6 December 2015 Volume 6 SI.No 1 A Facile Spectrophotometric Determination of Osmium(VIII) in very low 1 - 6 concentrations using DL-Pencillamine as Chromogenic Reagent Bincy Joseph and Abraham Joseph 2 Evaluation of insecticidal and larvicidal activity and the detection of lipase 7 - 14 from Eupatorium odoratum leaf extracts. Soniya P.A., Navia Sebastian and Dr. Deepa G Muricken 3 Biosynthesis of Gold Nanoparticles using Bacteria and Fungi 15 - 21 Nivea Wilson, Nileena PV, Dhanya KC 4 Comparative Study on Antibacterial profiles of Kanakasava 22 - 25 Elizabeth P Thomas, Uma V Menon P, Afeeda Beegum M K, Athira MR, Darsana NC, and KS Dhaneesha Sivadas 5 Antibacterial effect of citrus fruit juice against enteric and non enteric 26 - 33 pathogenic bacteria Geenat Paul , Rigi George A , Rahima N A 6 Hydrogen Peroxide Scavenging Ability of Scoparia Dulci&Piper Longum Linn 34 - 40 ABAS Geetha T December 2015 7 Effect of plant growth promoting Proteus spp.on fenugreek 41 - 49 Vol. 6, No.1 Jimtha John C, Mrudula M M, Anisha C, and Radhakrishnan EK 8 A study on the antibiotic sensitivity test of selected isolates from facial 50 - 60 microflora and their susceptibility to commercial face washes Femina K K, Finciya A T, Hanna T V, Jasira V, Jini Joy P & Mabel Merlen Jacob 9 Bioactive peptides derived from milk: a review 61 - 65 Reshma Chandran P 5 1 0 2 Annals of Basic and Applied Sciences December 2015, Volume 6, Number 1, (ISSN 2277-8756). (Official publication of St Mary's College, Trichur - 680020, Kerala, India) Editor Dr Meera C R Department of Microbiology, St. Mary's College, Trichur - 680020 Kerala, India. Associate Editors Dr. Dhanya KC Dr. Mabel Merlen Jacob Department of Microbiology, Department of Microbiology, St. Mary's College, Trichur - 680020, St. Mary's College, Trichur - 680020, Kerala, India. Kerala, India. Editorial Board Dr. Regi Raphael K Dr. Kezia Kuruvila Dr. Sheeja T Tharakan Dr. Manju Madhavan Department of Botany, Department of Zoology, Department of Botany, Department of Botany, St. Mary's College, Vimala College, Vimala College, Vimala College, Trichur-680020, Trichur-680009, Trichur - 680009, Trichur - 680020 Kerala, India. Kerala, India. Kerala, India. Kerala, India. Dr Geetha T Dr. Manju Sebastian Dr. Rekha K Department of Chemistry, Department of Department of Botany, St. Mary's College, Chemistry, St. Mary's College, Trichur - 680020, St.Mary's College, Trichur - 20 Kerala, India. Trichur - 680020, Kerala, India. Kerala, India. Scientific Advisory Board Dr. Sr Jacintha C C Dr. K K Janardhanan Dr.C K K Nair Principal, Professor & Head, Director of Research, St. Mary's College, Department of Microbiology, St. Gregorios Dental Trichur - 680020, Amala Cancer Research Centre, College & Research Centre, Kerala, India. Trichur - 680555, Kerala, India. Kothamangalam – 686681, Kerala,India. Dr. S G PrapuIla Dr.Valsa A K Department of Fermentation, Department of Microbiology, Technology & Bioengineering, Sree Sankara College. Kalady, CFTRI. Mysore - 570020, Emakulam-683574, Karnataka, India. Kerala,India. Publishers St.Mary'sCollege,Trichur-680020.Kerala,India. A Facile Spectrophotometric Determination of Osmium(VIII) in very low concentrations using DL-Pencillamine as Chromogenic Reagent Bincy Joseph and Abraham Joseph* * Department of Chemistry ,University of Calicut, Calicut University Corresponding Author:Bincy Joseph,Dept.Of Chemistry,St.Mary’s College,Thrissur.Ph.No.9946355330 Email:[email protected]. ABSTRACT A simple spectrophotometric technique of high sensitivity and selectivity has been developed for the determination of trace amount of osmium(VIII) using DL- Pencillamine(DL- Pen) as a chromogenic reagent. The method is based on the formation of a pale pink complex at a fast pace at room temperature by the reaction of osmium(VIII) with DL-Pen in strongly acidic solution of pH 1 which absorb at 540 nm. The decrease of absorbance is directly proportional to osmium concentration and obeys the Beer’s law in the range of 0.15-1.50 µg/ml. The optimum reaction condition and 4 - other analytical requirements were evaluated. The molar absorptivity(5.05 x 10 LMol 1 -1 -3 cm ), Sandell's sensitivity(3.8 x 10 -2 -1 -1 µgcm ), detection limit(0.066 µgml ) and quantitation limit(0.20 µgml ) of the method were computed. Key words Osmium, Spectrophotometry, DL-Pencillamine , Chromogenic reagent. 1 Annals of Basic and Applied Sciences, Vol 6, No.1, Dec 2015 1.Introduction emission spectrometry, electron microprobe analysis, total reflection X- 6 2 Osmium(Z=76,5d 6s ) is a bluish ray fluorescence spectrometry, atomic white metal, the heaviest among the absorption spectrometry and neutron platinum metals, exhibits high specific activation analysis, the visible density(22.61g cm-3), high melting spectrophotometric methods seems to be 0 point(3050 C)and hardness(7.0Mhos the most appropriate analytical approach for the determination of toxic metals like scale) , occurs in ten different oxidation osmium, as it provides sensitive, precise states from Os(II) to Os(VIII). The and accurate measurements of suitable metal and its alloys are used for the analytes and offers practical and production of materials of extreme economical advantages over other hardness. methods. Most of these instruments are highly expensive and their day to day The volatile osmium tetroxide, maintenance cost is high and are also OsO is formed by the oxidation of 4, not free from various types of inherent osmium, is one of the most important interferences (Somasiri LLWet al., compounds of the element and is easily 1991,Honegger K .,et al 1987 Ramesh et al., identified by its characteristic unpleasant 1992).Besides,visible spectrophotometric odour. Osmium tetroxide is a powerful detection is much more viable as a toxic agent, harmful to eyes and useful technique to develop a portable respiratory tracts. So special precautions on-line or at line system. are needed in sample collection, storage and other procedures due to its strong Most of the existing well tendency of oxidation to volatile established spectrphotometric methods tetroxide and possible losses of the using the sulfur containing molecules element. The volatility of OsO4 makes and ligands like thiourea, thiocynate and the basis of separation of osmium from 1,5-diphenylcarbazide lack adequate its mixtures with other noble metals by sensitivity and selectivity and necessitate the separation of osmium by distillation. The reduction of OsO4 to extraction or distillation before the the black osmium dioxide, OsO2, by determination. biological substances made the basis of its use as a staining reagent for the Many organic reagents have been microscopic examination of tissues. proposed for spectrophotometric determination of osmium, including Compared to the various modern Perphenazine (Gowda et al., 1984) optical methods of analysis including inductively coupled plasma atomic In the flotation methods, the molar 2 Annals of Basic and Applied Sciences, Vol 6, No.1, Dec 2015 5 absorptivities are 2.2 x 10 at 655 nm ,2.0 containing ∼100 ml of water acidified 5 x 10 (with crystal violet and malachite with 3 ml of H2SO4 (1+1) wash, dry and green) (Balcerzak M. 1991) . Larger weigh the glass fragments of the amounts of osmium can be determined ampoule and calculate the weight of 2- 3 as osmate, OSO4 (ε = 2.75 x 10 at 340 OsO4 by difference. Dilute the osmium nm) (Ensafi et al 1991) .Other than direct solution with double distilled water till 1 spectrophotometric methods of ml contains precisely 1.5 mg of osmium. determination, certain reagents (Jamshid Perform all these operations in a fume et al 2000) are employed for the cupboard, and keep the osmium solution spectrophotometric determination of in a bottle with precision ground stopper osmium based on its catalytic activity. on account of the toxic properties and Derivative spectrophotometric methods offensive odour of the tetroxide( are also used for the determination of Marczenko Z 1986). osmium under different experimental conditions (Balcerzak M e t al., 1996, Pencillamine solution (1%): Balcerzak M et al.,1997, Kosiorek A et al., Dissolve 1g of reagent (HIMEDIA) in 2006) . 100 ml of double distilled water. Apparatus: The absorbance was In the present work, a reaction of measured and absorption spectra were Os(VIII) with DL-pencillamine have recorded using a systronics double beam been examined at various experimental uv-vis spectrophotometer 2201with conditions and the most suitable Quartz Cells (1cm). Digital pH meter analytical requirements have been (M.C. Dalal and Co. Madras) was used established for the quantitative for pH measurements. determination the element in pure Procedure:Aliquots of the stock solution aliquots and in the presence of various containing 0.15-1.5 µg of osmium(VIII) other metal ions. The proposed method were pipetted out into a series of 10 ml for the element offers many advantages standard flask and made up to the mark over the conventional using dil. H2SO4 (to maintain pH1). 3ml spectrophotometric methods. each of these solutions were taken and mixed with 0.1ml of 1% DL- 2.Experimental pencillamine solution and shaken well. A pink colour is developed in the Reagents and chemicals:Standard solution and measure the absorbance at osmium solution (1.5 mg/ml) : carefully 540 nm against the reagent blank. The broken an accurately weighed glass calibration graphs were constructed by ampoule containing ∼1 g of OsO4 (J.M. plotting the absorbance against the Chemicals Ltd., London)in a beaker amount of metal ions. 3 Annals of Basic and Applied Sciences, Vol 6, No.1, Dec 2015 3. Results and Discussion 0.75µg of osmium. It was noticed that an excess of the reagent does not have DL-pen reacts with osmium at any adverse effect on the sensitivity and room temperature to form a pink stability of the complex. coloured complex species having maximum absorbance at 540 nm. 3.3 Effect of time on absorbance Subsequent studies have been therefore carried out at this wavelength.