Determination of trace elements in Brazilian rice grains and in biological reference materials by neutron activation analysis

Instrumental neutron activation analysis was applied to the determination of the elements Na, K, Br, As, Rb, Zn, Co, Fe and Sc in Brazilian rice samples and in biological standards. Hg and Se concentrations were determined by using a simple radiochemical separation. The chemical procedure was carried out by means of distillation of Hg and Se in HBr medium and subsequent precipitation of selenium by sodium metabisulfite and mercury by thioacetamide. The accuracy of the instrumental and radiochemical methods was evaluated by means of analysis of the Reference Materials NBS-Bovine Liver, Bowen's Kale and NBS-Rice Flour.     

Evaluation of Zn and Fe in diets of patients with chronic renal failure

Having in mind the importance of Fe and Zn content in the diets of nondialyzed patients with chronic renal failure, diets of 39 patients with ages varying from 18 to 79 years under a conservative treatment were analyzed by INAA. The 24-hour recall method was used for sample collection. The content of proximate composition was also determined. The average daily dietary intake was compared to the new recommended values by the Food and Nutrition Board. It was observed that the diets were deficient for these elements and, therefore, there should be a nutritional follow-up to avoid possible negative effects. This revised version was published online in August 2006 with corrections to the Cover Date.     

New far infrared laser lines obtained by optically pumping13CD3OD

We have obtained laser action on 34 far infrared lines for the first time in fully deuterated methyl alcohol with the¹³C isotope (¹³CD₃OD), and we have measured the frequency of 13 lines. The molecule was pumped by a cw CO₂ laser. We have measured the wavelength, the relative polarization, the relative intensity of most lines, the frequency, and the CO₂ pump frequency offset of the strongest lines. The new lines are distributed in the wavelength region from 75.27 m to 464.7 m.Supported in part by a joint grant with the U.S. National Science Foundation grant # INT 80-19014 and the Brazilian Conselho Nacional de Pesquisas (CNPq).     

Activation analysis of alkaline rocks. A comparison between destructive and non-destructive methods

The United States Geological Survey reference sample AGV-1 andesite, and three alkaline rocks from the apatite mine of Jacupiranga, Brasil, were analyzed by thermal neutron activation analysis using destructive and non-destructive methods, and high resolution Ge(Li) gamma-ray detectors. One of the rocks, a carbonatite, was also analyzed by instrumental activation analysis with epithermal neutrons. A greater number of elements can be determined using the radiochemical separation, but the precision and accuracy attained by INAA and RNAA were of the same order for most of the elements analyzed. Epithermal activation was more advantageous for tantalum, terbium and holmium. Comparison of the analytical results for USGS reference sample (AGV-1) with the data published by others gave good agreement. Statistical tests used for comparison of the results of destructive and non-destructive methods, as well as other results are presented.     

New FIR laser lines and frequency measurements in CD3OD

Twenty-four new submillimeter laser lines in fully deuterated methyl alcohol (CD₃OD) in the wavelength range from 52 to 328 m have been obtained in a Fabry-Perot FIR resonator by optically pumping the methanol with a cw CO₂ laser. We have made accurate wavelength measurements and have determined the relative polarization of most of the known CD₃OD laser lines. The frequencies of 13 of the strongest lines were also measured.Contribution of the U.S. Government, not subject to copyright.     

13C NMR quantification of mono and diacylglycerols obtained through the solvent‐free lipase‐catalyzed esterification of saturated fatty acids

In the present investigation, we studied the enzymatic synthesis of monoacylglycerols (MAG) and diacylglycerols (DAG) via the esterification of saturated fatty acids (stearic, palmitic and an industrial residue containing 87% palmitic acid) and glycerol in a solvent‐free system. Three immobilized lipases (Lipozyme RM IM, Lipozyme TL IM and Novozym 435) and different reaction conditions were evaluated. Under the optimal reaction conditions, esterifications catalyzed by Lipozyme RM IM resulted in a mixture of MAG and DAG at high conversion rates for all of the substrates. In addition, except for the reaction of industrial residue at atmospheric pressure, all of these products met the World Health Organization and European Union directives for acylglycerol mixtures for use in food applications. The products were quantified by ¹³C NMR, with the aid of an external reference signal which was generated from a sealed coaxial tube filled with acetonitrile‐d3. After calibrating the area of this signal using the classical external reference method, the same coaxial tube was used repeatedly to quantify the reaction products. Copyright © 2012 John Wiley & Sons, Ltd.     

Synthesis and Structural Determination of New Potential Chiral Tridentate Ligands Derivated from 1-(R)-(+)-Camphor

New alcohols 3d, 3e and 3f were efficiently prepared in enantiopure form (2 steps, 50–58%), from available 1-(R)-(+)-camphor 1. The absolute configurations were assigned by NMR and relative X-ray crystallographic analysis.