Analytical Chemistry

 List of Experiments in CBCS based UG/ B.Sc. Chemistry Core and General Elective Courses in Sido Kanhu Murmu University, Dumka

Semester I

CHEMISTRY CORE PRACTICAL-I                          [4 Credits =60 Lectures]

Group-A

(A) Titrimetric Analysis 
(i) Calibration and use of apparatus 
(ii) Preparationof solutions of different Molarity/Normality of titrants

(B) Acid-Base Titrations

(i) Estimation of carbonate and hydroxide present together in mixture.

(ii) Estimation of carbonate and bicarbonate present together in a mixture.

(iii) Estimation of free alkali present in different soaps/detergents

(C) Oxidation-Reduction Titrimetry

(i) Estimation of Fe(II) and oxalic acid using standardized KMnO4 solution.

(ii) Estimation of oxalic acid and sodium oxalate in a given mixture.

(iii) Estimation of Fe(II) with K2Cr2O7 using internal (diphenylamine, anthranilic acid) and external indicator.

Group-B

1. Surface tension measurements.

a. Determine the surface tension by (i) drop number (ii) drop weight method.

b. Study the variation of surface tension of detergent solutions with concentration.

2. Viscosity measurement using Ostwald’s viscometer.

a. Determination of viscosity of aqueous solutions of (i) polymer (ii) ethanol and (iii) sugar at room temperature.

b. Study the variation of viscosity of sucrose solution with the concentration of solute.
CHEMISTRY (GE Lab-1) General Elective PRACTICAL-I  [2 Credits =30 Lectures]

Section A: Inorganic Chemistry - Volumetric Analysis

1. Estimation of sodium carbonate and sodium hydrogen carbonate present in a mixture.

2. Estimation of oxalic acid by titrating it with KMnO₄.

3. Estimation of water of crystallization in Mohr’s salt by titrating with KMnO₄.

4. Estimation of Fe (II) ions by titrating it with K₂Cr₂O₇ using internal indicator.

5. Estimation of Cu (II) ions iodometrically using Na₂S₂O₃.

Section B:

Organic Chemistry

1. Detection of extra elements (N, S, Cl, Br, I) in organic compounds (containing upto two extra elements)

Semester II

CHEMISTRY CORE PRACTICAL-II                      [4 Credits =60 Lectures]

1. Checking the calibration of the thermometer

2. Purification of organic compounds by crystallization using the following solvents: a. Water b. Alcohol c. Alcohol-Water

3. Determination of the melting points of above compounds and unknown organic compounds (Kjeldahl method and electrically heated melting point apparatus)

4. Determination of boiling point of liquid compounds. (boiling point lower than and more than 100 °C by distillation and capillary method)

5. Thermochemistry

(a) Determination of heat capacity of a calorimeter for different volumes using change of enthalpy data of a known system (method of back calculation of heat capacity of calorimeter from known enthalpy of solution or enthalpy of neutralization).

(b) Determination of heat capacity of the calorimeter and enthalpy of neutralization of hydrochloric acid with sodium hydroxide.

(c) Calculation of the enthalpy of ionization of ethanoic acid.

(d) Determination of heat capacity of the calorimeter and integral enthalpy (endothermic and exothermic) solution of salts.

(e) Determination of basicity/proticity of a polyprotic acid by the thermochemical method in terms of the changes of temperatures observed in the graph of temperature versus time for different additions of a base. Also calculate the enthalpy of neutralization of the first step.

(f) Determination of enthalpy of hydration of copper sulphate.

(g) Study of the solubilityΔ of benzoic acid in water and determination of H. Any other experiment carried out in the class.
CHEMISTRY (GE Lab-2) General Elective PRACTICAL-II [2 Credits =30 Lectures]

Section A: Physical Chemistry

Thermochemistry

1.Determination of heat capacity of calorimeter for different volumes.

2.Determination of enthalpy of neutralization of hydrochloric acid with sodium hydroxide.

Ionic equilibria

pH measurements

a) Measurement of pH of different solutions like aerated drinks, fruit juices, shampoos and soaps (use dilute solutions of soaps and shampoos to prevent damage to the glass electrode) using pH-meter.

b) Preparation of buffer solutions:

(i) Sodium acetate-acetic acid

(ii) Ammonium chloride-ammonium hydroxide Measurement of the pH of buffer solutions and comparison of the values with theoretical values.

Section B: Organic Chemistry

1. Purification of organic compounds by crystallization (from water and

alcohol) and distillation.

2. Criteria of Purity: Determination of melting and boiling points.

3. Preparations: Recrystallisation, determination of melting point and calculation of quantitative yields to be done.

(a) Bromination of Phenol/Aniline

(b) Benzoylation of amines/phenols

(c) Oxime and 2,4 dinitrophenylhydrazone of aldehyde/ketone

Semester III

CHEMISTRY CORE PRACTICAL-III                        [6 Credits =75 Lectures]

(Group-A)

(A) Iodo / Iodimetric Titrations

(i)Estimation of Cu(II) and K2Cr2O7 using sodium thiosulphate solution(Iodimetrically). (ii) Estimation of available chlorine in bleaching powderiodometrically.

(B) Inorganic preparations

(i)Cuprous Chloride, Cu2Cl2 (ii) Preparation of Aluminium potassiumsulphate KAl(SO4)2.12H2O (Potash alum) or Chrome alum.

(Group – B)

1. Functional group tests for alcohols, phenols, carbonyl and carboxylicacid group.

2. Organic preparations:

i. Acetylation of one of the following compounds: amines (aniline, o-, m-,p-toluidines and o-, m-, p-anisidine)β and phenols ( - naphthol, vanillin,salicylic acid) by any one method: a. Using conventional method. b. Usinggreen approach

ii. Benzolyation of one of the following amines (aniline, o-, m-, ptoluidines and o-, m-, p-anisidine) andβ one of the following phenols ( - naphthol, resorcinol, p-cresol) by Schotten-Baumann reaction.

iii. Oxidation of ethanol/ isopropanol (Iodoform reaction).

iv. Bromination of any one of the following:

a. Acetanilide by conventional methods b. Acetanilide using green approach (Bromate-bromide method)

v. Nitration of any one of the following:

a. Acetanilide/nitrobenzene by conventional method b. Salicylic acid by green approach (using ceric ammonium nitrate).

vi. Selective reduction of meta dinitrobenzene to m-nitroaniline.

vii. Reduction of p-nitrobenzaldehyde by sodium borohydride.

viii. Hydrolysis of amides and esters. The above derivatives should be prepared using 0.5 1g of the organic compound. The solid samples must be collected and may be used for recrystallization, melting point and TLC.

Group-C

I. Distribution of acetic/ benzoic acid between water and cyclohexane.

II. Study the equilibrium of at least one of the following reactions by the distribution method:

(i) I₂(aq) + I^- →  I₃^-(aq)

(ii) Cu ²⁺ (aq) + nNH₃ →Cu(NH₃ )

(iii) Study the kinetics of the following reactions. 1. Integrated rate method: a. Acid hydrolysis of methyl acetate with hydrochloricacid. b. Saponification of ethyl acetate.

CHEMISTRY(GE Lab-3) General Elective PRACTICAL-III [2 Credits =30 Lectures]

Section A: Physical Chemistry

Distribution

Study of the equilibrium of one of the following reactions by the distribution method:

I₂(aq) + I^-(aq) ⇌ I₃ ^-(aq)

Cu²⁺(aq) + xNH²(aq) ⇌ [Cu(NH₃)x]²⁺

Conductance

i. Determination of cell constant

ii. Determination of equivalent conductance, degree of dissociation and dissociation constant of a weak acid.

iii. Perform the following conductometric titrations:

iv. Strong acid vs. strong base

v. Weak acid vs. strong base

vi. Weak acid vs. strong base

Section B: Organic Chemistry

Systematic Qualitative Organic Analysis of Organic Compounds possessing monofunctional groups (-COOH, phenolic, aldehydic, ketonic,amide, nitro, amines) and preparation of one derivative.

 Semester IV

CHEMISTRY CORE PRACTICAL-IV                      [6 Credits =75 Lectures]

(Group-A)

1. Detection of extra elements.

2. Functional group test for nitro, amine and amide groups.

3.Qualitative analysis of unknown organic compounds containing simple functional groups (alcohols, carboxylic acids, phenols and carbonyl compounds)

(Group-B)

Gravimetric Analysis:

i. Estimation of nickel using Dimethylglyoxime (DMG).

ii. Estimation of copper as CuSCN

Inorganic Preparations:

i. Tetraamminecopper (II) sulphate, [Cu(NH3)4]SO4.H2O

ii. Cis and trans K[Cr(C2O4)2. (H2O)2] Potassiumdioxalatodiaquachromate (III)

iii. Tetraamminecarbonatocobalt (III) ion

iv. Potassium tris (oxalate) ferrate(III)

Group-C

Conductometry

1) Perform the following conductometric titrations:

i. Strong acid vs. strong base

ii. Weak acid vs. strong base

iii. Mixture of strong acid and weak acid vs. strong base

iv. Strong acid vs. weak base

Potentiometry

2) Perform the following potentiometric titrations:

i. Strong acid vs. strong base

ii. Weak acid vs. strong base

iii. Dibasic acid vs. strong base

v. Potassium dichromate vs. Mohr's salt

CHEMISTRY(GE Lab-4) General Elective PRACTICAL-IV [2 Credits =30 Lectures]

Section A: Inorganic Chemistry

Semi-micro qualitative analysis using H₂S of mixtures- not more than four ionic species (two anions and two cations and excluding insoluble salts) out of the following:

Cations : NH4⁺, Pb²⁺, Ag⁺, Bi³⁺, Cu²⁺, Cd²⁺, Sn²⁺, Fe³⁺, Al³⁺, Co²⁺, Cr³⁺, Ni²⁺,Mn²⁺, Zn²⁺, Ba²⁺, Sr²⁺, Ca²⁺, K⁺ Anions : CO₃ ^2– , S^2–, SO^2–, S₂O₃^2–, NO₃ ^–, CH₃COO^–, Cl^–, Br^–, I^–, NO₃^–,SO₄^2-, PO₄^3-, BO₃^3-, C₂O₄ ^2-, F^-(Spot tests should be carried out wherever feasible)

Section B: Physical Chemistry

(I) Surface tension measurement (use of organic solvents excluded).

a) Determination of the surface tension of a liquid or a dilute solution using a stalagmometer.

b) Study of the variation of surface tension of a detergent solution with concentration.

(II) Viscosity measurement (use of organic solvents excluded).

a) Determination of the relative and absolute viscosity of a liquid or dilute solution using an Ostwald’s viscometer.

b) Study of the variation of viscosity of an aqueous solution with concentration of solute.

 Semester V

CHEMISTRY CORE PRACTICAL-I                      [4 Credits =60 Lectures]

(Group-A)

1. Estimation of glycine by Sorenson’s formalin method.

2. Study of the titration curve of glycine.

3. Saponification value of an oil or a fat.

4. Determination of Iodine number of an oil/ fat.

(Group-B)

Colourimetry

I. Verify Lambert-Beer’s law and determine the concentration of

CuSO₄/KMnO₄/K₂Cr₂O₇ in a solution of unknown concentration

II. Determine the concentrations of KMnO₄ and K₂Cr₂O₇ in a mixture.

III. Determine the amount of iron present in a sample using 1,10- phenathroline.

PRACTICAL-Discipline Specific Elective DSE LAB- I:[4 Credits=60 Lectures]

APPLICATIONS OF COMPUTERS IN CHEMISTRY 

Computer programs based on numerical methods for  

1.Roots of equations: (e.g. volume of van der Waals gas and comparison with ideal gas, pH of a weak acid).

2.Numerical differentiation (e.g., change in pressure for small change in volume of a van der Waals gas, potentiometric titrations).

3.Numerical integration (e.g. entropy/ enthalpy change from heat capacity data), probability distributions (gas kinetic theory) and mean values.

PRACTICALS- Discipline Specific Elective DSE LAB-II : [4 Credits=60 Lectures]

ANALYTICAL METHODS IN CHEMISTRY 

I. Separation Techniques

1. Chromatography: Separation of mixtures

(i) Paper chromatographic separation of Fe³⁺, Al³⁺, and Cr³⁺.

(ii) Separation and identification of the monosaccharides present in the given mixture (glucose & fructose) by paper chromatography. Reporting the Rf values.

2. Solvent Extractions:

To separate a mixture of Ni²⁺ & Fe²⁺ by complexation with DMG and extracting the Ni²⁺- DMG complex in chloroform, and determine its concentration by spectrophotometry. Solvent extraction of zisconium with amberliti LA-1, separation from a mixture of irons and gallium.

3. Determine the pH of the given aerated drinks fruit juices, shampoos and soaps.

4. Determination of Na, Ca, Li in cola drinks and fruit juices using flame photometric techniques.

5. Analysis of soil: Determination of pH of soil.

Semester VI

  

CHEMISTRY CORE PRACTICAL-VI                         [4 Credits =60 Lectures]

(Group-A)

Qualitative semimicro analysis of mixtures containing 3 anions and 3 cations. Emphasis should be given to the understanding of the chemistry of different reactions. The following radicals are suggested:

CO₃ ^{2 -}, NO2 ^-, S^2-, SO₃ ^2-,S₂O₃ ^{2 -}, CH₃COO^-, F^-, Cl^-, Br^-, I^-, NO₃ ^-, BO₃ ^3-,C₂O₄^2-, PO₄^3-, NH₄⁺, K⁺, Pb²⁺, Cu²⁺, Cd²⁺, Bi³⁺, Sn²⁺, Sb³⁺, Fe³⁺, Al³⁺, Cr³⁺,Zn²⁺, Mn²⁺, Co²⁺, Ni²⁺, Ba²⁺,Sr²⁺, Ca²⁺, Mg²⁺

Mixtures should preferably contain one interfering anion, or insoluble component (BaSO₄, SrSO₄, PbSO₄, CaF₂ or Al₂O₃) or combination of anions e.g. CO₃^2- and SO₃^2-, NO2^- and NO₃^-, Cl^- and Br^-, Cl^- and I^-, Br^- and I^- , NO₃ ^- and Br^- , NO₃^- and I^-.

Spot tests should be done whenever possible.

i.Measurement of 10 Dq by spectrophotometric method

ii.Verification of spectrochemical series.

iii.Controlled synthesis of two copper oxalate hydrate complexes: kinetic

vs thermodynamic factors.

iv.Preparation of acetylacetanato complexes of Cu²⁺/Fe³⁺. Find λ the max of the complex.

v.Synthesis of ammine complexes of Ni(II) and its ligand exchange reactions (e.g. bidentate ligands like acetylacetone, DMG, glycine) by substitution method.

(Group-B)

1. Extraction of caffeine from tea leaves.

2. Preparation of sodium poly acrylate.

3. Preparation of urea formaldehyde.

4.Analysis of Carbohydrate: aldoses and ketoses, reducing and non reducing sugars.

5. Qualitative analysis of unknown organic compounds containing monofunctional groups (carbohydrates, aryl halides, aromatic hydrocarbons,nitro compounds, amines and amides) and simple bi functional groups, fore.g. salicylic acid, cinnamic acid, nitrophenols etc.

6.Identification of simple organic compounds by IR spectroscopy andNMR spectroscopy (Spectra to be provided).

7. Preparation of methyl orange.

PRACTICALS- Discipline Specific Elective DSE LAB-III : [4 Credits=60 Lectures]

GREEN CHEMISTRY

1. Using renewable resources Preparation of biodiesel from vegetable oil.

2. Avoiding waste

Principle of atom economy.

Use of molecular model kit to stimulate the reaction to investigate how the atom economy can illustrate Green Chemistry. Preparation of propene by any one method can be studied (I) Triethylamine ion + OH- → propene + trimethylpropene + water H₂SO₄/ (II) 1-propanol propene + water

3. Diels Alder reaction in water

Reaction between furan and maleic acid in water and at room temperature rather than in benzene and reflux.

4. Extraction of D-limonene from orange peel using liquid CO₂ prepared form dry ice.

PRACTICALS- Discipline Specific Elective DSE LAB-IV : [4 Credits=60 Lectures] 

INDUSTRIAL CHEMICALS & ENVIRONMENT 

1. Determination of dissolved oxygen in water.

2. Determination of Chemical Oxygen Demand (COD)

3. Percentage of available chlorine in bleaching powder.

4. Measurement of chloride, sulphate and salinity of water samples by simple titration method (AgNO3 and potassium chromate).

5. Estimation of total alkalinity of water samples (CO3 2-, HCO3 -) using double titration method.

1.pH Measurements Working Principle

2.Conductivity Measurement Working Principle

3.Dissolved Oxygen Measurement Working Principle

4.pH Measurement Theory

5.Determination of Fe2+ in FAS using K2Cr2O7 through Potentiometric Titration