Comparison of slurry sampling and microwave-assisted digestion for calcium, magnesium, iron, copper and zinc determination in fish tissue samples by flame atomic absorption spectrometry

The development of a slurry sampling method for the determination of calcium, copper, iron, magnesium and zinc in fish tissue samples by flame atomic absorption spectrometry is described. In comparison with microwave-assisted digestion, the proposed method is simple, requires short time and eliminates total sample dissolution before analysis. Suspension medium was optimized for each analyte to obtain quantitative recoveries from fish tissue samples without matrix interferences. Nevertheless, iron recoveries higher than 46% were not found. Treatment of samples slurried in nitric acid by microwave irradiation for 15-30 s at 75-285 W permitted to achieve efficient recoveries for calcium, iron, magnesium and zinc. Further improvement in the matrix effects for iron determination was accomplished by the use of an additional step of short microwave-assisted suspension treatment. However, standard addition method was required for calcium and copper determination, being necessary hydrochloric acid as suspension medium for the last one. Although copper could not be determined in the certified reference material using microwave-assisted digestion, the accuracy of the slurry sampling method was verified for all the investigated analytes. Detection limits were 22.8 ± 8.0, 0.884 ± 0.092, 5.07 ± 0.76, 35.5 ± 0.7 and 1.17 ± 0.04 μg g⁻¹ for calcium, copper, iron, magnesium and zinc, respectively. The standard deviations obtained using slurry sampling method and microwave-assisted digestion were not significantly different, and the mean relative standard deviation of the over-all method (n = 3) of the slurry sampling method for different concentration levels was below 12%.     

Calorimetric studies of refractory corundum

Calorimetry has been used in the investigations of calcium aluminate materials produced as a binder for aluminate-corundum composites of high refractoriness. The kinetics and of hydration process was thus characterized and the optimum compositions of initial binders and cement-corundum refractory filler blends could be selected for further tests. The acceleration of heat evolution - the shortening of so-called induction period and relatively high heat output in the presence of corundum was observed. It means the acceleration of hydration process, that is early crystallisation of hydration products and subsequent further dissolution of initial anhydrous aluminate phases. In the presence of fine grained corundum particles these phenomena should be attributed to the nucleating effect of fine corundum particles. This revised version was published online in July 2006 with corrections to the Cover Date.     

The effect of calcining conditions on the rehydration of dead burnt magnesium oxide using magnesium acetate as a hydrating agent

Summary Magnesium oxide was produced through calcination of magnesite ore. A rehydration percentage of MgO to Mg(OH)₂ of higher than 60% is obtained using calcination temperatures of 1000°C and below. At these temperatures medium reactive MgO was formed. The extend to which dead burnt MgO (obtained after calcination at 1200°C and higher) may be rehydrated is dependent on the calcination time, but even after 1 h and using magnesium acetate as a hydrating agent only 40% of the initial product has rehydrated to Mg(OH)₂. After 4 and more hours of calcinations at 1200°C, a maximum of approximately 14% of the initial MgO is rehydrated back to Mg(OH)₂. Thermogravimetric analysis was performed on the various compounds to determine the amounts of Mg(OH)₂ that formed.     

An ab initio molecular orbital study of the grignard reagents CH3MgCl and [CH3MgCl]2: The Schlenk equilibrium

Ab initio molecular orbital calculations are used to study the modified Schlenk equilibrium: 2RMgCl (RMgCl)² MgR₂ + MgCl₂ Mg(Cl₂)MgR₂ with R=H and CH₃. In the absence of any solvents, calculations indicate that the formation of the various possible bridged dimers (RMgCl)₂ is substantially exothermic. However, using dimethylether as a model solvent, we show that the formation of the dimer (Me₂O)(CH₃)Mg(Cl₂)Mg(CH₃)(OMe₂) is exothermic only when entropic effects are included.     

Syntheses and structures of magnesium pyridine thiolates--model compounds for magnesium binding in photosystem I

Novel magnesium pyridine-2-thiolates were prepared by using alkane elimination chemistry. The resulting complexes display a metal coordination environment composed of sulfur/nitrogen bonding from the intramolecularly stabilized mercaptopyridine ligand, in addition to coordination by the oxygen centers from two THF donors. The compounds are well-suited model compounds for the magnesium centers in Photosystem I, in which magnesium, situated in the central chlorophyll ligand, is bound to sulfur from a nearby methionine residue. All compounds were characterized by (1)H, (13)C NMR, and IR spectroscopy, in addition to Xray crystallography.     

Defect clusters and precipitation/oxidation of MgO-Co1−xO solid solution

MgO and Co_1−xO powders in 9:1 and 1:9 molar ratio (denoted as M₉C₁ and M₁C₉, respectively) were sintered and homogenized at 1600°C followed by annealing at 850°C and 800°C, respectively to form defect clusters and precipitates. Analytical electron microscopic observations indicated the protoxide remained as rock salt structure with complicated planar diffraction contrast for M₉C₁ sample, however with spinel paracrystal precipitated from the M₁C₉ sample due to the assembly of charge- and volume-compensating defects of the 4:1 type, i.e., four octahedral vacant sites surrounding one Co³⁺-filled tetrahedral interstitial site. The spacing of such defect clusters is 4.5 times the lattice spacing of the average spinel structure of Mg-doped Co_3−δO₄, indicating a higher defect cluster concentration than undoped Co_3−δO₄. The {111} faulting of Mg-doped Co_3−δO₄/Co_1−xO in the annealed M₁C₉ sample implies the possible presence of zinc blend-type defect clusters with cation vacancies assembled along oxygen close packed (111) plane.     

Coprecipitation with metal hydroxides for the determination of beryllium in seawater by graphite furnace atomic absorption spectrometry

Coprecipitation first with magnesium hydroxide, next with tin(IV) hydroxide is developed for the determination of traces of beryllium in sea-water. To a 200-ml sample is added a sodium hydroxide solution to form magnesium hydroxide at pH 11.5, on which beryllium is quantitatively coprecipitated. The precipitate is separated by centrifugation and dissolved in 2 ml of 12 mol/l hydrochloric acid. The resulting solution (ca. 10 ml) is mixed with 2 mg of tin (IV) carrier and the pH is adjusted to 5.0 to collect the beryllium on tin (IV) hydroxide, leaving magnesium ions in the solution. The tin (IV) hydroxide is centrifuged, dissolved in 0.1 ml of 5 mol/l hydrobromic acid, and then diluted to 1 ml with water. Magnesium is so added as to be 500 g/ml for increasing the sensitivity about four times, and the beryllium in the solution is determined by graphite furnace atomic absorption spectrometry. The experiments with synthetic seawater samples showed that pg — g amounts of beryllium can be coprecipitated on the metal hydroxides and beryllium at the low ng/1 level can be determined with reasonable precision (RSD < 10%). The detection limit of the proposed method is 0.5 ng/l of beryllium in seawater.     

2型糖尿病患者血清钙镁与甲状腺激素含量变化及临床意义

为了监测 2型糖尿病人血清钙、镁和甲状腺激素含量 ,分析其临床意义及相关性 ,应用放射免疫分析法测定了 1 1 5例 2型糖尿病及 1 5 0例健康人血清甲状腺激素含量。同时用美国杜邦RXL自动生化仪测定了其血清钙、镁含量。结果表明 ,在 2型糖尿病伴有明显并发症者血镁、FT3水平明显降低 (P <0 0 5 ) ,钙镁两种元素与甲状腺激素水平无明显相关性。 2型糖尿病患者适当补镁对预防其并发症是有益的 ,测定FT3 等可作为判断 2型糖尿病严重程度和估计预后的参考指标。     

草酸镁二水合物的非等温热分解动力学

The thermal decomposition of the magnesium oxalate dihydrate in a static air atmosphere was investigated by TG-DTG techniques. The intermediate and residue of each decomposition were identified from their TG curve. The kinetic triplet, the activation energy E, the pre-exponential factor A and the mechanism functionsf（a） were obtained from analysis of the TG-DTG curves of thermal decomposition of the first stage and the second stage by the Popesou method and the Flynn-Wall-Ozawa method.     

Thermoanalytical study of glibenclamide and excipients

Summary Taking into account the problems of desertification and agricultural practices able to provide income to the population at the semi-arid region of North-East Brazil, this work presents the results of the chemical and thermal characterization by TG and DSC of the seed derivatives of Cnidoscolus quercifolius, hereinafter called faveleira, aiming at the application of these materials as an alternative of food source for animals and for the human population at this region. The faveleira seed derivatives present thermodynamic properties similar to the ones of other foods utilized for human use, as well as an acceptable calorific value. According to TG and DSC results, was verified that the faveleira derivatives presents good thermal and oxidative stabilities.