A pre-irradiation separation procedure based on ion-exchange chromatography for gallium determination in biological and environmental materials by neutron activation analysis

A pre-irradiation separation procedure, for gallium determination in biological and environmental materials by neutron activation analysis (NAA) is reported. The proposed method, based on ion-exchange chromatography, allows to eliminate the radiation risk, while taking the advantages of high sensitivity of NAA. The single comparator method is employed for gallium quantitative evaluation. Since no standard reference materials with certified gallium contents were available, the reliability of the proposed method was extensively investigated by various approaches. Four biological and one environmental standard reference materials, with gallium contents ranging from 54 g/g-3 ng/g, have been analyzed.     

Mössbauer and XRD Comparative Study of Host Rock and Iron Rich Mineral Samples from Paz del Rio Iron Ore Mineral Mine in Colombia

The local environment of implanted ¹¹¹Ag (t _1/2 = 7.45 d) in single-crystalline [0001] ZnO was evaluated by means of the perturbed angular correlation (PAC) technique. Following the 60 keV low dose (1 × 10¹³ cm⁻²) ¹¹¹Ag implantation, the PAC measurements were performed for the as-implanted state and following 30 min air annealing steps, at temperatures ranging from 200 to 1050°C. The results revealed that 42% of the probes are located at defect-free S_Zn sites (ν _Q ∼ 32 MHz, η = 0) in the as-implanted state and that this fraction did not significantly change with annealing. Moreover, a progressive lattice recovery in the near vicinity of the probes was observed. Different EFGs assigned to point defects were furthermore measured and a general modification of their parameters occurred after 600°C. The 900°C annealing induced the loss of 30% of the ¹¹¹Ag atoms, 7% of which were located in regions of high defects concentration.     

Tin(IV) complexes obtained by reacting 2-benzoylpyridine-derived thiosemicarbazones with SnCl4 and Ph2SnCl2

Reaction of 2-benzoylpyridine thiosemicarbazone (H2Bz4DH, HL1) and its N(4)-methyl (H2Bz4Me, HL2) and N(4)-phenyl (H2Bz4Ph, HL3) derivatives with SnCl₄ and diphenyltin dichloride (Ph₂SnCl₂) gave [Sn(L1)Cl₃] (1), [Sn(L1)PhCl₂] (2), [Sn(L2)Cl₃] (3), (4) [Sn(L3)PhCl₂] (5) and [Sn(L3)Ph₂Cl] (6). Infrared and ¹H, ¹³C and ¹¹⁹Sn NMR spectra of 1-3, 5 and 6 are compatible with the presence of an anionic ligand attached to the metal through the N_py-N-S chelating system and formation of hexacoordinated tin complexes. The crystal structures of 1-3, 5 and 6 show that the geometry around the metal is a distorted octahedron formed by the thiosemicarbazone and either chlorides or chlorides and phenyl groups. The crystal structure of 4 reveals the presence of and trans [Ph₂SnCl₄]²⁻.     

Trace element characterization by INAA of three sediments to be certified as standard reference materials

Three environmental matrices proposed as Certified Reference Materials, issued by the EU Standards, Measurement and Testing Programme (SMTP) formerly Bureau Communautaire de Reference (BCR) have been characterized for their trace element contents.The materials are: BCR 277 R Estuarine Sediment, BCR 280 R Lake Sediment and BCR 320 R Channel Sediment.Several trace elements, including As, Co, Cr, Fe, Mn, Ni, Sb, Sc, Th, U and Zn have been determined by our laboratory using Instrumental Neutron Activation Analysis (INAA). Our contributed values are being considered for the final certification.     

Synthesis of a Novel Nickel(II) Complex with Dithiocarbimate from Sulfonamide

Potassium N-4-methylphenylsulfonyldithiocarbimate, K₂(4-CH₃C₆H₄SO₂N=CS₂), reacted with nickel(II) chloride hexahydrate and tetrabutylammonium bromide to form the bis(N-4-methylphenylsulfonyldithiocarbimate)nickelate(II) tetrabutylammonium salt (Bu₄N)₂[Ni(4-CH₃C₆H₄S₂C=NSO₂)₂]. The elemental analyses, IR and UV-Vis data obtained were consistent with the formation of a diamagnetic planar complex. The ¹H NMR and the ¹³C NMR spectra showed the expected signals for the dithiocarbimate moiety and the tetrabutylammonium cation. The single-crystal structure analysis showed that this substance crystallizes in the triclinic space group with a = 10.474(3) Å, b = 10.767(3) Å, c = 13.657(3) Å and = 81.54(2)°, = 80.44(2)°, = 67.63(2)°, V = 1398.5(8) ų, and Z = 2. The nickel atom is coordinated to four sulfur atoms.     

Minor and trace element contents in pituitary gland of “normal” humans: an evaluation of analytical data

In the study of trace elements in the different human brain areas, a critical evaluation of the values available in the literature is of great importance in attempting to establish reliable baseline levels, i.e., Reference Values (RVs) for toxicological assessment studies.This paper reviews the published values of minor and trace elements in the pituitary gland (hypophysis) of “normal” humans.Eighteen published papers are taken into account, 15 of which refer to the entire gland, whereas in three of them, only the adenohypophysis is considered.It turns out that essential elements such as Cu, Fe, Se and Zn were more frequently determined, whereas As, Br, Ca, Co, Cr, Cs, K, Mg, Mn, Ni and Rb were seldom investigated.Mercury was determined by several authors because of the concern caused by Hg release from dental amalgam fillings.Most values were obtained by Neutron Activation Analysis (NAA), which appears to have played a pioneer role in this field.Literature data on trace element levels in pituitary gland are at present insufficient to establish RVs; rather, they can be considered only as indicative values.Future investigations based on large populations of control subjects, with standardization of the preanalytical factors and the use of fit-for-purpose Standard or Certified Reference Materials (SRMs, CRMs) should therefore be envisaged.     

Mössbauer effect study of natural chromites of Brazilian and Philippine origin

Mössbauer spectroscopy has been used to study nine natural chromite samples from deposits throughout Brazil and one sample from Philippine. It was possible to identify three different groups of chromite spinels, depending on the iron distribution over tetrahedral and octahedral sites. Using the Mössbauer Fe³⁺/Fe²⁺ ratio, chemical analysis and x-ray data a chemical formula was proposed for each group.