ANALYTICALCHEMISTRY(Practical Handbook for M.Sc. Semester – III and IV

as per Revised Syllabus from 2018-19)

DR. KALPANA PATANKAR JAINVice Principal and Head,Department of Chemistry,BNN College, Bhiwandi,

Dist. Thane.

DR. RAJESH SAMANTDepartment of Chemistry,

K.C. College, Churchgate, Mumbai.

ISO 9001:2015 CERTIFIED

© AuthorsNo part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by anymeans, electronic, mechanical, photocopying, recording and/or otherwise without the prior written permission of theauthors and the publisher.

First Edition : 2015Second Revised Edition : 2018

(As per Revised Syllabus)

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Preface

This book has been written keeping in mind the revised syllabus and related requirements ofM.Sc. students, which can help them to perform their experiments efficiently. Most prominentfeature of this book is that it provides a comprehensive approach to the theoretical and practicalaspects of Analytical Chemistry in a simple way. The beauty of the book is embossed in the factthat the authors have tried their best to keep language simple, which a postgraduate student canunderstand. The procedure and observations are given pointwise which makes it easier to preparethe topics even for viva-voce. The details of all calculations and solution preparation are given indetails.

We hope that this book will bring uniformity in the procedures of the experiments for thestudents. By referring the book, the students can perform the experiments confidently. We indeedare very glad to launch this first practical handbook for M.Sc. Part – II (Sem. III and IV)Analytical students. Any valuable suggestions for the improvement of this book are mostwelcome.

Authors

Syllabus

Semester – IIIPracticals

PSCHA3P1 Group – A:1. Determination of the pK value of an indicator.2. Determination of copper and bismuth in mixture by photometric titration.3. Estimation of strong acid, weak acid and salt in the given mixture conductometrically.4. Analysis of mixture of carbonate and bicarbonate (present in ppm range) using

pH-metry.5. Determination of copper by extractive photometry using Diethyldithiocarbamate.

PSCHA3P2 Group – B:1. Estimation of drugs by non-aqueous titration: Pyridoxine hydrochloride and

Sulphamethoxazole.2. Determination of percentage purity of methylene blue indicator.3. Estimation of cholesterol and uric acid in the given sample of blood serum.4. Estimation of fluoride in a toothpaste.5. Determination of silica by molybdenum blue method.

PSCHA3P3 Group – C:1. Total reducing sugars before and after inversion in honey using: (a) Cole’ s Ferricyanide

(b) Lane-Eynon method.2. Analysis of lactose in milk.3. Estimation of Caffeine in tea.4. Estimation of Vitamin C in lemon juice/squash by Dichlorophenol-Indophenol method.5. Iodine value of oil/fat.6. Analysis of alcoholic beverages (Beer) for alcohol content by distillation followed by

specific gravity method, acidity by titration, total residue by evaporation.

PSCHA3P4 Group – D:1. To analyze Pyrolusite for Fe by colorimetry and/or Mn by volumetry.2. To analyze Magnelium for Mg by complexometry.3. Analysis of Bauxite for Ti by colorimetry/Al by gravimetry/Fe (volumetry).4. Analysis of water sample: Total hardness and salinity.5. Analysis of water sample: Acidity and sulphate (Benzidine method).

Note:1. The candidate is expected to submit a journal certified by the Head of the

Department/institution at the time of the practical examination.2. A candidate will not be allowed to appear for the practical examination unless he/she

produces a certified journal or a certificate from the Head of the institution/departmentstating that the journal is lost and the candidate has performed the required number ofexperiments satisfactorily.

3. The list of the experiments performed by the candidate should be attached with suchcertificate.

4. Use of non-programmable calculator is allowed both at the theory and the practicalexamination.

Semester – IV

PSCHA4P1 Group – A:1. Determination of pK value of H3PO4 potentimetrically.2. Estimation of Na+ in dairy whitener by flame photometry.3. Spectrophotometric determination of pH of buffer solution.4. Simultaneous determination of Ti3+ and V5+ spectrophotometrically by H2O2 method.5. To analyze Bronze for Zn by complexometric method.

PSCHA4P2 Group – B:1. Analysis of drugs by non-aqueous titration: Glycine and Sodium Benzoate.2. Analysis of detergents: Active detergent matter, alkalinity and oxygen releasing capacity.3. Determination of the purity of crystal violet.4. Estimation of Ca in Ca-pentathonate/calcium lactate tablets.5. Canned food: Limits test for tin/zinc.

PSCHA4P3 Group – C:1. Analysis of Calcium, Iron and Phosphorous in milk.2. Determination of SAP value of oil.3. Estimation of Aldehyde in lemon grass oil/cinnamon oil.4. Estimation of Glucose by Folin-Wu method.5. Analysis of water sample: Mn2+ by colorimetric method.

PSCHA4P4 Group – D:1. Project Evaluation

Contents

SEMESTER – III

Group – A

1. Determination of the pK Value of an Indicator 1 – 3

2. Determination of Copper and Bismuth in Mixture byPhotometric Titration

4 – 6

3. Estimation of Strong Acid, Weak Acid and Salt in the GivenMixture Conductometrically

7 – 10

4. Analysis of Mixture of Carbonate and Bicarbonate usingpH-metry

11 – 14

5. Determination of Copper by Extractive Photometry usingDiethyldithiocarbamate

15 – 17

Group – B

1. Estimation of Drugs by Non-Aqueous Titration: PyridoxineHydrochloride and Sulphamethoxazole

18 – 20

2. Determination of Percentage Purity of Methylene Blue Indicator 21 – 24

3. Estimation of Cholesterol and Uric Acid in the Given Sample ofBlood Serum

25 – 29

4. Estimation of Fluoride in a Toothpaste 30 – 32

5. Determination of Silica by Molybdenum Blue Method 33 – 35

Group – C

1. Total Reducing Sugars before and after Inversion in Honeyusing: (a) Cole’s Ferricyanide

(b) Lane-Eynon Method

36 – 42

2. Analysis of Lactose in Milk 43 – 46

3. Estimation of Caffeine in Tea 47 – 48

4. Estimation of Vitamin C in Lemon Juice/Squash byDichlorophenol-Indophenol Method

49 – 51

5. Iodine Value of Oil/Fat Sample 52 – 54

6. Analysis of Alcoholic Beverages (Beer) for Alcohol Content byDistillation Followed by Specific Gravity Method, Acidity byTitration and Total Residue by Evaporation

55 – 59

Group – D

1. To Analyze Pyrolusite for Fe by Colorimetry and/or Mn byVolumetry

60 – 64

2. To Analyze Magnelium for Mg Titrimetrically 65 – 67

3. Analysis of Bauxite for Ti by Colorimetry/Al by Gravimetry/Feby Volumetry

68 – 73

4. Analysis of Water Sample: Total Hardness and Salinity 74 – 77

5. Analysis of Water Sample: Acidity and Sulphate (BenzidineMethod)

78 – 82

SEMESTER – IV

Group – A

1. Determination of pK Value of H3PO4 Potentiometrically 83 – 85

2. Estimation of Na+ in Dairy Whitener by Flame Photometry 86 – 88

3. Spectrophotometric Determination of pH of Buffer Solution 89 – 91

4. Simultaneous Determination of Ti3+ and V5+

Spectrophotometrically by H2O2 Method92 – 95

5. To Analyze Bronze for Zn by Complexometric Method 96 – 98

Group – B

1. Analysis of Drugs by Non-Aqueous Titration: Glycine andSodium Benzoate

99 – 101

2. Analysis of Detergents: Active Detergent Matter, Alkalinity andOxygen Releasing Capacity

102 – 106

3. Determination of the Purity of Crystal Violet 107 – 110

4. Estimation of Ca in Ca-pentathonate/Calcium Lactate Tablets 111 – 113

Group – C

1. Analysis of Calcium, Iron and Phosphorous in Milk 114 – 118

2. Determination of SAP Value of Oil 119 – 120

3. Estimation of Aldehyde in Lemon Oil/Cinnamon Oil 121 – 123

4. Estimation of Glucose by Folin-Wu Method 124 – 126

5. Analysis of Water Sample: Mn2+ by Colorimetric Method 127 – 128

Group – D

1. Research Project/Experimental Sample Analysis Report and itsPresentation

129 – 130

1

SEMESTER III

GROUP – A

1

Determination of the pKValue of an Indicator

Exp. No. A-1

Aim: To determine the pKin value of an indicator spectrophotometrically.

Theory

An indicator is a compound that itself acts as a weak acid or a weak base. Being an indicatorit possesses two different colours in its two forms, i.e., the acidic and the basic forms of theindicator. The max. values of the two coloured forms will be different. The method involvesdetermination of the absorbance of several solutions, in which a constant amount of the indicatoris added. These solutions will have different pH values. Even though the total amount of theindicator added is the same the concentration of the indicator in the acidic and in the basic formwill defer depending on the pH of the solution. All the measurements are made at the samewavelength. Moreover, in addition to these solutions two more solutions are prepared such that inone of them the added indicator will be totally in the acidic form and in the other it will be totallyin the basic form. For the calculation of the indicator constant the Henderson’s equation is used.The equation is,

pH = pKin + log [salt]/[acid] when the [salt] = [acid]

That is the [base form] = [acid form] last term will be equal zero. Then pH = pKin.

2 Analytical Chemistry

The concentration of the acid and the base forms are calculated from the measured values ofthe absorbance of the solutions and that for the indicator in totally in the acidic and totally in thebasic form.

Requirements

Chemicals: Disodium hydrogen phosphate, potassium dihydrogen phosphate,Bromothymol blue, 20% ethanol.

Glassware and Instruments: 50 cm3 volumetric flasks 8 Nos., Graduated pipettes10 cm3 and 5 cm3, 250 cm3 beaker, 100 cm3 borosil beakers 8 Nos., watch glass, funnel,glass rod etc. and Spectrophotometer.

Preparation of Solutions

1. Bromothymol blue indicator: 0.100 g of Bromothymol blue indicator is dissolved in20% ethanol.

2. 0.2 M Na2HPO4: Dissolve 3.55 g Na2HPO4 in 100 cm3 distilled water.

3. 0.2 M KH2PO4: Dissolve 2.72 g KH2PO4 in 100 cm3 distilled water.

4. 3 M HCl: 133 cm3 conc. HCl dilute to 500 cm3 with distilled water.

5. 3 M NaOH: 60 g NaOH dissolved in 500 cm3 with distilled water.

Procedure

1. Dissolve 100 mg of bromothymol blue, in 100 cm3 of 20% ethanol.

2. Dissolve 2.4 g of disodium hydrogen phosphate in 100 cm3 of water to produce 0.2 Msolution.

3. Similarly, dissolve 3.4 g of potassium dihydrogen phosphate in 100 cm3 of water toprepare 0.2 M solution.

4. Prepare a series of buffer solutions as follows:

Flask Volume of KH2PO4

(cm3)Volume of Na2HPO4

(cm3)HCl or NaOH Absorbance

1 5.0 0.0 2 drops of 3 M HCl Aa =

2 5.0 1.0

3 10.0 5.0

4 5.0 10.0

Determination of the pK Value of an Indicator 3

5 1.0 5.0

6 1.0 10.0

7 0.0 5.0 2 drops of 3 M NaOH Ab =

5. Add 2.0 cm3 of bromothymol blue to each flask.

6. Make up the volume to 50 cm3.

7. Measure the pH of each solution.

8. Measure the absorbance of each solution.

9. Plot the graphs of absorbance Vs. pH of the solution at 525 nm.

10. Plot a graph of the log [A – Aa]/[Ab – A].

11. Obtain the pKin value from the intercept. Where Aa stands for the absorbance of theflask no. 1, Ab stands for the absorbance of flask no. 7.

12. Calculate the pKin value both from the graph and by calculation.

Calculation

Sr. No. A – Aa Ab – A [A – Aa]/[Ab – A] log [A – Aa]/[Ab – A]

pKin = pH – log [A – Aa]/[Ab – A]

Calculate Mean pKin

Result

1. pKin value for indicator is = __________.

2. Kin value for indicator is = __________.