Removal of bromophenol blue from polluted water using a novel azo-functionalized magnetic nano-adsorbent.

Water pollution from organic dyes poses a serious danger to the environment. In the present work, we report a novel adsorbent (ADFS) based on azo-dye-functionalized superparamagnetic iron oxide nanoparticles (SPIONs) for the removal of the anionic dye bromophenol blue (BPB) from contaminated water. The fabricated SPIONs, azo dye, and ADFS adsorbent were characterized with FTIR and UV-vis absorption spectroscopy, 1HNMR spectroscopy, mass spectrometry, SEM imaging, dynamic light scattering (DLS), zeta potential measurements, vibrating sample magnetometry, thermogravimetric analysis, differential thermal analysis, and X-ray diffraction analysis. DLS measurements showed a particle size of 46.1 and 176.5 nm for the SPIONs and the ADFS, respectively. The adsorbent exhibited an adsorption capacity of 7.43 mg g-1 and followed the pseudo-second-order kinetics model (r2 = 0.9981). The ADFS could efficiently remove BPB from water after stirring for 120 minutes at room temperature and pH 2. The adsorption process was proved to occur via physisorption, as revealed by the Freundlich isotherm (n = 1.82 and KF = 11.5). Thermodynamic studies implied that the adsorption is spontaneous (-8.03 ≤ ΔG ≤ -0.58 kJ mol-1) and enthalpy-driven might take place via van der Waals interactions and/or hydrogen bonding (ΔH = -82.19 kJ mol-1 and ΔS = -0.24 kJ mol-1 K-1).

Azo-functionalized superparamagnetic Fe3O4 nanoparticles: an efficient adsorbent for the removal of bromocresol green from contaminated water.

Water contamination is regarded as one of the world's worst tragedies owing to the continual depletion of water resources suitable for drinking and agriculture. Researchers have recently been interested in developing novel and more effective adsorbents for wastewater purification. We report herein a magnetic adsorbent nanomaterial for the removal of the anionic dye bromocresol green (BCG) from wastewater. The adsorbent is based on superparamagnetic iron oxide (cubic Fe3O4) nanoparticles (SPIONs) coated with a high-molecular-weight azo dye synthesized via diazo coupling of vitamin B1 with a trisubstituted benzene derivative. The proposed adsorbent was characterized using scanning electron microscopy, FTIR and 1H-NMR spectroscopy, mass spectrometry, dynamic light scattering, vibrating sample magnetometry, thermal analysis, and X-ray diffraction crystallography. At room temperature and pH 2.0, the synthesized adsorbent showed an average particle size of 65.9 ± 8.0 nm, a high magnetization saturation (65.58 emu g-1), a high equilibrium adsorption capacity (36.91 mg g-1). Adsorption of BCG was found to take place via a physisorption mechanism and followed a pseudo-second-order rate kinetics. Thermodynamic studies revealed that the adsorption process is enthalpy driven by hydrogen bonding and/or van der Waals interactions. After treating water samples with the suggested adsorbent, it can be easily removed from water using a strong external magnetic field.

Evaluation of Human Wharton's Jelly-Derived Mesenchymal Stem Cells Conditioning Medium (hWJ-MSCs-CM) or Scorpion Venom Breast Cancer Cell Line In Vitro.

PURPOSE: The present study aimed to evaluate the anticancer potential of Egyptian scorpion Leiurus quinquestriatus venom (ScV) or human Wharton's jelly-derived mesenchymal stem cells conditioning medium (hWJ-MSCs-CM)/CM against breast cancer (MCF-7) cell line as an alternative effective cancer biotherapy. METHODS: Venom (ScV) toxicity was performed recording concentration-dependent viability % and ScV IC50 value was in the order of 100 µg/ml. MCF-7 were treated with hWJ-MSCs-CM used as (25%, 50%, and 75% ml) or the IC50 of ScV. Apoptotic activity was traced via evaluation the apoptotic (Bax, Casp-3, and Casp-9) and anti-apoptotic genes (Bcl2, ALDOA, and PKM2) profile. RESULTS: Both Bax and Casp-3 showed a significant upregulation while anti-apoptotic genes were significantly downregulated. In the meantime, Casp-3 and Casp-9 protein were monitored using ELISA, and their level was less than in control. Additionally, MCF-7 apoptosis was monitored using flow cytometry recording a significant DNA accumulation in the G0-G1 and S phases in case of cell treatment with ScV or CM75% ml and 50% ml. Also, there was a significant total necrotic cells % compared with control cells, and total apoptosis under the effect of ScV or CM75% ml was significantly elevated than rest of treatment. CONCLUSION: Apoptosis induction was both dose- and time-dependent for hWJ-MSCs-CM and ScV. According to the present study and other studies, there is an ample evidence that hWJ-MSCs-CM and the venom IC50 abolish tumor growth.

Matrix-dispersed magnetic molecularly-imprinted polyaniline for the effective removal of chlorpyrifos pesticide from contaminated water.

We report a new adsorbent nanocomposite material based on matrix-dispersed superparamagnetic iron oxide nanoparticles (SPIONs) in molecularly-imprinted polyaniline for the removal of chlorpyrifos (CPF), a hazardous organophosphate pesticide, from water. The synthesized magnetic molecularly-imprinted polymer (MMIP) was characterized by FTIR spectroscopy, XRD, magnetic susceptibility, DLS, zeta potential measurement, SEM and high-resolution TEM imaging. The average size of the naked SPIONs ranges from 15 to 30 nm according to the high-resolution TEM analysis. Moreover, the adsorption kinetics, thermodynamic parameters (ΔG, ΔH and ΔS), adsorption isotherms and rebinding conditions were investigated in detail. The proposed MMIP has an imprinting factor of 1.64. In addition, it showed a high experimental adsorption capacity of 1.77 mg g-1 and a removal efficiency of nearly 80%. The fabricated MMIP material demonstrated excellent magnetic susceptibility allowing for easy separation using an external magnetic field. The adsorption mechanism of CPF onto the MMIP adsorbent followed the second-order kinetics model and fitted to the Temkin adsorption isotherm. By studying the adsorption thermodynamics, negative ΔG values (-1.955 kJ mol-1 at room temperature) were obtained revealing that the adsorption process is spontaneous. Furthermore, the maximum adsorption capacity was obtained at room temperature (ca. 303 K), neutral pH and using a high CPF concentration.

Antimicrobial ruthenium complex coating on the surface of titanium alloy. High efficiency anticorrosion protection of ruthenium complex.

A ruthenium complex was prepared and structurally characterized using various techniques. Antibacterial and antifungal activities of ruthenium complex were evaluated. High significant antimicrobial activity against Escherichia coli, Staphylococcus aureus and Candida albicans was recorded. Minor cytotoxicity records were reported at the highest concentration level using MTT assay. The influence of Cu(II), Cr(III), Fe(III) and Ru(III) metal ions of salen Schiff base on the corrosion resistance of Ti-alloy in 0.5M HCl was studied. In vitro corrosion resistance was investigated using electrochemical impedance spectroscopy (EIS) measurements and confirmed by surface examination via scanning electron microscope (SEM) technique. Both impedance and phase angle maximum (θ(max)) values were at maximum in the case of the ruthenium complex with promising antibacterial and antifungal activities. The surface film created by the ruthenium complex was highly resistant against attack or deterioration by bacteria. The EIS study showed high impedance values for the ruthenium complex with increasing exposure time up to 8 days. SEM images showed uniform distribution and adsorption of Ru(III) ions on Ti-alloy surface. The ruthenium complex, as a model of organic-inorganic hybrid complex, offered new prospects with desired properties in industrial and medical applications.

Design and synthesis of novel complexes containing N-phenyl-1H-pyrazole moiety: Ni complex as potential antifungal and antiproliferative compound.

Cu(II) (1), Ni(II) (2), Cr(III) (3) and Fe(III) (4) complexes with 3-acetyl-4-benzoyl-1-phenyl-1H-pyrazole (L1) were prepared and structurally characterized. Usual coordination of L1 was achieved through nitrogen of pyrazole moiety and carbonyl acetyl group. Electronic spectra of the complexes indicate that the geometry of the metal center was six coordinate octahedral. In vitro antimicrobial activity of the ligand and complex compounds was screened in terms of antibacterial effect on Staphylococcus aureus (Gram-positive), Escherichia coli (Gram-negative) and antifungal effect on the fungi Aspergillus flavus and candida albicans using the modified Kirby-Bauer disc diffusion and minimum inhibitory concentrations (MIC) methods. Ni(II) complex (2) exhibited remarkable antifungal inhibition against Candida albicans equal to the standard antifungal agent. To continue our study some structural modifications are formed by adding 4-fluoro-benzoyl moiety to L1 in different forms to produce different ligands, 3-acetyl-4-(4-flourobenzoyl)-1-phenyl-1H-pyrazole (L2) and 3-[(3-acetyl-1-phenyl-1H-4-pyrazolyl)carbonyl]-1-phenyl-4-(4-flourobenzoyl)-1H-pyrazole (L3), Ni complexes (5 and 6) are prepared and comparable in vitro antimicrobial study is evaluated. In vitro cytotoxicity of the Ni(II) complex (2) is studied using MTT assay. The analysis of the cell test showed that (2) displayed quite small cytotoxic response at the higher concentration level which indeed would further enable us for more opportunities in therapeutic and biomedical challenges. Both of the capability as a potent in vitro antifungal agent and the cell test analysis show Ni(II) complex (2) as a promising material in the translation of observed in vitro biological phenomenon into clinical therapies settings.

Silver(I) complexes as precursors to produce silver nanowires: structure characterization, antimicrobial activity and cell viability.

In this contribution a simple method has been employed to synthesis silver nanowires by thermal decomposition of silver complexes. Nanowires are the product of possible chemical reduction of metallic silver residue that remains after the thermal degradation process. Silver(I) complexes of quinolone antibacterial drugs sparfloxacin [Ag(SPHX)2·NO3]·3H2O (1) and enrofloxacin [Ag(ENRX)2·NO3]·2H2O (2) have been prepared and structurally characterized. In the literature the carboxylate and the carbonyl oxygen atoms were the most predominant coordination sites used for quinolones. The resulted complexes presented the drugs as monodentate ligands; however sparfloxacin displayed different behaviour than enrofloxacin. Sparfloxacin coordinated through the nitrogen atom of the piperazine ring, while enrofloxacin coordinated through carboxylate oxygen. Antimicrobial and antifungal activities of the reported complexes are evaluated using a modified Kirby-Bauer disc diffusion and MIC methods. High significant antimicrobial activity is recorded especially against Escherichia coli and Aspergillus flavus. In vitro cytotoxicity of the complexes is measured using MTT assay. The analysis of the cell test showed that the selected complexes displayed no significant cytotoxic response which opens up opportunities for creating further advances in therapeutic challenges. The functional diversity of the prepared silver complexes as precursors of producing nanowires is a subject of high interest in the field of material science. The prepared complexes represent a unique capability when set in the context of biomaterials for therapeutic actions and material engineering. This work provides insight into the mutual amenability of the prepared complexes which can be used to influence both cell-biomaterials interactions and in technical research community.

Synthesis, characterization and application of enrofloxacin complexes as thermal stabilizers for rigid poly(vinyl chloride).

Synthesis and characterization of both binary Co(II)- (1), Ni(II)- (2) complexes with enrofloxacin drug (HL(1)) and ternary Co(II)- (3), Ni(II)- (4) complexes in presence of DL-alanine (H(2)L(2)) are reported using physico-chemical techniques. The antimicrobial activity of these complexes has been screened against two gram-positive and two gram-negative bacteria. Antifungal activity against two different fungi has been evaluated and compared with reference drug. All the binary and ternary complexes showed remarkable potential antimicrobial activity higher than the recommended standard agents. Ni(II)-complexes exhibited higher potency as compared to the parent drug against bacterial and fungal strain. In addition, it was of interest to investigate the reported complexes as thermal stabilizers and co-stabilizers for rigid PVC in air at 180 °C. Their high stabilizing efficiency is detected by their high induction period values (T(s)) compared with some of the common reference stabilizers used industrially, such as dibasic lead carbonate (DBLC) and calcium-zinc soap. Blending these complexes with some of the reference stabilizers in different ratios had a synergistic effect on both induction period as it gave better thermal stability and lower extent of discoloration. The stabilizing efficiency is attributed at least partially to the ability of the metal complex stabilizer to be incorporated in the polymeric chains, thus disrupting the chain degradation and replace the labile chlorine atoms on PVC chains by a relatively more s moiety of the inorganic stabilizer. Their amenability to use as a biomedical additives for PVC, has afforded them great potential for various medical applications.

SiO2@Fe2O3 core-shell nanoparticles for covalent immobilization and release of sparfloxacin drug.

Silica-coated Fe(2)O(3) nanoparticles were synthesized as carriers for the covalent immobilization and release of antimicrobial drug sparfloxacin (SPFX). SPFX-loaded nanoparticles exhibited time-dependent drug release, with no measurable in vitro cytotoxicity, making the drug@nanoparticle conjugates potentially relevant for nanomedicine applications.

Synthesis, structural characterization and antimicrobial activity evaluation of metal complexes of sparfloxacin.

The synthesis and characterization of binary Cu(II)- (1), Co(II)- (2), Ni(II)- (3), Mn(II)- (4), Cr(III)- (5), Fe(III)- (6), La(III)- (7), UO(2)(VI)- (8) complexes with sparfloxacin (HL(1)) and ternary Cu(II)- (9), Co(II)- (10), Ni(II)- (11), Mn(II)- (12), Cr(III)- (13), Fe(III)- (14), La(III)- (15), UO(2)(VI)- (16) complexes with sparfloxacin (HL(1)) and DL-alanine (H(2)L(2)) complexes are reported using elemental analysis, molar conductance, magnetic susceptibility, IR, UV-Vis, thermal analysis and (1)H-NMR spectral studies. The molar conductance measurements of all the complexes in DMF solution correspond to non-electrolytic nature. All complexes were of the high-spin type and found to have six-coordinate octahedral geometry except the Cu(II) complexes which were four coordinate, square planar and U- and La-atoms in the uranyl and lanthanide have a pentagonal bipyramidal coordination sphere. The antimicrobial activity of these complexes has been screened against two gram-positive and two gram-negative bacteria. Antifungal activity against two different fungi has been evaluated and compared with reference drug sparfloxacin. All the binary and ternary complexes showed remarkable potential antimicrobial activity higher than the recommended standard agents. Ni(II)- and Mn(II) complexes exhibited higher potency as compared to the parent drug against gram-negative bacteria.

Uranyl binary and ternary chelates of tenoxicam Synthesis, spectroscopic and thermal characterization of ternary chelates of tenoxicam and alanine with transition metals.

Ternary Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and UO(2)(II) chelates with tenoxicam (Ten) drug (H(2)L(1)) and dl-alanine (Ala) (HL(2)) and also the binary UO(2)(II) chelate with Ten were studied. The structures of the chelates were elucidated using elemental, molar conductance, magnetic moment, IR, diffused reflectance and thermal analyses. UO(2)(II) binary chelate was isolated in 1:2 ratio with the formula [UO(2)(H(2)L)(2)](NO(3))(2). The ternary chelates were isolated in 1:1:1 (M:H(2)L(1):L(2)) ratios and have the general formulae [M(H(2)L(1))(L(2))(Cl)(n)(H(2)O)(m)].yH(2)O (M=Fe(III) (n=2, m=0, y=2), Co(II) (n=1, m=1, y=2) and Ni(II) (n=1, m=1, y=3)); [M(H(2)L(1))(L(2))](X)(z).yH(2)O (M=Cu(II) (X=AcO, z=1, y=0), Zn(II) (X=AcO, z=1, y=3) and UO(2)(II) (X=NO(3), z=1, y=2)). IR spectra reveal that Ten behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine-N and carbonyl-O groups, while Ala behaves as a uninegatively bidentate ligand coordinated to the metal ions via the deprotonated carboxylate-O and amino-N. The magnetic and reflectance spectral data confirm that all the chelates have octahedral geometry except Cu(II) and Zn(II) chelates have tetrahedral structures. Thermal decomposition of the chelates was discussed in relation to structure and different thermodynamic parameters of the decomposition stages were evaluated.

The tautomeric forms of cyameluric acid derivatives.

The tautomerism of cyameluric acid C6N7O3H3 (1 a), cyamelurates and other heptazine derivatives has recently been studied by several theoretical investigations. In this experimental study we prepared stannyl and silyl derivatives of cyameluric acid (1 a): C6N7O3[Sn(C4H9)3]3 (3 a), C6N7O3[Sn(C2H5)3]3 (3 b), and C6N7O3[Si(CH3)3]3 (4). In order to investigate the structure of 1 a the mono- and dipotassium cyamelurate hydrates K(C6N7O3H2)2 H2O (5) and K2(C6N7O3H)1 H2O (6) were synthesized by UV/Vis-controlled titration of a potassium cyamelurate solution with aqueous hydrochloric acid. Compounds 3-6 were characterized by FTIR and solid-state NMR spectroscopy as well as simultaneous thermal analysis (TGA, DTA). The single crystal X-ray structures of the salts 5 and 6 show that the hydrogen atoms in both anions are localized on the peripheral nitrogen atoms. This indicates-in combination with the solid-state NMR studies-that the most stable tautomer of solid 1 a is the triketo form with C3h symmetry. However, derivatives of both the hydroxyl and the amido tautomers may be formed depending on the substituent atoms: The spectroscopic data and single crystal structures of compounds C6N7O3[Si(CH3)3]3 (4) and the solvate C6N7O3[Sn(C2H5)3]3C2H4Cl2 (3 b') show that the former is derived from the symmetric trihydroxy form of 1 a, while 3 b' crystallizes as a chain-like polymer, which contains the tin atoms as multifunctional building blocks, that is, bridging pentacoordinated Et3SnO2 and Et3SnON units as well as non-bridging four-coordinated Et3SnN units. The cyameluric nucleus is part of the polymeric chains of C6N7O3[Sn(C2H5)3]3C2H4Cl2 (3 b'), by the action of both tautomeric forms of cyameluric acid, the amide and the ester form.

s-Triazine and tri-s-triazine based organic-inorganic hybrid gels prepared from chlorosilanes by exchange reactions.

Hybrid polymers [(DeltaO3)4Si3]n and [(DeltaO3)SiMe]n (where Delta = C6N7 or C3N3) have been prepared by a novel sol-gel process based on exchange reactions of MeSiCl3 or SiCl4 with C6N7(OSiMe3)3 and C3N3(OSiMe3)3.

Synthesis and thermal characterization of new ternary chelates of piroxicam and tenoxicam with glycine and DL-phenylalanine and some transition metals.

The ternary chelates of piroxicam (Pir) and tenoxicam (Ten) with Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) in the presence of various amino acids such as glycine (Gly) or dl-phenylalanine (PhA) were prepared and characterized with different physicochemical methods. IR spectra confirm that Pir and Ten behave as a neutral bidentate ligand coordinated to the metal ions via the pyridine-N and carbonyl group of the amide moiety. Gly molecule acted as a uninegatively monodentate ligand and coordinate to the metal ions through its deprotonated carboxylic group. In addition, PhA acted as a uninegatively bidentate ligand and coordinate to the metal ions through its deprotonated carboxylic and amino groups. The solid reflectance spectra and magnetic moment measurements confirm that all the chelates have octahedral geometrical structures while Cu(II)- and Zn(II)-ternary chelates with PhA have square planar geometrical structures. Thermal behaviour of the complexes is extensively studied using TG and DTA techniques. TG results show that water molecules (hydrated and coordinated) and anions are removed in the first and second steps while Gly, PhA, Pir and Ten are decomposed in the next and subsequent steps. The pyrolyses of the chelates into different gases are observed in the DTA curves as exo- or endothermic peaks. Also, phase transition states are observed in some chelates. Different thermodynamic parameters are calculated using Coats-Redfern method and the results are interpreted.

Structural, spectroscopic and thermal characterization of 2-tert-butylaminomethylpyridine-6-carboxylic acid methylester and its Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and UO(2)(II) complexes.

Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and UO(2)(II) complexes with the ligand 2-tert-butylaminomethylpyridine-6-carboxylic acid methylester (HL(2)) have been prepared and characterized by elemental analyses, molar conductance, magnetic moment, thermal analysis and spectral data. 1:1 M:HL(2) complexes, with the general formula [M(HL(2))X(2)].nH(2)O (where M = Co(II) (X = Cl, n = 0), Ni(II) (X = Cl, n = 3), Cu(II) (grey colour, X = AcO, n = 1), Cu(II) (yellow colour, X = Cl, n = 0) and Zn(II) (X = Br, n = 0). In addition, the Fe(III) and UO(2)(II) complexes of the type 1:2 M:HL(2) and with the formulae [Fe(L(2))(2)]Cl and [UO(2)(HL(2))(2)](NO(3))(2) are prepared. From the IR data, it is seen that HL(2) ligand behaves as a terdentate ligand coordinated to the metal ions via the pyridyl N, carboxylate O and protonated NH group; except the Fe(III) complex, it coordinates via the deprotonated NH group. This is supported by the molar conductance data, which show that all the complexes are non-electrolytes, while the Fe(III) and UO(2)(II) complexes are 1:1 electrolytes. IR and H1-NMR spectral studies suggest a similar behaviour of the Zn(II) complex in solid and solution states. From the solid reflectance spectral data and magnetic moment measurements, the complexes have a trigonal bipyramidal (Co(II), Ni(II), Cu(II) and Zn(II) complexes) and octahedral (Fe(III), UO(2)(II) complexes) geometrical structures. The thermal behaviour of the complexes is studied and the different dynamic parameters are calculated applying Coats-Redfern equation.

Synthesis, investigation and spectroscopic characterization of piroxicam ternary complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with glycine and DL-phenylalanine.

The ternary piroxicam (Pir; 4-hydroxy-2-methyl-N-(2-pyridyl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide) complexes of Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with various amino acids (AA) such as glycine (Gly) or DL-phenylalanine (PhA) were prepared and characterized by elemental analyses, molar conductance, IR, UV-Vis, magnetic moment, diffuse reflectance and X-ray powder diffraction. The UV-Vis spectra of Pir and the effect of metal chelation on the different interligand transitions are discussed in detailed manner. IR and UV-Vis spectra confirm that Pir behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine-N and carbonyl group of the amide moiety. Gly molecule acted as a uninegatively monodentate ligand and coordinate to the metal ions through its carboxylic group, in addition PhA acted as a uninegatively bidentate ligand and coordinate to the metal ions through its carboxylic and amino groups. All the chelates have octahedral geometrical structures while Cu(II)- and Zn(II)-ternary chelates with PhA have square planar geometrical structures. The molar conductance data reveal that most of these chelates are non electrolytes, while Fe(III)-Pir-Gly, Co(II)-, Ni(II)-, Cu(II)- and Zn(II)-Pir-PhA chelates were 1:1 electrolytes. X-ray powder diffraction is used as a new tool to estimate the crystallinity of chelates as well as to elucidate their geometrical structures.

Structure investigation, spectral, thermal, X-ray and mass characterization of piroxicam and its metal complexes.

[M(H2L)2](A)2.yH2O (where H2L: neutral piroxicam (Pir), A: Cl- in case of Ni(II) or acetate anion in case of Cu(II) and Zn(II) ions and y=0-2.5) and [M(H2L)3](A)z.yH2O (A: SO4(2-) in case of Fe(II) ion (z=1) or Cl(-) in case of Fe(III) (z=3) and Co(II) ions (z=2) and y=1-4) chelates are prepared and characterized using elemental analyses, IR, magnetic and electronic reflectance measurements, mass spectra and thermal analyses. IR spectra reveal that Pir behaves a neutral bidentate ligand coordinated to the metal ions through the pyridyl-N and carbonyl-O of the amide moiety. The reflectance and magnetic moment measurements reveal that these chelates have tetrahedral, square planar and octahedral geometrical structures. Mass spectra and thermal analyses are also used to confirm the proposed formulae and the possible fragments resulted from fragmentation of Pir and its chelates. The thermal behaviour of the chelates (TGA and DTA) are discussed in detail and the thermal stability of the anhydrous chelates follow the order Ni(II) congruent with Cu(II) Fe(II)

Thermal and kinetic studies on solid complexes of 2-(2-benzimidazolylazo)-4-acetamidophenol with some transition metals.

The preparation and characterization of 2-(2-benzimidazolylazo)-4-acetamidophenol (BIAAP) complexes are reported. Different physico-chemical methods like IR, Magnetic, solid reflectance spectra and molar conductance, were used to investigate the structure of BIAAP complexes. In particular, the thermal decomposition of Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes of BIAAP is studied in nitrogen atmosphere. All the complexes do not contain coordinated water molecules but contain (2-4) water molecules of crystallization. The water molecules were removed in a single step. The complexes of Co(II) and Ni(II) ions exhibited a phase transition and the decomposition or combustion of BIAAP occurred in the second and subsequent steps. The final decomposition products were identified by mass spectrometry as the corresponding metal oxides or carbonate. The activation thermodynamic parameters, such as, energy of activation, enthalpy, entropy and free energy change of the complexes were evaluated and the stabilities of the thermal decomposition of the complexes are discussed. From the kinetic point of view, it is found that the thermal stability of the complexes follows the order Ni(II) > Cu(II) > Zn(II) > Fe(III) > Co(II) > Cd(II).