Irradiation techniques for the release of bound heavy metals in natural waters and blood

Irradiation techniques are compared with conventional acid digestion procedures for the release of bound heavy metals in natural waters and in blood, before their determination by anodic stripping voltammetry. Ultra-violet irradiation of acidified water with a 550-W mercury vapour lamp releases bound zinc, cadmium, lead and copper after 4 h. The same results can be achieved with a 30-Mrad dose of high-energy γ-irradiation. These techniques are also effective for the release of metals in whole blood and blood plasma, where sample volumes as small as 200 μl are adequate in analyses for zinc, copper and lead. By comparison with acid digestion and solvent extraction methods, irradiation treatments offer the advantages of minimum sample manipulation and negligible reagent blanks.     

Dynamic nuclear polarization at 9T using a novel 250 GHz gyrotron microwave source. 2003

In this communication, we report enhancements of nuclear spin polarization by dynamic nuclear polarization (DNP) in static and spinning solids at a magnetic field strength of 9 T (250 GHz for g = 2 electrons, 380 MHz for ¹H). In these experiments, ¹H enhancements of up to 170 ± 50 have been observed in 1-¹³C-glycine dispersed in a 60:40 glycerol/water matrix at temperatures of 20 K; in addition, we have observed significant enhancements in ¹⁵N spectra of unoriented pf1-bacteriophage. Finally, enhancements of ∼17 have been obtained in two-dimensional ¹³C–¹³C chemical shift correlation spectra of the amino acid U–¹³C, ¹⁵N-proline during magic angle spinning (MAS), demonstrating the stability of the DNP experiment for sustained acquisition and for quantitative experiments incorporating dipolar recoupling. In all cases, we have exploited the thermal mixing DNP mechanism with the nitroxide radical 4-amino-TEMPO as the paramagnetic dopant. These are the highest frequency DNP experiments performed to date and indicate that significant signal enhancements can be realized using the thermal mixing mechanism even at elevated magnetic fields. In large measure, this is due to the high microwave power output of the 250 GHz gyrotron oscillator used in these experiments.     

Measurement of the absolute Raman scattering cross sections of sulfur and the standoff Raman detection of a 6‐mm‐thick sulfur specimen at 1500 m

The absolute Raman scattering cross sections (σ_RS) for the 471, 217, and 153 cm⁻¹ modes of sulfur were measured as 6.0 ± 1.2 × 10⁻²⁷, 7.7 ± 1.6 × 10⁻²⁷, and 1.2 ± 0.24 × 10⁻²⁶ cm² at 815, 799, and 794 nm, respectively, using a 785‐nm pump laser. The corresponding values of σ_RS at 1120, 1089, and 1081 nm were determined to be 1.5 ± 0.3 × 10⁻²⁷, 1.2 ± 0.24 × 10⁻²⁷, and 1.2 ± 0.24 × 10⁻²⁷ cm² using a 1064‐nm laser. A temperature‐controlled, small‐cavity (2.125 mm diameter) blackbody source was used to calibrate the signal output of the Raman spectrometers for these measurements. Standoff Raman detection of a 6‐mm‐thick sulfur specimen located at 1500 m from the pump laser and the Raman spectrometer was made using a 1.4‐W, CW, 785‐nm pump laser. Copyright © 2010 John Wiley & Sons, Ltd.