Application of Scanning Electron Microscopy and X-Ray Evaluation of the Main Digestion Methods for Determination of Macroelements in Plant Tissue

Three commonly used digestion methods (dry ashing, acid digestion, and microwave digestion) in different variants were compared for digestion of tobacco leaves. Three main macroelements (K, Ca and Mg) were analysed using AAS Spectrometer Spectra АА 220, Varian, Australia. The accuracy and precision of the measurements were evaluated by using Polish reference material CTR-VTL-2 (Virginia tobacco leaves). To elucidate the problems with elemental recovery X-Ray and SEM–EDS analysis of all residues after digestion were performed. The X-ray investigation showed a formation of KClO4 when HClO4 was used as a part of the acids mixture. The use of HF at Ca and Mg determination led to the formation of CaF2 and MgF2. The results were confirmed by energy dispersive X-ray microanalysis. SPSS program for Windows was used for statistical data processing.

Seasonal Variation of the Impact of Mining Activities on Ga-Selati River in Limpopo Province, South Africa

Water is a very rare natural resource in South Africa. Ga-Selati River is used for both domestic and industrial purposes. This study was carried out in order to assess the quality of Ga-Selati River in a mining area of Limpopo Province-Phalaborwa. The pH, Electrical Conductivity (EC) and Total Dissolved Solids (TDS) were determined using a Crinson multimeter while turbidity was measured using a Labcon Turbidimeter. The concentrations of Al, Ca, Cd, Cr, Fe, K, Mg, Mn, Na and Pb were analysed in triplicate using a Varian 520 flame atomic absorption spectrometer (AAS) supplied by PerkinElmer, after acid digestion with nitric acid in a fume cupboard. The average pH of the river from eight different sampling sites was 8.00 and 9.38 in wet and dry season respectively. Higher EC values were determined in the dry season (138.7 mS/m) than in the wet season (96.93 mS/m). Similarly, TDS values were higher in dry (929.29 mg/L) than in the wet season (640.72 mg/L) season. These values exceeded the recommended guideline of South Africa Department of Water Affairs and Forestry (DWAF) for domestic water use (70 mS/m) and that of the World Health Organization (WHO) (600 mS/m), respectively. Turbidity varied between 1.78-5.20 and 0.95-2.37 NTU in both wet and dry seasons. Total hardness of 312.50 mg/L and 297.75 mg/L as the concentration of CaCO3 was computed for the river in both the wet and the dry seasons and the river water was categorised as very hard. Mean concentration of the metals studied in both the wet and the dry seasons are: Na (94.06 mg/L and 196.3 mg/L), K (11.79 mg/L and 13.62 mg/L), Ca (45.60 mg/L and 41.30 mg/L), Mg (48.41 mg/L and 44.71 mg/L), Al (0.31 mg/L and 0.38 mg/L), Cd (0.01 mg/L and 0.01 mg/L), Cr (0.02 mg/L and 0.09 mg/L), Pb (0.05 mg/L and 0.06 mg/L), Mn (0.31 mg/L and 0.11 mg/L) and Fe (0.76 mg/L and 0.69 mg/L). Results from this study reveal that most of the metals were present in concentrations higher than the recommended guidelines of DWAF and WHO for domestic use and the protection of aquatic life.

Application of a Modified BCR Approach to Investigate the Mobility and Availability of Trace Elements (As, Ba, Cd, Co, Cr, Cu, Mo,Ni, Pb, Zn, and Hg) from a Solid Residue Matrix Designed for Soil Amendment

Trace element speciation of an integrated soil amendment matrix was studied with a modified BCR sequential extraction procedure. The analysis included pseudo-total concentration determinations according to USEPA 3051A and relevant physicochemical properties by standardized methods. Based on the results, the soil amendment matrix possessed neutralization capacity comparable to commercial fertilizers. Additionally, the pseudo-total concentrations of all trace elements included in the Finnish regulation for agricultural fertilizers were lower than the respective statutory limit values. According to chemical speciation, the lability of trace elements increased in the following order: Hg < Cr < Co < Cu < As < Zn < Ni < Pb < Cd < V < Mo < Ba. The validity of the BCR approach as a tool for chemical speciation was confirmed by the additional acid digestion phase. Recovery of trace elements during the procedure assured the validity of the approach and indicated good quality of the analytical work.

Thermal and Electrical Properties of Carbon Nanotubes Purified by Acid Digestion

Carbon nanotubes (CNTs) possess unique structural, mechanical, thermal and electronic properties, and have been proposed to be used for applications in many fields. However, to reach the full potential of the CNTs, many problems still need to be solved, including the development of an easy and effective purification procedure, since synthesized CNTs contain impurities, such as amorphous carbon, carbon nanoparticles and metal particles. Different purification methods yield different CNT characteristics and may be suitable for the production of different types of CNTs. In this study, the effect of different purification chemicals on carbon nanotube quality was investigated. CNTs were firstly synthesized by chemical vapor deposition (CVD) of acetylene (C2H2) on a magnesium oxide (MgO) powder impregnated with an iron nitrate (Fe(NO3)3·9H2O) solution. The synthesis parameters were selected as: the synthesis temperature of 800°C, the iron content in the precursor of 5% and the synthesis time of 30 min. The liquid phase oxidation method was applied for the purification of the synthesized CNT materials. Three different acid chemicals (HNO3, H2SO4, and HCl) were used in the removal of the metal catalysts from the synthesized CNT material to investigate the possible effects of each acid solution to the purification step. Purification experiments were carried out at two different temperatures (75 and 120 °C), two different acid concentrations (3 and 6 M) and for three different time intervals (6, 8 and 15 h). A 30% H2O2 : 3M HCl (1:1 v%) solution was also used in the purification step to remove both the metal catalysts and the amorphous carbon. The purifications using this solution were performed at the temperature of 75°C for 8 hours. Purification efficiencies at different conditions were evaluated by thermogravimetric analysis. Thermal and electrical properties of CNTs were also determined. It was found that the obtained electrical conductivity values for the carbon nanotubes were typical for organic semiconductor materials and thermal stabilities were changed depending on the purification chemicals.