sample copy. not for distribution.vi shaik.akram ali, shaik.afroz for their support &...

Sample Copy. Not For Distribution.

i

Comprehensive Practical Manual of Pharmaceutical Chemistry


ii

Publishing-in-support-of,

EDUCREATION PUBLISHING

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© Copyright, 2019, Authors

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ISBN: 978-93-88719-95-7

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Printed in India


iii

Comprehensive Practical

Manual of Pharmaceutical

Chemistry

Shaik. Munwar

Shaik. Ammaji

EDUCREATION PUBLISHING (Since 2011)

www.educreation.in


iv


v

Preface

The edition of Comprehensive Practical Manual of

Pharmaceutical Chemistry is authored in simple and

comprehensive style according to PCI (Pharmacy Council of

India) syllabus to meet the specific needs of the pharmacy

students.

It provides comprehensive yet concise chemistry for D.Pharmacy,

B.Pharmacy, M.Pharmacy and Pharm D students.

The main objective of this manual is to attract students to learn the

basic theories of pharmaceutical chemistry thus the manual is

aimed to enrich the inadequancy in teaching and learning of

pharmaceutical chemistry by providing enormous information. The

style of presentation of this manual is such that it not only gives

deeper understanding of the subject but also will help the beginners

to overcome the fright of the subject. The manual gives concise

and pointwise information required during practicals in single book

and eliminates the need of too many reference books during

practicals. The manual authored in simple,lucid and easy language.

I express my heartful and sincere thanks to Hon. Prof. Ramarao

Nadendla (Principal, Chalapathi Institute of Pharmaceutical

Sciences and Dean, Faculty of Pharmacy-Acharya Nagarjuna

University),

I will be failing in my duty if I don’t record the inspiration received

by my teachers Dr.S.Vidyadhara, Dr.G.Pratap Kumar,

Dr.Govindarajan Rajan Rangarajan, Dr.M.V. Nagabhushanam,

Prof.Sd.Abdul Azeez Basha, Dr.Nagulu Malothu, Dr.Raman Dang,

Dr.J.N.Suresh Kumar, Dr.C.B.Patil, Dr.S.A.Rahaman, Dr. A.M.S.

Sudhakar Babu, Dr. Prasada Rao Manchineni, Dr.A.Rajendhra

Prasad, Dr.T.Vinay Kumar, Dr.D.Varun, Prof.K.N.Rajinikanth and

Dr.A.Elphine Prabahar.

I am immensely grateful to my Parents Mr.Shaik. Ameer Jan and

Mrs.Shaik.Munni Begum, my Father-In-Law Abdul Haq, my

brother Mr.Shaik.Anwar, my Sister-In-Law Shaik.Meenaz

Begum, my Brother-In-Law Shaik.Ansari, my Sister-In-Laws

Mrs.Asiya, Miss.Roshini, Miss.Reshma, my nephew


vi

Shaik.Akram Ali, Shaik.Afroz for their support & inspiration and

my wife Shaik.Haseena Begum for her patience and my family

members for their support.

I am thankful to my friends Mr.Md.Mohid (Bossom Friend),

Dr.Md.Yunoos, Mr.Harekrishna Roy, Mr Sk.Liakhat Ali,

Mr.Sk.Nayab Rasool, Mrs.G.Sai Sri Lakshmi, Mr.M.Saifulla

Khan, Mr.R.Narasimha Naik, Mr.Md.Salahuddin,

Mr.P.Lingeswara Rao, Mr.Shaik Abdul Saleem,

Mr.G.Raghavendra Kumar, Mr. Sd.Gouse Firoz, Mrs.K.Uma

Maheshwari, Mr.K.Sudhakar, Mr.D.Prasanth, Mr.K.Dilip Raja,

Mr.K.Abhinav, Dr. Ramaiah Maddi, Mrs.B.Anitha, Mr.A.Gopi

Reddy, Dr.D.Harish and the teaching & non-teaching faculty

members and students of Chalapathi Institute of Pharmaceutical

Sciences for their help in bringing out this manual.

I hope that the readers will find the manual more informative and

rewarding.

There is always a room for improvement. I welcome constructive

suggestions from readers from all corners of scientific community

for further improving the preparation of subject matter of this

manual

------ SHAIK.MUNWAR


vii

I express my heartful and sincere thanks to Hon. Prof.

Y.Ankamma Chowdary (Principal, NRI College of pharmacy)

I will be failing in my duty if I don’t record the inspiration received

by my teachers Prof A.prameela rani, Dr.SK.Masthnamma,

Dr.Afzal Basha, Dr.V.Narendra, Dr.G.Vamsee krishna,

Dr.I.V.Rama rao, Dr.M.Vamsi Krishna.

I am immensely grateful to my Parents Mr.Shaik. Mahaboob

Subhani and Mrs.SK.Halimbee, my brother Mr.Shaik.Khaza, my

Sisters Shaik.Gowsiya banu, SK.Meherajunnisa, Sk.Shahanaz for

their support & inspiration and my husband MD.Khaja for his

patience.

I am thankful to my friends Sk.Basheer, S.Sasi mounika, U.Samba

moorthy, T.V.Sowjanya, P.kanchana, T.harika, P.Divya,

T.Bharathi, Y. Veerendrenadh, A. Surendra, P.Ramyasree,

U.Tulasi, CH.Manasa, CH.Sangeetha L.Vasantha, and other

teaching and non teaching faculty of NRI college of pharmacy for

their help.


viii

Dedicated to

My PARENTS,

My Soulmate

MOHAMMED. KHAJA and

My Daughter

MOHAMMED. PARVEEN

------ SHAIK.AMMAJI


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Content

Sr. Title Page

1 Importance of Wearing White Apron 1

2 Laboratory Safety Rules 3

3 Safety Symbols and Identification of Correct

Fire Extinguisher

11

4 Hands Washing Techniques in Laboratory 14

5 Emergency Procedure and First Aid 18

6 Adjustment and Handling of Bunsen Burner 21

7 Introduction to Basic Laboratory Glassware 27

8 Washing of Laboratory Glassware 52

9 Rinsing of Volumetric Glassware in Chemistry

Lab

57

10 Glassware Care and Use Recommendations 58

11 Safe Handling of Glassware 61

12 Introduction to Analytical Instruments 67

13 Methods of Expressing Concentrations 100

14 Methods of preparing Important Reagents 109

15 Introduction to Filtration Techniques 196

16 Calibration of Analytical Balance 206

17 Introduction to Limit Test 213

18 Limit Test For Chlorides 218

19 Limit Test For Sulphates 221

20 Limit Test For Iron 224

21 Limit Test For Heavy Metals 227

22 Limit Test For Lead 232

23 Limit Test For Arsenic 235

24 Modified Limit Test For Chlorides And

Sulphates

240

25 Introduction to Anions and Cations 242

26 Identification Tests For Ferrous Sulphate 264

27 Identification Tests For Magnesium Hydroxide 268

28 Identification Tests For Calcium Gluconate 271


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29 Identification Tests For Copper Sulphate 274

30 Identification Tests For Sodium Bicarbonate 277

31 Neutralizing Capacity of Aluminium Hydroxide

Gel

281

32 Determination of Potassium Iodate and Iodine in

Potassium Iodide

283

33 Swelling Power of Bentonite 285

34 Preparation of Potash Alum 287

35 Preparation of Ferrous Sulphate 289

36 Preparation of Boric Acid 391

37 Systematic Qualitative Analysis of Organic

Compounds

292

38 Experiments Involving Recrystallization 318

39 Experiments Involving Steam Distillation 321

40 Determination of Acid Value 324

41 Determination of Iodine Value 329

42 Determination of Saponification Value 335

43 Preparation of 2,4,6-Tribromo Aniline from

Aniline

338

44 Preparation of Para Bromo Acetanilide from

Aniline

340

45 Preparation of Acetanilide by Halogenation

(Bromination) Reaction

343

46 Preparartion of meta Di Nitro Benzene from

Nitro Benzene

345

47 Preparation of Benzoic Acid From Benzyl

Chloride by Oxidation Reaction

347

48 Preparation of Benzoic Acid from Alkyl

Benzoate

349

49 Preparation of Salicylic Acid from Alkyl

Salicylate

351

50 Preparation of 1-Phenyl Azo 2-Napthol from

Aniline

353

51 Preparation of Benzil from Benzoin by

Oxidation Reaction

355

52 Preparation of Dibenzal Acetone from

Benzaldehyde

357

53 Preparation of Cinnamic Acid from

Benzaldehyde

359


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54 Preparation of p-Iodo Benzoic Acid from p-

Amino Benzoic Acid

361

55 Preparation of 1,3-Pyrazole 363

56 Preparation of 1,3-Oxazole 364

57 Preparation of Benzimidazole 366

58 Preparation of Benztriazole 368

59 Preparation of 2,3-Diphenyl Quinoxaline 371

60 Preparation of Benzocaine 373

61 Preparation of Phenytoin 376

62 Preparation of Phenothiazine 379

63 Preparation of Barbiturates 382

64 Preparation of Sulphanilamide 386

65 Preparation of 7-Hydroxy, 4-Methyl Coumarin 390

66 Preparation of Chlorobutanol 393

67 Preparation of 2,4,5 Triphenyl Imidazole 396

68 Preparation of Tolbutamide 397

69 Preparation of Hexamine 400

70 Assay of Metronidazole 403

71 Assay of Ibuprofen 408

72 Assay of Furosemide Assay of Chloroquine 410

73 Assay of Atropine 411

74 Assay of Dapsone 413

75 Assay of Isonicotinic Acid Hydrazide 417

76 Assay of Benzyl Pencillin 421

77 Assay of Chlorphenaramine Melate 422

78 Assay of Phenobarbitone 424

79 Assay of Chlorpromazine 428

80 Assay of Aspirin 432

81 Assay of Chloroquine 433

82 Atomic Mass of 30 Elements 437


xii



1

1. Importance of Wearing White Apron

APRON

A white coat or lab coat (often popular as apron) is a knee-length

overcoat worn by professionals in the medical field or by those

involved in laboratory work. The garment is made from white or

light-colored cotton, linen, or cotton polyester blend, allowing it to

be washed at high temperature and make it easy to see if it is clean.

THE MEANING OF WHITENESS:

White was chosen with good reason as the new standard of the

medical profession. This color, representing purity, is a visual

reminder of the physician’s and pharmacist commitment to do no

harm. White represents goodness and often described as being clad

in white also conveys cleanliness and connotes a purging of

infection. Further, the white coat symbolizes seriousness of

purpose. It communicates the Pharmacist and physician’s medical

intent and serves as a symbolic barrier that maintains the

professional distance between physician, pharmacist and patient.

Perhaps most importantly, the white coat is a garment

of compassion. The white coat reminds physicians and pharmacists


https://drdipendrapandey.files.wordpress.com/2013/07/1273148196_91980460_2-corporate-wear-doctors-apron-safety-jacket-and-t-shirt-thanesar-1273148196.jpg


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of their professional duties, as prescribed by Hippocrates, to lead

their lives and practice their art in uprightness and honor.

An international survey about the causes for wearing white

apron by doctors, pharmacist showed the following result:

Faster recognition by patients, nurses and other doctors, 25

percent.

Large pockets for carrying items such as stethoscopes, 23 percent.

Protecting clothes from being soiled, 15 percent.

Emphasis on status as physician, 7 percent.

Following social expectations for doctors, 7 percent.

Protecting self against contamination from surroundings and

patients, 5 percent.

Exuding an impression of cleanliness, 5 percent.

Protecting patients against contamination from self, 3 percent.

Maintaining warm body temperature in often chilly hospitals, 3

percent.

Erecting a psychological barrier and thereby not easily accessible,

1 percent.

Other reasons, 6 percent



3

2. LABORATORY RULES AND SAFETY

Chemistry wet laboratories contain certain inherent dangers and

hazards. As a chemistry student working in a laboratory, you must

learn how to work safely with these hazards in order to prevent

injury to yourself and others around you. You must make a

constant effort to think about the potential hazards associated with

what you are doing, and to think about how to work safely to

prevent or minimize these hazards as much as possible. The

following guidelines are here to help you. Please understand and

follow these guidelines and act according to the principles behind

them to help everybody to be as safe as possible. Ultimately, your

own safety is your own responsibility. Please make sure you are

familiar with the safety precautions, hazard warnings and

procedures of the experiment you are performing on a given day

before you start any work. If you are unsure of how to do

something safely, please ask the TA before proceeding.

Experiments should not be performed without an instructor in

attendance and must not be left unattended while in progress. No

unauthorized experiments are allowed. No modification of the

experiments is allowed. No work outside of regular hours is

allowed, except under exceptional circumstances.

The Equipment You Will Encounter and Their Functions

Safety goggles and safety equipment


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