A Practical Approach to

PharmaceuticalAnalysis

Instrumental and Manual

for B. Pharmacy and M. Pharmacy Students

-jEditedbyj-

Rajesh Kumar NemaDirector, SD College of Pharmacy and Vocational Studies, Muzaffarnagar, UP

S. N. MeyyanathanProfessor and Head. Department of Pharmaceutical Analysis.

JSS College of Pharmacy. Ooty, Tamilnadu

Chandra Shekhar SharmaSenior Lecturer, BN College of Pharmacy, Udaipur. Rajasthan

Mahesh VermaSenior Lecturer, Faculty of Pharmacy, Integral University, Lucknow, UP

C.S. BhanPrincipal, MGCPS, Jaipur, Rajasthan

CBS Publishers & DistributorsNew Delhi Bangalore

Contents

Preface

1. Spectrophotometric Analysis

2. Flame Photometry

3. Potentiometry

4. Fluorimetry

5. Polarimetry

6. Conductometry

7. Refractometry

8. Nephloturbidimetry

9. Chromatography (TLC Paper, HPLC, HPTLC)

10. Infrared Spectroscopy

11. Mass Spectrometry

12. Miscellaneous Methods of Analysis

Karl Fischer Titration

Kleldahl's Method

1

63

76

86

98

116

127

140

146

176

193

202

202

206

EXPERIMENTS

1. Spectrophotometric Analysis 11.1 To determine the Xmax of Potassium Permanganate. 71.2 To determine the percentage purity of given sample of Paracetamol by Spectroscopy. 91.3 To perform the assay of Paracetamol tablet using calibration curve method. 141.4 To determine the percentage purity of given sample of Isoniazid by Spectroscopy. 201.5 Tp cdrry out the analysis of Diclofenac sodium and Paracetamol in combined dosage form. 241.6 To study the effect of solvents upon the absorption spectrum of.Griseofulvin. 311.7 To find out percentage purity of Diltiazem HCI tablet IP by calibration curve method. 361.8 To find out X of Diltiazem HCI in different solvents. 421.9 To determine percentage purity of the given sample of Chloramphenicol capsules I.P. 46

1.10 To determine the percentage purity of given sample of Furosemide injection I.P. 51

A Practical Approach to Pharmaceutical Analysis

EXPERIMENTS

1.11 To determine the percentage purity of given sample of Allopurinol tablets I.P. 541.12 To determine the percentage purity of given sample of Propranolol HCI tablets I.P. 58

2. Flame Photometry 632.1 To determine the Sodium concentration in the given sample by Flame Photometry. 632.2 To determine the potassium concentration in given sample of KCI (Potassium Chloride) 682.3 To determine the Sodium and Potassium concentration in given sample. 72

3. Potentiometry 763.1 To determine the strength of strong suiphuric acid using strong base sodium hydroxide

by Potentiometry. 763.2 To study the effect of Quenching on the fluorescence of Quinine sulphate. 82

4. Fluorimetry 864.1 To determine the concentration of Quinine Sulphate by fluorimetry. 864.2 To perform the assay of Quinine Sulphate Tablet by fluorimetry. 91

5. Polarimetry 985.1 To find out the glucose (dextrose) content in a supplied sample by polarimetry. 985.2 To find out the percentage of glucose content in the marketed product of glucose. 1035.3 To find out the glucose content in the marketed product of Dextrose injection I.P. 1085.4 To find out the percentage of glucose content in the marketed product of Oral

Rehydration Salt (ORS). 112

6. Conductometry 1166.1 To determine the end-point and normality of given acid by conductometric tltration. 1166.2 To carry out the conductometric titration of mixture of acids (0.1N HCI -t 0.1N CH3COOH)

vs. strong base (1N NaOH) 121

7. Refractometry 1277.1 To find out the refractive indices of different llquids (Benzene, Glycerin and Water) by

Abbes refractometer. 1277.2 To find out the molar refraction of benzene by abbe's refractometer and also conflrm

the structure of benzene . 1 3 17.3 To find out the Concentration of unknown sample of glycerin by refractometry. 136

8.Nephtohjrbldlmetry)8.1 To perform the limit fest for Chloride in the given solution by using nephldturbidimetry 1408.2 To perform the limit test for sulphate in the given solution by using nephloturbidimetry. 143

9. Chromatography

Contents

EXPERIMENTS

9.2 To identify the given drug amongst the paracetamol, aspirin and caffeine citrate withthe help of thin layer chromatography and calculate its Rf value. 152

9.3 To identify the given sulpha drug among the sulphadiazine, sulphamethoxazole andtrimethoprim with the help of thin layer chromatography and calculate its Rf value. 154

9.4 To perform the Separation of amino acids by paper chromatography. 1569.5 To identify the given sample of sugar with the help of ascending paper

chromatography and calculate its Rf value. 1609.6 To demonstrate high Performance liquid chromatography. 1669.7 To analyze the given tablets of paracetamol/ibuprofen-paracetamol combination

byHPTLC method. 168

10. Infrared Spectroscopy 176To interpret the I.R. spectra of the following compounds. 1763-Pentanone, Acetophenone, Benzyl alcohol, Benzyl Nitrite, Benzaldehyde, N- Methylacetamide, Ethylacetate.

11. Mass Spectrometry 193To interpret the mass spectra of the following compounds, 3-Pentanol, 3-Phenyl-2-propanol,Hesane, 2-Methyl butyramide, n-Butylamine, Naphthlene, 2-Butanoic acid, Ethylacetate,Ethyl methyl ether, 1 -Bromopropanone, 4- Heptanone.

12. MisceltaneousMethodsof Analysis 20212.1 Karl Fischer Titration 202

12.1. To determine Percentage of moisture content of the given sample by Karl Fischer Titration.

12.2 Kieldahl's Method 20612,2. To determine Percentage of nitrogen content of the given sample by Kjeldahl's Method.