Spectroscopic characterization and biological activity of dihydrazone transition metal complexes: crystal structure of 2,3-butanedione bis(isonicotinylhydrazone).

Metal complexes of the chloride, nitrate and acetate salts of Co(II), Ni(II) Cu(II), Zn(II), Cd(II) or Hg(II) with 2,3-butanedione bis(isonicotinylhydrazone) [BBINH] have been synthesized and structurally characterized. The crystal of BBINH was solved to crystallize as monoclinic system with space group of P121/c14. The formulae of the complexes were assigned based on the elemental analysis and mass spectra. The formation of BBINH complexes depend on the metal anion used. All complexes are nonelectrolytes except for the complexes 2, 3, 4 are (1:1) and 13 and 14 which are 1:2 electrolytes. BBINH behaves as a neutral tetradentate (N2O2) in the chloride complexes of Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II). In [Co2(BBINH)(H2O)Cl3]Cl⋅H2O, BBINH has the same dentate but with the two Co(II) ions. In the acetate complexes, [Ni2(BBINH-2H)(H2O)2(OAc)2]⋅3H2O and [Cu2(BBINH-2H)(OAc)2]⋅5H2O, BBINH acts as a binegative tetradentate with the two metal ions. The ligand in the nitrate complexes acts as a neutral bidentate via the two hydrazone azomethine C=NHy; the nitrate ions are ionic in the Cd(II) and Zn(II) complexes and covalent in the Ni(II) complex. The data are supported by NMR ((1)H and (13)C) spectra. The magnetic moments and electronic spectra of all complexes provide tetrahedral, square planar and/or octahedral structure. The decomposition of the complexes revealed the outer and inner solvents as well as the remaining residue based on TGA. The complexes have variable activities against some bacteria and fungi. The ligand is inactive against all tested organisms. The activity of Cd(II) and Hg(II) may be related to the geometry of the complexes.

Chelation, spectroscopic characterization, biological activity and crystal structure of 2,3-butanedione isonicotinylhydrazone: Determination of Zr(4+) after flotation separation.

New metal complexes of Co(II), Ni(II) Cu(II), Zn(II), Cd(II), Pd(II) and Hg(II) with 2,3-butanedione isonicotinylhydrazone [BINH] have been prepared and investigated. Single crystal for BINH is grown and solved as orthorhombic with P 21 21 2 space group. The formula of the ligand was assigned based on the elemental analysis, mass spectra and conductivity measurements. The complexes assigned the formulae [M(BINH-H)Cl]⋅nH2O (MCo(II), Ni(II), Cu(II), Zn(II); n=0 or 1); [Hg(BINH-H)(H2O)2Cl]; [Cd(BINH)Cl2]⋅2H2O and [Pd(BINH)Cl2]⋅H2O. All complexes are nonelectrolytes. BINH acts as a tridentate ligand in [M(BINH-H)Cl]⋅nH2O and [Hg(BINH-H)(H2O)2Cl] coordinating through COketonic, COamedic and CNhy and as a neutral bidentate through COketonic and CNhy in [Cd(BINH)Cl2]⋅2H2O and [Pd(BINH)Cl2]⋅H2O; the pyridine nitrogen has no rule in coordination. The data are supported by NMR ((1)H and (13)C) spectra. The magnetic moments and electronic spectra provide a tetrahedral structure for the Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes; square-planar for the Pd(II) complex and octahedral for the Hg(II) complex. The TGA of the complexes depicted the outer and inner water molecules as well as the final residue. The cobalt and cadmium complexes ended with the metal while the Cu(II), Zn(II) and Pd(II) complexes ended with complex species. [Hg(BINH-H)(H2O)2Cl] has no residue. The ligand is inactive against all tested organisms except for Bacillus thuringiensis. The Hg(II) complex is found more active than the other complexes. The flotation technique is found applicable for the separation of micro amount (10ppm) of Zr(4+) using 10ppm of BINH and 1×10(-5)molL(-1) of oleic acid at pH 6 with efficiency of 98% with no interferences.

Study of lead exposure from automobile exhaust as a risk for nephrotoxicity among traffic policemen.

BACKGROUND: Traffic policemen are the most exposed population to lead (Pb) from automobile exhaust. There has been increasing concern about the possible harmful effects of Pb from automobile exhaust on health of traffic policemen. However, no such study was concerned with the impact of Pb exposure on renal function among them. Therefore, we aimed to study the effect of Pb exposure from automobile exhaust on renal integrity among traffic policemen. METHODS: Markers of tubular damage [urinary excretion of beta(2)-microglobulin (beta(2)M), N-acetyl-beta-D-glucosaminidase (NAG), alkaline phosphatase (ALP) and gamma-glutamyl transferase (gamma-GT)], a marker of glomerular injury (albuminuria), and markers of glomerular filtration [serum creatinine, serum beta(2)M and blood urea nitrogen (BUN)] were determined in 43 traffic policemen (Pb-exposed group) and 52 matched healthy persons (control group). Pb levels in blood, urine, hair and nails were determined in the two groups as exposure indices of Pb. RESULTS: The results obtained show that the Pb-exposed group had higher Pb levels in blood, urine, hair and nails than the controls. Among the Pb-exposed group, Pb levels in blood, hair and nails showed significant and positive correlations with the duration of exposure to Pb which is measured as the duration of employment. Among the studied markers of kidney damage, urinary excretion of NAG and albumin were significantly higher in the Pb-exposed group than in the controls. Urinary excretion of NAG was positively correlated with duration of exposure, blood Pb and nail Pb. Urinary albumin was positively correlated with duration of exposure, blood Pb and hair Pb. The other markers of kidney damage were neither elevated nor correlated with exposure indices of Pb. CONCLUSION: Traffic policemen are liable to Pb toxicity, and the determination of Pb in blood, hair and nails are good markers of such toxicity. In these exposure conditions, kidney damage is possible. Such damage is both tubular and glomerular in nature and can be documented by determination of the urinary excretion of NAG and albumin.

Characterization and elimination of the interfering effects of foreign species in the atomic-absorption determination of iron.

The inhibition-release titration method has been used to study interference effects in flame atomic-absorption determination of iron. Interferences from anions, cations and complexing agents with the atomic-absorption of iron when a stoichiometric air-acetylene flame is used, can be obviated by a preliminary treatment of the sample solution with sulphosalicylic acid to convert the iron into the same complex before aspiration, thus giving a constant environment for the iron in the flame processes.