Chelon approach to analysis (II). Illustrative experiments

Reilley, Charles N.; Schmid, R.; Sadek, F.

doi:10.1021/ed036p619

Cited by 107 publications

(19 citation statements)

References 4 publications

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“…The heating rate was maintained at 10 °C min -1 . The metal contents were estimated by complexometric titrations, 15 while the chlorine was determined gravimetrically as AgCl in case of Cr(III) and Fe(III) complexes. 16 …”

Section: Methodsmentioning

confidence: 99%

Template synthesis of symmetrical transition metal dithiocarbamates

Siddiqi¹,

Nami²,

Lutfullah³

et al. 2006

J. Braz. Chem. Soc.

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have chlorine bridged distorted-octahedral geometry. It has been observed that the dithiocarbamato moiety is symmetrically bonded in all the cases. A three stage TGA profile is observed for all the complexes leading to the formation of respective metal sulfide as the end-product. The molar conductance of 10 -3 mol L -1 solution of the complexes measured in DMSO is indicative of their non-ionic nature. Keywords: dithiocarbamates, transition metals, thermal analysis, symmetrical bonding IntroductionDithiocarbamates are used to stabilize a wide range of oxidation states of different metal ions. 1 A large number of compounds are known where CS 2 binds in η 1 -end on, η 2 -side or in η 3 -coordination modes. 2-4 The major advantage of using the small bite-angle of dithiocarbamato moiety as a stabilizing chelating ligand, is its unique property to remain intact under a variety of reaction conditions. 5 Nowadays copper(II) dithiocarbamate is successfully used as single source precursor for the growth of semiconducting copper sulfide thin films. 6 The iron(II), iron(III) dithiocarbamates have been studied for their spincrossover phenomenon, 7 radical traps for NO, 8 and as antioxidants and pro-oxidants in biological systems. 9 Diethyl dithiocarbamates are also known to inhibit the activity of Cu/Zn-superoxidedismutase (SOD) through the withdrawal of copper from the protein both in vivo and in vitro. 10 Some dialkyl-substituted dithiocarbamates have proved to be an efficient anti-alkylating, anti-HIV and froth-floatation agents. 11 The optical and electrochemical properties of dithiocarbamates can effectively be used to construct sensors for guest molecules and macromolecules. [12][13][14] In this paper, we report a convenient one-pot synthesis of the transition metal dithiocarbamates via template procedure. In the present work, a condensation reaction was carried out between acetylacetone, ethylenediamine, 108 Siddiqi et al. J. Braz. Chem. Soc. carbon disulfide in a single step leading to the formation of a ring like complex ( Figure 1 and Figure 2). ExperimentalHydrated metal chlorides (BDH) acetylacetone, carbon disulfide (Merck) and ethylenediamine (Ranbaxy) were used as received. Methanol was used after distillation. Elemental analyses (C, H, N and S) were carried out with a Flash EA-1112 Analyser, CE Instrument. IR spectra (4000-400 cm -1 ) were recorded on a FT-IR Perkin-Elmer Spectrum BX as KBr disc while the 600-200 cm -1 range were scanned on CsI on Nexus FT-IR Thermo Nicolet, Madison Wisconsin. The conductivity measurements were carried out with a CM-82T Elico conductivity bridge in DMSO. The electronic spectra were recorded on a Cintra 5GBC spectrophotometer in DMSO. Magnetic susceptibility measurements were done with a Sherwood Scientific MSB Auto at room temperature. TGA/DSC was performed with a Universal V3.8 B TA SDT Q600 Build 51 Thermal Analyzer under nitrogen atmosphere using alumina powder as reference material. The heating rate was maintained at 10 °C min -1 . The metal contents were estimated by...

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Section: Methodsmentioning

confidence: 99%

Template synthesis of symmetrical transition metal dithiocarbamates

Siddiqi¹,

Nami²,

Lutfullah³

et al. 2006

J. Braz. Chem. Soc.

View full text Add to dashboard Cite

show abstract

“…Elemental analysis (C, H, N) were performed using a VarioEL elementar analysensysteme. Metals and chlorides were determined volumetrically 11 and gravimetrically 12 . IR spectra were recorded using KBr discs (4000-400 cm -1 ) on a Shimadzu 8300 IR spectrophotometer.…”

Section: Methodsmentioning

confidence: 99%

Synthesis, Characterization and Antimicrobial Studies of Novel Binuclear Transition Metal Complexes of Schiff Base Derived from 1-Amino-5-methyl-2,6-pyrimidine-dione and 2,3-Butanedione

Singh¹,

Srivastava²

2013

Asian J. Chem.

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CH3COO-and L = ligand) of a Schiff base ligand derived from 1-amino-5-methyl-2,6-pyrimidine-dione and 2,3-butanedione have been synthesized and characterized by elemental analysis, molar conductance measurements, magnetic moment measurements, IR, UV-visible, 1 H NMR, EPR and mass spectral studies. Electronic spectral data and magnetic moment values indicate octahedral geometry for all the metal complexes. In vitro antimicrobial activity of ligand and its metal complexes were also studied against bacteria (Bacillus subtilis and Escherichia coli) and fungi (Aspergillus niger and Aspergillus flavus) which show antimicrobial activity of ligand and binuclear metal complexes.

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“…The metal contents were estimated by complexometric titration. 40 The IR spectra (4000-400 cm -1 ) were recorded on a Perkin-Elmer model 377 spectrometer using KBr disks. The conductivity measurements were carried out on a CM-82T Elico conductivity bridge in DMSO.…”

Section: Physical and Spectral Measurementsmentioning

confidence: 99%

Synthesis and Characterization of Two Novel Complexes of Cr(III) with Benzilmonoxime

Soleimani

2011

J Chinese Chemical Soc

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The reaction of benzilmonoxime (BMOH) with CrCl 3 .6H 2 O in methanol gives the mono nuclear Cr(III) complex, [Cr(BMO) 3 ] (1). Reaction of complex 1 with a methanolic solution of KOH at room temperature leads to a di-nuclear Cr(III)-Cr(III) complex, [Cr(BMO) 2 (OH)] 2 (2). The complexes were characterized on the basis of their elemental analysis, Mass, IR, 1 H and 13 C-NMR and electronic spectra. The IR studies were useful in assigning the coordination mode of the benzilmonoxime ligand to the chromium(III) ion. In addition, the presence of a hydroxo bridge in the dimeric complex 2 is inferred from the IR spectral studies. The electronic spectra of the complexes revealed two bands due to d-d transitions, and one band assignable to an oxygen (p p )®Cr(eg * ) LMCT transition observed in both complexes. An additional charge transfer transition, assignable to m-OH(p p )®Cr(eg * ), was only observed for the dimeric complex 2.The splitting energy and Racah parameter were calculated to be 18484 cm -1 and 560 cm -1 for [Cr(BMO) 3 ] (1), 17986 cm -1 and 545 cm -1 for [Cr(BMO) 2 (OH)] 2 (2) respectively.

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Chelon approach to analysis (II). Illustrative experiments

Abstract: This paper describes chelon titration methods and various ways of achieving selectivity, lists some hints and precautions for practical work, and provides 15 experimental procedures for applying these techniques.

Cited by 107 publications

References 4 publications

Template synthesis of symmetrical transition metal dithiocarbamates

Template synthesis of symmetrical transition metal dithiocarbamates

Synthesis, Characterization and Antimicrobial Studies of Novel Binuclear Transition Metal Complexes of Schiff Base Derived from 1-Amino-5-methyl-2,6-pyrimidine-dione and 2,3-Butanedione

Synthesis and Characterization of Two Novel Complexes of Cr(III) with Benzilmonoxime

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