M.Sc Chemistry Inorganic Chemistry Practical Syllabus Semester : 1 A.

Qualitative Analysis of Inorganic Mixture - (21 Marks) Identification of seven radicals including insoluble residue and rare ea rth metal ions by semi micro analysis. (ii) Rare elements: Tl, W, Se, Mo, Ti, Zr, Ce, Th, V, U, Li (iii) Insolubles: PbSO4, SrSO4, Al2O3, Cr2O3, Fe2O3, SnO2, TiO2, ThO2, WO3.xH2O B. 1. 2. 3. 4. 5. 6. 7. Preparations of Inorganic Complex Compounds - (14 Marks) Prussian Blue (Potassium Ferric Ferro cyanide) Reineckes salt (Ammonium diammine tetra thio cyanato chromate (III)) Potassium tri oxalato ferrate (III) trihrdrate. trans-potassium di aqua bis(oxalato) chromate (III) cis-potassium di aqua bis(oxalato) chromate (III) Sodium hexa nitrito cobaltate (III) tris (acetylacetonato) manganese (III)

Semester : 2 A. Quantitative Analysis : Quantitative Separation and determination of two metal ions : Cu-Ni, Ni-Zn, Cu-Z n etc using volumetric and gravimetric methods. B. Chromatography :

1. Paper chromatographic separation of Pb, Ag and Hg ions . 2. Determination of the Rf value of Pb, Hg, Cu and Cd ions by using paper c hromatographic technique. 3. Determination of the Rf value of Fe, Al, Cr ions by using paper chromato graphic technique. 4. Determination of the Rf value of Ba, Sr, Ca ions by using paper chromato graphic technique. 5. TLC separation and determination of the Rf values of Ni, Mn, Co and Zn i ons. 6. Radial paper chromatographic seperation of Cu, Cd ions. 7. Radial paper chromatographic seperation of Ni, Cu ions. 17. Spectrophotometric determination (in ppm) of Fe (II) or Fe(III) using 1 ,10 Phenanthroline (or thiocyanate) as colorimetric reagent. 18. Colorimetric determination of chromium (VI) (in ppm) using 1,5 diphenyl carb azide as a reagent for colour development.

Object : To determine the dissociation constant , pKa, of an acid base indicator (methyl red) by spectrophotometric method. Object : (a) To carry out absorbance measurements for Chromium (VI) and Mangane se (VII) solutions on a spectrophotometer and draw its UV-VIS spectrum. (b)To determine the wavelength of maximum absoption (l max) of Chromium (VI) and Manganese (VII) and compute the corresponding molar absorption coefficient, (c) To calculate the concentrations of chromium and manganese in a mixture from the absorption measurements of the mixture at two different wavelengths.

Semester: 3 A. Colorimetry / Spectrophotometry

(a) Determination of the wavelength of maximum absoption . 1. To carry out absorbance measurements for Chromium (VI) and Manganese (VII) s olutions on a spectrophotometer and draw its UV-VIS spectrum and determine the wavelength of maximum absoption (l max) of Chromium (VI) and Manganese (VII) and compute the corresponding molar absorption coefficient. (b) Verification of Beer-Lambert law and Determination of Metal Ions (in ppm) in supplied solution. 1. Verification of the Beer-Lambert law and determination the concentration of s upplied KMnO4 solution. 2. To test the validity of the Beer-Lambert law and determine the concentration of supplied K2Cr2O4 solution. 3. To analyse the validity of Beer s law using colorimeter and determine the conce ntration of supplied CuSO4.5H2O 4. Determination of the concentration of supplied NiSO4.7H2O solution as Ni-dmg complex spectrophotometrically. (c) Determination of Metal Ions (in ppm) in unknown sample 1. Spectrophotometric Determination of Iron in Vitamin Tablets. 2. Spectrophotometric Determination of Manganese in Steel. (d) Spectrophotometric Titration 1.Determination of the concentration of the supplied FeCl3 solution by spectroph otometric titration with EDTA. 2. Determination of Copper by EDTA (e) Determination of composition of binary mixture. 1. To calculate the concentrations of Chromium (VI) and Manganese (VII) in a mix ture from the absorption measurements of the mixture at two different wavelength s. 2. To calculate the concentrations of Cobalt (II) and Chromium (III) in a mixtur e from the absorption measurements of the mixture at two different wavelengths. (f) Spectrophotometric determination of anions . 1.To determine the concentration of given unknown phosphate solution by Molybdo phosphoric acid Method with the help of spectrophotometer. 2.To determine the concentration of given unknown phosphate solution by Phospho vanadomolybdate method with the help of spectrophotometer. (g) Determination of Dissociation Constants of an Indicator. 1. To determine the dissociation constant , pKa, of an acid base indicator (methyl red) by spectrophotometric method. 2. To determine the dissociation constant , pKa, of an acid base indicator (Brom othymol Blue or Phenol Red) by spectrophotometric method. (h) Determination of Composition (formula) and Stability Constant of Complexs. 1. Fe(III) thiocynate complex by Job's method. 2. Fe(III) sulpho salicylic acid (SSA) complex by Job's method. 3. Copper-ethylene diamine complex by mole fraction or Slope ratio method. B. Flame photometry

1. Determination of Na concentration in the given solution flame photometri cally by calibration curve method 2. Using a flame photometer, determine K in the given solution 3. Determination of calcium concentration flame photometrically 4. Determination of total Na, K & Ca concentration in a plant material 5. Determination of total sodium, potassium, calcium concentration in milk 6. Determination of total Na, K, Ca concentration in banana 7. Determination of Lithium concentration flame photometrically Semester: 4 A. Water Analysis 1. Determination of alkalinity of the given water sample 2. To determine temporary hardness of water by the HCl method 3. Determination of total hardness of water by complexometric titration met hod 4. Determination of temporary hardness of water by EDTA method 5. Determination of calcium and magnesium in water by EDTA method 6. To determine chloride content of the given water sample by Mohr s method 7. Determination of COD of the water sample 8. Determination of DO in water by iodometric method 9. Determination of percentage of available chlorine in the supplied sample of bleaching powder 10. To determine the residual chlorine 11. Determination of pH & electrical conductivity 12. Determination of dissolved carbon dioxide 13. Determination of Inorganic P, total P & Sulphate spectrophotometrically. B. 1. 2. 3. 4. 5. 6. 7. Soil Analysis Determination Determination Determination Determination Determination Determination Determination of of of of of of of pH conductivity total alkalinity chloride & sulphate organic matter phosphorus & total phosphorus Na, K, Ca, Mg

C. Quantitative analysis of minerals/alloys/coins 1. Analysis the given brass (50-70% Cu+20-40%Zn+0-6%Sn+0-2%Pb+0-1%Fe) sampl e for its Cu and Zn contents colorimetrically. Alternatively,Cu by iodometry and Zn by EDTA method. 2. Analysis of the given sample of gun metal (90% Cu+10%Sn) for its Cu cont ent by iodometry. 3. To determine ferrous content in the supplied sample of iron ore/rust/ste el volumetrically against standard potassium dichromate solution using potassium ferricyanide as external indicator. 4. Analysis of the given sample of dolomite (equimolar CaCO3+MgCO3) for its volatile matter, insoluble matter, and its Ca & Mg contents by EDTA method. 5. Analyse the given five-rupee coin for its Cu content iodometrically, and Ni content as Ni-dmg complex colorimetrically or gravimetrically. Potentiometry and pH-metry (a) Determination of Concentration of Metal ions by potentiometric titration. 1. Determination of Fe(II) with potassium dichromate. 2. Cu(II) by iodometric method. (b) Determination of Dissociation Constants, pK values of 1. Glycine 2. Sulpho salicylic Acid 3. ortho-Phosphoric Acid

(c) Determination of Stability Constant of Complexs. 1. The stepwise and the overall stability constants of Cu(II)-Sulpho salicylic A cid Complexs. 2. The stepwise and the overall stability constants of Mn(II)-Amino Acid (eg Gly cine) Complexs.