. Using (18)O labeling we determined that in each peak the ratios of the constituent proteins were different. When these ratios were normalized using the TIC to account for abundance, the resulting ratio corresponded to that determined by UV. The predicted value for the PF-2D score corresponded to the observed value for each peak irrespective of the number or proteins detected.     

Lactic acid demineralization of green crab (Carcinus maenas) shells: effect of reaction conditions and isolation of an unusual calcium complex

Chitin and chitosan are potentially useful and environmentally friendly biopolymers with a wide range of value-added applications. Effective and green technologies for isolation of these materials are potentially important. Here, we report the use of lactic acid for the demineralization of green crab shells. Green crab shells and lactic acid, produced during cheese making, are two waste streams that could be tapped for large-scale chitin and chitosan processing. We have studied the effect of concentration and temperature on the demineralization of green crab shells. An unusual calcium lactate/lactic acid complex was also isolated and crystallographically characterized. The results have implications not only for the use of weak acids in the isolation of chitin and chitosan but also for the use of lactic acid as a solvent in green chemistry.