Determination of selenium in biological tissue samples rich in phosphorus using electrothermal atomization with Zeeman-effect background correction and (NH4)3RhCl6+citric acid as a mixed chemical modifier

Spectral interferences from phosphorus on the determination of selenium in biological tissue materials were not observed when a Zeeman-effect background correction was used with rhodium as a chemical modifier. A suppression effect on the selenium signal resulted when the concentration of phosphorus present was greater than 1.0 mg ml⁻¹. Rhodium was found to be more effective than palladium in overcoming the phosphate interference. Analytical procedures for the direct determination of trace selenium in standard reference materials by graphite furnace atomic absorption spectrometry following sample dissolution in nitric acid and hydrogen peroxide using a microwave oven has been described. The results obtained agreed favourably with the certified values.     

A problem in the spectrophotometric determination of dissolved total phosphorus in brackish anoxic waters

When dissolved total phosphorus in anoxic brackish waters was determined spectrophotometrically by the heteropoly molybdenum blue method after oxidation with potassium peroxodisulfate, negative dissolved organic phosphorus contents were obtained from the differences between the total phosphorus and inorganic phosphorus contents. A major cause of this inconsistency is coprecipitation of phosphate with the colloidal hydrated iron(III) oxide produced fro miron in these waters, or the formation of iron(III) phosphate during the oxidation process. The problem can be avoided by oxidation with nitric and perchloric acids.     

Microanalytical determination of tin in organotin compounds

Existing procedures for the determination of tin in organotin compounds are reviewed, and a new procedure is described which can be used for the rapid microanalysis of most organotin compounds. Wet oxidation with sulphuric acid and 30% hydrogen peroxide is followed by spectrophotometric determination of the extracted ternary tin(IV)-chloride-oxine complex in chloroform. Time for a single determination is 20 min, and the relative standard deviation is 0.7% for 1-5 mg of tin. On account of their volatility, methyltin compounds must be subjected to a sealed-tube wet oxidation in sulphuric-nitric acid mixture. Addition of sulphamic acid after boiling to remove most of the nitric acid makes this compatible with the solvent extraction step. Tin present as organotin stabilizer in PVC samples can also be determined by this method, after destruction of the organic matter with sulphuric acid and 50% hydrogen peroxide.     

Electronic structure of carbon nanotube network

Covalently cross-linked carbon nanotube network has been synthesized using spark plasma sintering followed by nitric acid treatment. EPR investigation of its electronic structure in comparison with pristine carbon nanotubes has revealed that the covalent cross-linking leads to a decrease in the number of paramagnetic centers, while the oxidation results in an increase in their number. The oxidation affects the cross-linked and pristine materials in a different manner     

Determination of molybdenum, chromium and aluminium in human urine by electrothermal atomic absorption spectrometry using fast-programme methodology

Rapid and direct procedures for the determination of molybdenum, chromium and aluminium in human urine samples are developed. Fast-programme methodology is used to simplify the heating cycles. Hydrogen peroxide, nitric acid and Triton X-100 are added to the urine samples which are directly introduced into the furnace. For molybdenum, two successive injection steps are required due to the low level of this element in the samples analyzed. Calibration is carried out using aqueous standards for aluminium and the standard additions method for both molybdenum and chromium. The reliability of the procedures is checked by analyzing two certified reference materials.     

Prospects for industrial implementation of the nitric acid processing of alkali aluminosilicate raw materials

The aim of this work is to attract attention of the scientific community and businessmen to fundamentally new technology for processing alkali aluminosilicate raw materials. The technology is based on the combination of two widely known processes, the manufacture of nitric acid by oxidation of atmospheric nitrogen in a nitrogen-oxygen plasma and the nitric acid processing of alkali aluminosilicate stock using a plasma at the step of thermal treatment of nitrate liquors. The results of a pilot-scale trial of the combined process are presented. Deceased.     

A comparison of two digestion procedures for the determination of selenium in biological material

Two digestion procedures have been tested on samples of flour, blood and urine for application in the determination of selenium by hydride-generation atomic-absorption spectrometry. The first utilizes a mixture of concentrated nitric, perchloric and sulphuric acids and the second a mixture of magnesium nitrate hexahydrate, concentrated nitric acid and 6M hydrochloric acid. The accuracy of the procedures was tested by analysis of standard reference materials and by comparison with results from neutron-activation analysis. It was found that the "magnesium method" can replace the more common procedure, which includes perchloric acid, for the sample types investigated in this paper.     

Caractérisation physicochimique et mécanique de matériaux céramiques obtenus à partir d'une argile kaolinitique du Burkina Faso

Physicochemical and mechanical characterization of ceramic materials obtained from a kaolinite-rich clay from Burkina Faso. The presence, even in the form of impurities and in small quantity, of alkaline or alkaline earth oxides in clay pastes can influence the thermal transformations during firing. We studied the influence of calcite on the products ceramics resulting from kaolinite-rich clay from Burkina Faso, while establishing correlations between their mechanical properties and their microstructure characteristics. It appears that the calcite addition affects the mechanical characteristics of the fired products by a broader distribution of the flexural strengths. The major parameter allowing one to connect the tenacity of these materials with the content of calcite of the initial paste is the mean free path in the solid phase.     

Determination of diamond

Analytical procedures are outlined for the determination of the diamond content of grinding wheels, drill crowns, saws, drills, hones, polishing powders and pastes, and other tools and materials employing industrial diamonds. Since the materials used as a matrix for industrial diamonds or a carrier for diamond abrasive powders may include a wide variety of metals, ceramics, plastics, cemented carbides, and organic pastes, the isolation and determination of diamond is often a rather complicated analytical task.     

Decomposition Studies of Aqueous Phase Ligands Used in Advanced Reprocessing Flowsheets

Two potential methods for decomposing organic ligands in nitric acid have been studied using acetic acid and diethylenetriaminepentaacetic acid (DTPA) as examples; these methods were oxidation by nitric acid at elevated temperatures (70-110 °C) and electrochemical oxidation, both direct and mediated electrochemical oxidation. Based on total carbon measurements, acetic acid proved to be rather stable against nitric acid oxidation whereas 60-80% of DTPA was decomposed at 100-110°C. Electrochemical oxidation methods were generally more effective in decomposing acetic acid and DTPA with mediated electrochemical oxidation using Ag(II) ions the most effective method under the conditions tested, with ∼80 and >90% loss of carbon from acetic acid and DTPA solutions respectively, at ambient temperature in 6 M HNO₃.