Two acid digestion procedures (microwave-assisted and room temperature) were developed for the quantitative analysis of ferromanganese nodules by inductively coupled plasma double focusing sector field mass spectrometry (ICP-SFMS). Different compositions of the acid mixture, dilution factors and corrections for spectral interferences were tested. A combination of nitric, hydrochloric and hydrofluoric acids is necessary for complete sample digestion, with lowest acid to sample ratios (v/m) of 15 and 1.5. respectively, for the last two acids. Sample dilution factors higher than 2 X 104 should be used in order to decrease matrix effects and provide robust long-term instrumental operation. In spite of high dilution. method detection limits in the sub-mug g(-1) range were obtained for 54 out of 71 elements tested. due to the high detection capability of ICP-SFMS, as well as the special care taken to ensure the purity of reagents, to clean the instrument sample introduction system and to minimise sample handling. Owing to the presence of unresolved (at the resolution available) spectral interferences, accurate determination of Au, Hg, Os, Pd, Re and Rh is impossible without matrix separation. The accuracy of the entire analytical method was tested by the analysis of two nodule reference materials. The results generated agreed to within +/-2% for about 10, within +/-10% for more than 40 and within +/-20% for about 50 of 53 elements for which certified, recommended or literature values are available. A precision better than 3%, expressed as the between-digestion relative standard deviation (n=4). was obtained for the majority of elements, except in cases limited by low analyte concentrations
Most Raman spectroscopic studies on tissue are performed in vitro. To assure that the results are applicable to in vivo examinations, preparation protocols and measurement procedures of tissue for in vitro studies should preserve tissue characteristics close to the native state. This study had two aims. The first was to elucidate if photoinduced effects arise during 5 minutes' continuous illumination of tissue with an 830 nm laser at an irradiance of 3 × 1010 W/m2. The second was to investigate the effects of snap-freezing of porcine prostate tissue in liquid nitrogen and subsequent storage at -80 °C, by means of multivariate analysis. 830 nm laser illumination of the specified irradiance did not affect the Raman spectra. A decrease of the spectral background was observed, likely due to photobleaching of tissue fluorophores. Snap-freezing and subsequent storage at -80 °C gave rise to subtle but significant alterations in Raman spectra, most likely related to changes in the protein conformations
Specific surface reactions on kaolinite were investigated by deuterium exchange of the hydroxyl protons of kaolinite, The kaolinite samples were reacted with deuterium oxide for 48 h and 2.5 and 5 weeks, at various pH values (3, natural and 8) and at different temperatures (ambient, and 30, 60 and 100 degrees C), Analyses were performed using diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy. The spectral results show that it is very difficult at room temperature to exchange the hydroxyl protons isotopically with deuterons at the surface of kaolinite, The temperature and the reaction time must be increased for successful exchange. It was found that the most suitable temperature for isotopic exchange was 60 degrees C. The pH did not significantly influence the deuteration, Only at high pH were changes of the OD bands in the DRIFT spectra observed, This study shows that it is possible to deuterate kaolinite without using intercalation. All three types of hydroxyl protons from the inner, inner surface and edge were exchanged.