Pharmaceutical Analysis-I (Volume-I : Theory and Practicals)
  by P.C. Kamboj
 
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   ISBN 978-81-85731-89-6; 3rd Ed. 2014; pp.xxii+706

   Delhi price: 350      Outside Delhi price: 370      Overseas price : 1050

 About The Book  


   This volume includes 15 Chapters involving basic pharmacopoeial terms, general instructions, various lab techniques, basic principles, primary chemometrics, qualitative (semimicro) analysis, gravimetry, volumetry (acid-base, non-aqueous, redox, complex and precipitation titrations) and food analysis. The chemistry of chemicals, applications, illustrative diagrams, data tables, solved examples, numerous practical exercises, a large questionnaire, a detailed contents and index alongwith 15 appendices is provided.

 Content


1 Introduction
Sample size
Chemical purity
Pharmacopœia
Pharmacopœial monographs

2 General Instructions & Basic Laboratory Techniques
General instructions
Basic laboratory techniques
Cleaning of glass apparatus
Dilution of concentrated acids
Analytical balance
Weight box, Weighing
Calibration of weights
Quantitative transfer of a substance to a graduated flask
Instruments used for measuring liquids and their Calibration
Desiccators and desiccants
Stirring of liquids
Boiling rods and policeman
Filtration
Distillation
Extraction with a solvent
Crystallization
Experimental techniques in semi-micro procedure
Preparation of the original solution (O.S.) of an inorganic mixture
Spot tests techniques
Determination of melting point
Determination of boiling point
Purification of the solvents
Drying by simple distillation
Preliminary tests for Inorganic substances
Cobalt nitrate test
Flame test
Oxidising fusion mixture test
Borax-bead test
Micro cosmic salt-bead test
Constant Weight of the crucible (in gravimetry)
Evaporation

3 Basic Principles of Chemical Analysis
Polar and non-polar solvents
Acids and bases
Relative strengths of acids and bases
Salts
Law of mass action and its applications
Ostwald's dilution law
Common-ion effect
Solubility product
Application in separation of IInd and IV groups cations
Complex ions
Oxidation and reduction
Oxidation number
Ionic product of water
Hydrogen ion exponent (pH)
Buffer solutions
Hydrolysis of salts
Colloidal state
Peptisation
Flocculation (coagulation)
Adsorption and absorption
Co-precipitation
Post-precipitation
Digestion
Optimum conditions and completeness of precipitation
Characteristics of a substance as a precipitate in the gravimetry
Titrimetric glossary
Strength (concentration) of a solution
Characteristics of a chemical reaction for use in titrimetry
Primary requirements of a titrimetric analysis
Types of reactions used in titrimetric analysis
Primary standards
Secondary standards
Indicators
Acid-base indicators
Precipitation indicators
Redox indicators
Metallochromic indicators
Preparation of a standard solution
Aliquots
Mixed indicators
Neutralisation curves
Polyprotic systems
Preparation of some standard solutions
Recording of observations in titrimetry
Some additional instructions for titrimetric exercises

4 Errors and Computation of Analytical Data
Units and dimensions
Mathematical symbols
Exponents
Extensive, intensive and proper quantities
Dimensional analysis
Logarithm
Atomic masses, the mole and the Avogadro's number
Significant figures
Precision and accuracy
Accuracy
Classification of errors
Minimisation of errors
Testing for significance
Confidence limit
Rejection of a result
How to report analytical data
Statistical parameters and analytical data
Propagation of determinate errors
Propagation of indeterminate errors

5 Systematic Qualitative Analysis (Semi-micro Scale)
Analysis of anions–acid radicals
Group I (dilute H2SO4), Group II (conc. H2SO4), Group III (other anions not covered in gp I and II)
Special tests for combination of anions
Interfering acids and their removal
Analysis of cations–basic radicals
Group I, Group II, Group III, Group IV, Group V, Group VI
Test for NH4+ cation

6 Gravimetry
Precipitation methods
Procedure for gravimetric analysis
Sampling, dissolution, precipitation
Precipitation from homogeneous solution
Digestion and curing
Filtration and washing
Drying of precipitate
Ignition and incineration
Treatement of ash
Gravimetric calculations
Some gravimetric factors
Gravimetric numerical problems
Simple Gravimetric Determinations
Iron (as Fe2O3); Barium (as BaSO4), Sulphate (as BaSO4), Silver (as AgCl), Chloride (as AgCl), Aluminium (as Al2O3), (Aluminium (as oxinate), Lead (as chromate), Calcium (as CaCO3 or CaO), Zinc as (zinc ammonium phosphate or as pyrophosphate), Magnesium (as magnesium ammonium phosphate or pyrophosphate), Magnesium (as oxinate), Water of crystallization (in BaCl2•2H2O), Nickel (as Ni-dimethyl gyoxime chelate), Barium (as chromate), Assay of BaSO4, zinc (as oxide), copper (as cuprous thiocyanate), Gravimetric determinations (summary)
   Amodiaquine hydrochloride as amodiaquine base
   Thiamine hydrochloride as thiamine silicotungstate
   Benzylpenicillin
   Histamine as histamine nitranilic acid complex
   Proguanil as proguanil cupric complex
   Percentage of gold in sodium auriothiomalate
   Caffeine citrate as anhydrous caffeine
   Total alcohol in sodium lauryl sulphate
   Cholesterol (%) as the cholesterol-digitonin complex
Thermogravimetric curves
Organic precipitants (general)
Some important organic precipitants

7 Pharmacopœial Substances and their Titrimetric Assays
Introduction
Acidimetry and alkalimetry
Standardization of acids and bases
Direct titration of weak acids
Special modifications in direct titrations of weak acids
Direct titration of strong acids
Direct titration of strong bases
Special modifications in the direct titration of strong bases
Back titrations
Back titrations with blank determination
Alkalinity of natural waters and is determination
Pharmacopoeial substances (Chemistry) and therapeutical types:
Sodium hydroxide, Alkalisers, Hydrochloric acid, Acidifiers, Sulphuric acid, Astringent, Topical agents, Phosphoric acid, Boric acid, Borax, Sodium bicarobonate, Sodium carbonate, Calcium hydroxide, Ammonia solutions, Calcium carbonate, Ammonium chloride, Expectorant, Magnesium hydroxide

8 Titrations in Non-aqueous Solvents
Introduction
Solvent systems in non-aqueous media
Differentiating and levelling solvents
Dielectric constant
Completeness of the titration reaction
Effects of concentration
Titrants
Effect of temperature on Non-aqueous titrations
Indicators in non-aqueous titrations
Standard 0.1N HClO4 solution
Solvents for nonaqueous titrations
Potentiometric titrations in nonaqueous solvents
Glass electrode, calomel electrode, Silver – silver chloride—reference electrode, Double-junction reference electrode
Preparation of silver–silver chloride electrode
Apparatus and assembly for potentiometric titrations
Standard 0.1 N, 0.05 N, and 0.02 N HClO4 solutions and its standardization with KHP
Preparation of standard 0.1N CH3COONa
solutions and its standardization
Relative concentrations of HClO4 and NaOOCCH3
Determination of the percentage purity of a hyderated sodium acetate sample
Determination of amines
Determination of the % of nitrazepam
Determination of amino acids
Alternative procedure
Determination of phenols
Percentage purity of adrenaline
Titration of halogen salts of organic bases
Determination of benzhexol hydrochloride
Determination of Acidic Substances
Preparation of 0.1 lithium-methoxide
Preparation of 0.1 N CH3OK and its standardisation
Preparation of 0.1 N tetrabutylammonium hydroxide and its standardisation
Determination of amylobarbitone
Determination of phenobarbitone
Determination of sulphonamides
Excipients
Table of non-aqueous analysis of official compounds in IP
(using 0.1N HClO4)

9 Complexation Titrations
Introduction
Chelate effect
Chelating agents
EDTA titrations and equilibria
Significance of ay4 Conditional formation constant
Masking and demasking
Titration curves
Feasibility of complexometric titrations
Types of EDTA titrations
Indicators for complexometric (EDTA) titrations
Preparation and standardisation of sodium EDTA solution
Complexometric Titrations of Some Metals with EDTA
Calcium, Chemistry of calcium chloride, Calcium carbonate, Dibasic calcium phosphate, Tricalcium phosphate, Determination of Ca, in an insoluble salt like phosphate, Calcium gluconate, Dentrifices, Calcium (D in gluconate), Calcium (displacement titration), Chemistry of Magnesium oxides (magnesia), Magnesium hydroxide, Magnesium carbonate, Laxative, Magnesium sulphate, Magmesium chloride, Magnesium (titration), Calcium and magnesium present together (titration)
Total hardness of water
Permanent and temporary hardness of water separately
Magnesium trisilicate
Determination of Mg and SiO2 in magnesium trisilicate
Chemistry of aluminium hydroxide
Aluminium (back tiration)
Chemistry of bismuth subcarbonate, Bismuth subsalicylate, Bismuth subcitrate, Bismuth
Zinc, Chemistry of zinc, Zinc Chloride, Zinc sulphate, Zinc Oxide, Zinc

 
10 Oxidation–Reduction Titrations
Introduction
Nernst equation (electrode potentials)
Standard hydrogen electrode (SHE)
Standard reduction potential
Equilibrium constant of the redox reactions
Some common oxidising agents as titrants
Potassium permanganate, Potassium dichromate, Cerium (IV) sulphate, Potassium bromate, Potassium iodate
Iodine, Iodine solution, Starch indicator, Iodimetric titration, Iodometric titration, Iodimetric determinations, Iodometric determination
Redox indicators
Permanganatometry
KMnO4 (chemistry), 0.1N KMnO4 solution(approximate), Anti infective, Standardization of KMnO4 with: Sodium oxalate, Arsenic(III) oxide,
metallic iron wire, FeSO4•7H2O (chemistry), Hematinic
    Determination of the % purity of a sample of FeSO4.7H2O
    % Iron in the given iron filings
    Calcium in a sample of CaCO3/CaCl2 solution
    H2O2 (Chemistry)
    Strength of commercial H2O2
    % of MnO2 and available oxygen in pyrolusite
    NaNO2 (chemistry), Antidoes
    % Purity of a sample of NaNO2
Chromatometry
    Preparation and standardisation of 0.1N K2Cr2O7 solution
    % Purity of FeSO4.7H2O (External indicator)
    % Purity of FeSO4.7H2O (Internal indicator)
    % Iron in a sample of iron wire
Cerimetry [Ce(IV) solutions]
    Preparation and standardisation of a 0.1N cerium(IV) solution
    With Ferrous ammonium sulphate
    Pure iron wire
    Arsenic(III) oxide
    Oxalic acid/sodium oxalate
    Determination of the % purity of a sample of FeSO4•7H2O
    Total iron contents of an iron wire
    % Purity of a sample of NaNO2
Bromometry (bromate-bromide mixture)
    Determination of As(III) in As2O3
    Determination of the phenol
    Determination of an amino group
Iodatometry
    Potassium iodide (chemistry)
    Standard 0.1N KIO3 solution
    % Iodine in a sample of KI
    Sodium thiosulphate (chemistry)
    Standardisation of sodium thiosulpate
    Potassium antimonyl tartrate (chemistry)
    Emetic
    % Antimony in tartar emetic
Iodimetry
    Preparation of a 0.1N iodine solution
    Standardisation of 0.1N iodine solution against
    (i) As2O3
    (ii) Sodium thiosulphate
    % Purity of As2O3 sample
    % Sb in tartar emetic
    Determination of vitamin C
    Determination of K4[Fe(CN)6]
    Chlorinated lime (chemistry)
    Available chlorine in bleaching powder
    Determination of formaldehyde
Iodometry
    Preparation and standardisation of a 0.1N Na2S2O3.5H2O solution
    With K2Cr2O7
    [CuSO4.5H2O (Chemistry)]
    with CuSO4.5H2O
    Determination of % purity of a sample of CuSO4.5H2O
    Available chlorine in bleaching powder
    Strength of unknown KMnO4 solution
    Determination of dissolved oxygen )DO) in water

11 Precipitation Titrations
Introduction
AgNO3 (Chemistry), Sodium chloride (chemistry), Potassium chloride(chemistry), Potassium bromide (chemistry)
Standard solutions of substances used in precipitation titrations
Standardisation of AgNO3 with KCNS
Mohr's method
Fajan's method
Volhard's method
Determination of the amount of NaCl in a given sample
Mohr's method
Fajan's method
Volhard's method
Determination of HCl content of commercial conc. HCl
Volhard's method
Determination of bromides and iodides
Volhard's method
% Purity of a sample of KCl
Fajan's method
% Composition of a mixture of NaCl and KCl
Mohr's method
% Purity of a sample of KI
Volhard's method
Determination of the amount of HCl and HNO3 present in the mixture,
Mohr's method
Mercurous Perchlorate Solutions
Determination of chlorides and bromides
List of some drugs assayed by precipitation titrations

12. Miscellaneous Titrations
Determination of vitamin C using 2,6-dichloroindophenol
Determination of chloride concentration of a given sample of water/waste water
Determination of chloride in NH4Cl and BaCl2.2H2O separately
Liebig's titration of cyanide with silver nitrate
Determination of chloramine-T, iodometrically
Mercurometric titrations
Yellow mercuric oxide

13. Solvent Extraction Methods
Introduction
Nernst distribution law
Distribution coefficient
Distribution ratio
Solvent extraction systems
Mechansim of extraction
Extraction by chelation
Extraction by solvent
Techniques of extraction
Counter-current extraction
Extraction by ion-pair formation
Solid-liquid extraction
Dithizone method (determination of lead)

14. Miscellaneous Determinations
Determinations with titanous salts
Determination of iron in an iron ore
Determination of a nitro compound
Oxygen-flask method
Determination of individual element
Estimation of nitrogen (Kjeldahl method)
Estimation of sulphur (Messenger;s method)
Karl Fischer reagent (determination of moisture and water)
Aquametry
Alcohol content in liquid galenicals
Diazotization (or Nitrite) titrations
Determination of nitrates
Rast's camphor method (determination of mol.wt.)

15. Food Analysis
Introduction
Analysis of moisture in various foods
Moisture in butter and ghee
Moisture in vegetables oils
Moisture in honey
Moisture in spices and condiments
Dry ashing
Ash of honey
Ash of spices
Analysis of fat in butter
Analysis of protein (in milk)
Analysis of crude fibres in spices
Analysis of starch contents
Adulterants in food
Detection of adulteration of
Vanaspatic ghee in desi ghee
Invert sugar in honey
Tea seed oil in vegetable oil
Coal tar dyes in food stuffs
Rhodamine B colour in chilly powder
Lead Chromate in turmeric powder

APPENDICES

I Atomic weights of the elements (1989)
II Table of formula weights
III Reagents
IV Acidity constants for aqueous solution at 298K in order of acid strength
V Standard potentials at 298K in electrochemical order
VI Table-A : Acid-base indicators
     Table-B : Indicators and their preparation
VII Weights of some substances to be dissolved in 1 dm3 to get 0.25 g and 0.3 g of the weighed precipitate in gravimetry
VIII Molecular weights, equivalent weights and weights of some substances for preparing 1 dm3 solution
IX Some physical constants
     Table-A : Absolute density of water, maximum density is at 3.98°C, the value being 0.999973 (C.G.S.)
     Table-B : Some physical constants of water at different temperatures
     Table-C : Dielectric constants of some liquids
X First-aid in laboratory
XI Greek alphabet
     International system of units (SI, Systeme International)
     SI derivative units, SI prefixes
XII Water as solvent and vehicle
XIII List of Common Apparatus
XIV List of Semimicro Apparatus
XV Logarithms and antilogarithms tables