Journal of Chemical and Pharmaceutical Research

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1 vailable online Journal o Chemical and Pharmaceutical Research ISSN No: CODEN(US): JCPRC5 J. Chem. Pharm. Res., 2011, 3(6): Spectrophotometric study on stability constants o copper(ii) complex with 1-amidino-O-methylurea L. Jadumani Singh and k. Manihar Singh * Department o Chemistry, Manipur University, Canchipur, Manipur, India BSTRCT The stoichiometries and stability constants o copper(ii) ions with 1-amidino-O-methylurea have been determined in aqueous solution at dierent temperatures 20 0 C, 25 0 C, 30 0 C, 35 0 C and 40 0 C with constant ionic strength o 0.5 M KNO 3 by using Job s continuous variation method spectrophotometrically. In all cases, the Job s curves displayed a maximum at a mole raction X metal =0.5 indicating the ormation o complex with 1:1 metal to ligand ratio. It was observed that metal-ligand stability constant decreases with increasing temperature indicating exothermic nature o the reaction. Plots o thermodynamic stability constants versus 1/T gave linear curves indicating high temperature sensitivity or the -NH group o the ligand. The thermodynamic parameters i.e., G 0, H 0 and S 0 have also been calculated. Keywords: Stability constant, spectrophotometrically, 1-amidino-O-methylurea, thermodynamic parameters, copper(ii). INTRODUCTION Copper is one o the several metal ions that play an important role in biological system. It has a vital role during cell respiration, in the blood o invertebrate animals and in the ormation o haemocyanin [1]. part rom the biological utility o the copper, it also inds applications in industries as ine wires, commuter bars and high conductivity tubes [2]. Metal ions play an important role in all living systems and any malunctioning o these ions can initiate a number o physiological abnormalities and symptoms o clinical disorders (Wattoo, 2001). Transition metal ions are responsible or proper unctioning o dierent enzymes. Researchers have become increasingly interested in the coordination chemistry o copper complexes as models or the active sites in copper-containing enzymes. This is largely due to the discovery o copper at the centers o many important enzymes [3]. 1022

2 k. Manihar Singh J. Chem. Pharm. Res., 2011, 3(6): Copper is essential or lie but is highly toxic above certain limits to organisms like certain algae, ungi and many bacteria or viruses [4,5]. In addition, the accumulation o copper in the human liver is a characteristic o Wilson s disease which produces neurological and psychiatric deects [6]. Stable complexes o trivalent and bivalent transition metal ions are ound to orm with 1- amidino-o-methylurea [7-10]. The ligand 1-amidino-O-methylurea (MUH) serves as a bidentate ligand satisying both the primary and secondary valencies with the ormation o inner metallic complexes. In view o the signiicant importance o biguanide, MUH, we report here, the stability constants o copper(ii) complex with MUH in the ionic strength o 0.5 M KNO 3 at varying temperatures o 20 0 C, 25 0 C, 30 0 C, 35 0 C and 40 0 C respectively by using Job s method (continuous variation method) spectrophotometrically along with their thermodynamic parameters. EXPERIMENTL SECTION Synthesis o ligand The ligand 1-amidino-O-methylurea was prepared by published method [11]. The compound was characterized through elemental analysis (Found: C, 23.81; H, 5.98; N, 36.86; Cl, 23.61; calculated or C 3 H 8 N 4 O.HCl: C, 23.61; H, 5.9; N, 36.72; Cl, 23.27); melting point at C; literature C. Structure o ligand 1-amidino-O-methylurea (MUH) Double distilled water was used in the preparation o desired concentrations o ligand solutions. The metal ion solution o desired concentration was prepared rom the standardized stock solution o CuSO 4.5H 2 O. NaOH, HNO 3 and KNO 3 solutions were prepared in CO 2 ree double distilled water [12]. By using the usual methods, NaOH and HNO 3 solutions were standardized. ll the ph measurements were perormed on a Digital systronic µ ph system 362. In all the cases, the ph-meter was calibrated at two ph values i.e., 4.0 and 9.2 ± 0.05 using (BDH) buer tablets. ll the measurements were carried out at dierent temperatures by using a thermostat, Haake (Model DC 10) enclosed with the spectrophotometer Shimadzu UV-2450 along with 1 cm quartz cells with an accuracy o ± C and at the ionic strength o 0.5 M KNO 3. Copper(II) sulphate standard solution o M was pippetted into eleven 25 ml volumetric lasks (0, 1, 2, 3,, 9, 10 ml) and an aliquot o M MUH (10, 9, 8, 7,, 1, 0 ml) was added keeping both the number o moles o metal and ligand constant but varying either mole ractions o metal or ligand. Ionic strengths were maintained by adding appropriate quantity o 1.25 M KNO 3. λ max was determined using one o the composition at which there is maximum absorption. The absorption or all the compositions was recorded at a constant wavelength (λ max ) [13]. The data o absorption and percentage composition o metal ion and ligand solution at constant ph can be used and curves were constructed. With the help o variable volume ccupipet, Model T200 (20 µl to 200 µl), ph values were adjusted with M HNO 3 and M NaOH solutions ranging rom 0.02 ml to 0.25 ml. The above reaction mixtures were separately measured with their absorbance values. 1023

3 k. Manihar Singh J. Chem. Pharm. Res., 2011, 3(6): RESULTS ND DISCUSSION The spectral curves o the reaction mixtures o copper(ii) with 1-amidino-O-methylurea in the ionic strength o 0.5 M KNO 3 at ive dierent temperatures are shown (Fig.1). The measurements were carried out at 261 nm and ph = 4.6 (Table 1). On plotting measured absorbance against mole ractions o the two constituents o the complex gives a characteristic triangular plot indicating ormation o a more stable complex [14]. The composition o the complex was calculated rom the point o intersection o the tangents to the curve [15] and was ound to be 1:1, metal to ligand ratio at the mole raction X metal =0.5 (Fig.1). Reaction o copper(ii) with 1-amidino-O-methylurea at ive dierent temperatures in the ionic strength o 0.5 M KNO 3 at 261 nm are shown in Table 1. It was observed that the stoichiometric ratio o copper(ii) to 1-amidino-O-methylurea in the complex is 1:1. Table 1: Experimental Data o Copper(II)-1-amidino-O-methylurea by Continuous Variation Method Sl. Metal Conc. Ligand Conc. bsorbance at 261 nm No. ( 10-4 M) ( 10-4 X M) Cu 20 0 C 25 0 C 30 0 C 35 0 C 40 0 C The stability constants o the complexes were calculated rom the ollowing relation [16]. [ ML ] K = [ M ][ L ] 1 K = [1 2 1 [ 2 ] [ C L 1 ] C M 2 1 ].2 Here, 1 = absorbance at break point, 2 = actual absorbance, C M = concentration o metal and C L = concentration o ligand. 1024

4 k. Manihar Singh J. Chem. Pharm. Res., 2011, 3(6): Fig.1. Job s curves o equimolar solutions o Copper(II)-1-amidino-O-methylurea at () 20 0 C; (B) 25 0 C; (C) 30 0 C; (D) 35 0 C and (E) 40 0 C at 261 nm and ph = 4.6. In all Figures, the mole raction o the metal ion is represented by abscissa. Very close values o 1 and 2 in Fig.1 is due to the ormation o more stable copper(ii) complex with MUH [14]. Table 2 shows log k values o copper(ii) with 1-amidino-O-methylurea at ph 4.6 with dierent temperatures along with their thermodynamic parameters. Exothermic nature o the reactions [Fig.2, 3] was also observed rom the value o stability constant at dierent temperatures as the value o stability constant decreases with the rise in temperature. Table 2: Stability constant and Thermodynamic parameters Sl. No. Metal ion Ligand ph 1 Cu(II) 1-amidino-Omethylurea 4.6 Temp. log k (K) G 0 (kjmol -1 ) H 0 (kjmol -1 ) S 0 (kjk -1 mol -1 )

5 k. Manihar Singh J. Chem. Pharm. Res., 2011, 3(6): The values o overall change in ree energy ( G 0 ), enthalpy ( H 0 ) and entropy ( S 0 ) accompanying complexation reaction have been determined using temperature coeicient and Gibbs-Helmholtz equation. Fig.3 represents the plot o log k vs 1/T or Cu(II)-MUH complex. From the curve the values o G 0, H 0 and S 0 are evaluated and are given in Table 2. The negative values o G 0 relect spontaneity o the reaction [17]. The change in enthalpy ( H 0 ) being negative, the reaction occurred is exothermic and ormation o complex is avourable. Negative value o enthalpy change also suggests that the metal-ligand bonds are airly strong [18]. Since the value o S 0 is positive the reaction will tend to proceed spontaneously [19]. Positive entropy changes accompanying a given reaction are due to the release o bound water molecules rom the metal chelates [18]. During ormation o metal chelates, water molecules rom the primary hydration sphere o the metal ion are displaced by the chelating ligand. Thus there is an increase in the number o particles in the system i.e., randomness o the system increases as shown in the ollowing equation. M +2 (aq) + L -2 (aq) === ML (aq) + nh 2 O Williams [20] has pointed out that usually a high entropy value was associated when positively charged cations and negatively charged ligands combined involving the displacement o water molecules, which then become a part o the solvent. Since the water molecules bound to the metal ions are highly distorted and oriented, the entropy is low. The value o correlation coeicient (r) shows almost perect positive correlation between log and 1/T which indicates a reproducible one. Standard deviation value o and relative k standard deviation value o 1.421% or Cu(II)-MUH complex show within the reproducible limit [21]. The plot o log k vs. 1/T yields distinct straight lines (Fig.3) which relects the high temperature sensitivity or the -NH group o the ligand [22]. CONCLUSION The value o log k or Cu(II)-MUH complex at (25 ± 0.1) 0 C in the ionic strength o 0.5 M KNO 3 was ound to be spectrophotometrically. Exothermic nature o the reactions was 1026

6 k. Manihar Singh J. Chem. Pharm. Res., 2011, 3(6): observed rom the value o stability constant. The composition o the complex was 1:1 metal to ligand ratio. REFERENCES [1]. T.Z. Judith, T. Peter and T. Thomas, Immunotoxicology o Environment Occupational Metals, School o Environment Occupational Metals, School o Medicine, New York, [2]. B.K. Sharma, Environmental Chemistry, Goel Publishing House, 1997, Meerut, India. [3]. Syed hmad Tirmizi, Feroza Hamid Wattoo, Muhammad Hamid Sarwar Wattoo Saadia Sarwar, llah Nawz Memon and llah Bux Ghangro, rabian Journal o Chemistry, doi: /j. arabje [4]. U. Borgmann and K. M. Ralph, Complexation and toxicity o copper and the ree metal bioassay technique, Water Research, 1983, 17, [5]. Y. M. Nor, Ecotoxicity o copper to aquatic biota: review, Environmental Research, 1987, 43, [6]. G. J. Brewer and V. Y. Gurkan, Wilson s disease, Medicine, 1992, 71, [7]. R.L. Dutta and P. Ray. J. Indian Chem. Soc., 1959, 36(7), 449. [8]. R.L. Dutta, Bimanesh Sur and N.R. Sengupta, J. Indian Chem. Soc., 1960, 37(9), [9]. R.L. Dutta and. Syamal, Coord. Chem. Rev., 1967, 2, [10]. R.L. Dutta and k. Manihar Singh, J. Indian Chem. Soc., 1975, 52, [11]. R.L. Dutta and P. Ray, J. Indian Chem. Soc., 1959, 36, [12]..I. Vogel, Quantitative Inorganic nalysis, Longmans, Green and Co. Ltd., London, 3 rd Edn., 1962, [13] U. P. Meshram, B. G. Khobragade, M. L. Narwade and. R. Yaul, J. Chem. Pharm. Res., 2011, 3(3), [14]. Juan M. Bosque-Sendra, Eva lmansa-lopez, na M, Garcia-Compana and Luis Cuadros- Rodriguez, nal. Sci., 2003, 19, [15]. P.V. Chalapathi1, Y. Subba Rao, M. Jagadeesh, B. Prathima,. Sreenath Reddy, K. Janardhan Reddy and.varadareddy, J. Chem. Pharm. Res., 2011, 3(3), [16]. Syed hmad. Tirmizi, Muhammad Hamid Sarwar. Wattoo, Sarwar Saadia and Waheed. nwar, The rabian Journal or Science and Engineering, 2009, 34 (2), 46. [17]. Ramandeep Kaur and B.S. Sekhon, J. Indian Chem. Soc., 2006, 83, 645. [18]. K. Kiranmai, Y.Prashanthi, Vijay Kumar Chityala and Shivaraj, J. Chem. Pharm. Res., 2011, 3(5), [19]. Gordon M. Barrow, Physical Chemistry, 5 th Edn., Tata McGraw-Hill Publishing Co. Ltd., New Delhi, 1992, 191. [20]. R. S. P. Williams, J. Phys. Chem. 1954, 58, 12. [21] D. Nagarjuna Reddy, K. Vasudeva Reddy and K. Hussain Reddy, J. Chem. Pharm. Res., 2011, 3(3), [22]. M. bdelbary, H.. Shehata, M..F. Ez Ei-rab,.. Mohammad and M.M. Emara, J. Indian Chem. Soc., 1996, 73,

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