A Textbook of Pharmaceutical Analysis
| Author’s Name | Kenneth A. Connors |
| Editions | 3rd edition, 2007 |
| Publishers | Wiley India Edition |
Pharmaceutical Analysis (PCI Books)
| Author’s Name | Dr K. R. Mahadhik, Dr L Sathiyanarayanan |
| Editions | First editions, 2019 |
| Publishers | Nirali Prakashan |
Pharmaceutical Analysis (Volume I)
| Author’s Name | S.K. Bhasin |
| Editions | Latest Edition |
| Publishers | Himalaya Publishing House |
Pharmaceutical Analysis-I (PV Books)
(Strictly as per B Pharmacy 1st Semester Syllabus issued by PCI, New Delhi)
| Author’s Name | Dr Uttam Sing Bhagel, Dr Pragi Arora, Ruchika Kabra, Atamjit Sing |
| Edition | Latest Edition |
| Publishers | Pee Vee (Regd.) |
Pharmaceutical Analysis- A textbook for pharmacy student
| Author’s Name | David G. Watson |
| Edition | Third Edition |
| Publishers | Churchill Livingstone Elsevier |
A Basic Knowledge of Pharmaceutical Analysis
| Author’s Name | Prof. S. Karmakar and Prof. (Dr.) A. Ghosh |
| Editions | Latest Edition |
| Publishers | Pharmamedix India Publication Pvt. Ltd. |
Textbook of Pharmaceutical Analysis
| Author’s Name | Dr S. Ravi Sankar |
| Edition | Fourth Edition |
| Publishers | Rx Publications |
Pharmaceutical Analysis Book Topic-wise Summary
✓ Different Techniques of Analysis
• different techniques for Pharmaceutical Analysis can be classified into two major categories such Qualitative analysis and Quantitative analysis.
• Qualitative analysis involves different test procedures which are designed for the identification of the sample compounds.
• Quantitative analysis involves the quantitative determination of sample compounds.
✓ Methods of Expressing Concentration
• There are various methods for the expression of concentration in pharmaceutical analysis. Some of the methods are here:
• Normality (N): Normality can be defined as the number of equivalents of solute dissolved per litre of solutions.
• Percent Concentration: Solution concentrations are expressed in terms of percentage. The percentage concentration for different solutions is expressed in different ways.
• Molality (m): Molality can be defined as the number of moles of solute present per 1000 gm of solvent.
• Molarity (M): Molarity can be defined as the number of moles of solute present per litre of solutions.
• Formality: When components exist in the ionic form either solution state or solid, the molecular weight is not considered for the solution preparation. Instead of this formula weight is used for the solution preparation and the concentration is expressed as Formality.
✓ Primary and Secondary Standard
• Primary Standard: The substances that can be easily obtained in highly pure and crystalline forms and also used in the preparation of the standard solution are called Primary Standard substances.
Examples: Oxalic Acid, Sodium carbonate
• Secondary Standard: Secondary Standard substances are used for the standardization and whose concentration has been determined by comparison with the Primary Standard substances.
• As the no. of the primary standard is limited, a substance having less but known purity and used in the standardization process is known as Secondary Standard.
✓ Preparation and Standardization of Various Solution
• For the preparation of known quantity standard solutions of standard substances based on the requirements are dissolved into a known amount of water and make up the desired volume.
• examples of such types of compounds are used in the preparation & standardization of the various normal and molar solutions.
- Oxalic Acid
- Sodium Hydroxide
- Potassium Permanganate
- Sulphuric Acid
- Hydrochloric Acid
- Sodium Thiosulphate
- Eric Ammonium Sulphate
✓ Errors
• During the pharmaceutical analysis, the result should be highly accurate and precise. The error happens in this analysis due to various factors.
• Two major types of errors are classified as Absolute error and relative error. Depending upon the nature of errors they can be divided into Determination errors and Indeterminate errors.
✓ Accuracy and Precision
• Accuracy: Accuracy can be defined as the agreement of the experimental value with the true value. It is expressed in terms of errors.
• Precision: Precision can be defined as the degree of agreement between the various results of the same quantity.
✓ Significant Figures
• In Pharmaceutical Analysis it is important to understand the significant figures terms. It can be defined as the no. of digits needed to express the results of the measurements consistent with measured precision.
✓ Limit Tests
• Limit Tests can be defined as semi-quantitative or quantitative tests that are performed to identify and control the small number of impurities that are present with the substance to be analysed.
• During the performing limit test, it is necessary to follow the instructions indicated by the Pharmacopoeia. In the section, we did limit tests for Chloride, Sulphate, Iron, Arsenic, and Heavy Metals.
✓ Acid Base Titrations
• Acid-base titrations also called neutralization titrations. The titrations involve the reaction between the Hydroxynium ion against the Hydroxyl ion.
• Thus, the Acid-base titrations reaction affects the prescribed standard condition of the volumetric titrations. The endpoint is detected by the use of a suitable indicator.
✓ Acid-Base Indicators
• For the explanation of the Acid-base indicators two major theories are discussed below: Oswald Theory and Resonance Theory.
• Oswald Theory: Oswald Theory explains the behaviour of the indicator. According to the theory, the undissociated indicator acid or base has a different colour than its ion.
• Resonance Theory: Resonance theory explains that the Acid-base indicators are used in organic compounds. However, they produced colour in the acid-base medium.
✓ Neutralization Curves
• Neutralization reactions can be defined by closely observing the process of changes in the hydrogen ion concentration during the process of titrations. The pH is the parameter in the neutralization reactions which determines the selection of Indicators by the detection of the endpoint.
✓ Non Aqueous Titration
• When an acid or base is used it should have dissolved in an aqueous medium to achieve the desired concentration. However, water is the most commonly used solvent due to its common availability, solubilizing, low cost etc.
• The reactions where difficulties arise using the water as a solvent, the probable remedy is to replace the water with organic solvents. The titrations carried out omitting the water are called Non-aqueous titrations.
✓ Sodium Benzoate and Ephedrine Hydrochloride
• Sodium Benzoate: The formula of sodium benzoate is C7H5NaO2. These are white crystalline or granular powders with odourless colour.
• Ephedrine Hydrochloride: The molecular formula is C10H15NO, HCl. This is the colourless or white crystalline powder and is affected by light.
✓ Precipitation Titrations
• Combination of anions and cations aqueous solutions formed that precipitates are insoluble ionic solids. However, all the reactions in an aqueous solution aren’t necessary to produce precipitates.
• In precipitation reactions, the intermolecular forces between the molecules of the product are high and solute-solvent forces are replaced by solute-solute forces. This strong attraction makes insoluble precipitates.
✓ Mohr’s Methods
• Mohr’s Methods determine the concentration of chloride ions in the solution by titration with silver nitrate. In this method, the silver nitrate solution is slowly added to the chloride solution to produce silver nitrate precipitates.
✓ Volhard’s Methods
• Volhard’s Methods can determine the concentration of chloride ions in the solution using the back titrations with potassium thiocyanate. Initially, the excess amount of silver nitrate solution is added to the chloride ions solution.
✓ Modified-Volhard Methods
• In Volhard’s Methods, a slight change is done to prevent the interference of the silver chloride with the whole titration process. Hence, it is called modified Volhard’s Methods.
✓ Fajans Methods
• Fajan’ s methods involve the titrations of the chloride ions with the silver ions using adsorption indicators. Fajan introduced precipitation titrations adsorption type indicators which absorb or reabsorb on the surface of the precipitates at the equivalence point and produced a change of colours.
✓ Complexometric Titrations
• In the Complexometric titrations complex are formed. The compound has metals for that analysis this titration is used.
• In these titrations, metal ions accept electrons and the ligand donates them. Ligand Involved at least one lone pair of electrons and co-ordinate linkage with a metal ion to produce the complex.
✓ Masking and Demasking Agents
• Masking Agents: The most important aspect of the Complexometric titrations is adaptability in the estimation of two or more metals in the same solution. This can be done either by the selection of suitable pH at that one metal forms a complex without the involvement of the other metal ion or by use of the suitable Masking agents.
A Masking agent is also called the auxiliary chelating agent or the complexing agent. An example of masking agents is Cyanide ions
• Demasking Agents: Demasking agents is the substance that released the masked metal ion. The cyanide complexes of zinc and cadmium can be demasked by the use of the formaldehyde-acetic acid solution.
✓ Metal Ion Indicators
• Metal Ion Indicators are dyed. It shows colour in the solution depending upon the presence of the metal ion. Reactions with metal ions form colour and with other metal ions, they became colourless or form different colours.
✓ Gravimetry
• Gravimetry involves measurements of the weight of the substances to be analysed from a solution after isolation by precipitating the components as insoluble compounds of the known chemical composition.
• Gravimetric analysis is a quantitative method by weight. From the weight of the compounds the basic calculation to done to the determination of the contents.
✓ Co-Precipitation and Post-precipitation
• Co-Precipitation: co-precipitation means an impurity that is precipitated along with the analyte normally is not expected. This process is called co-precipitation.
• Post-precipitation: When the precipitates are allowed to stand in the presence of mother liquor, another substance will form the precipitates with the precipitating reagent, this is called post-precipitation.
✓ Diazotization Titrations
• Diazotization titrations mean the primary aromatic amines present in the sample react with the sodium nitrite in the presence of acid (HCl) to obtain diazonium salt.
• This method was first discovered in 1853 and this mechanism of reactions was first proposed by Peter Griessin. Initially, this method was applied in the synthetic dye industry.
✓ Redox Titrations
• The chemical reactions involved in the different titrimetry reactions. This reaction is also known as an oxidation-reduction reaction. The reaction is also called Redox titration.
• Oxidation-reduction reaction can be defined as the addition of oxygen or removal of hydrogen or loss of electron during a reaction.
✓ Cerimetry
• Cerimetry titration can be defined as oxidation-reduction titrations involving ceric sulphate as an oxidising agent. Ceric sulphate is a powerful oxidant that can be used in acidic solutions.
✓ Iodimetry
• Iodimetry covers the titrations with the standard solutions of iodine. It deals with the titrations of iodine liberated in chemical reactions. The method of analysis is based on the interconversion of Iodine and Iodide ions.
✓ Iodometry
• Iodometry is used for the determination of the concentration of the oxidising agents through an indirect process involving iodine as the intermediary. In the presence of iodine, Thiosulphate ions oxidise quantitatively with tetrathionate ions.
✓ Bromatometry
• Bromatometry involves the use of bromine in place of iodine as an oxidising agent in the Redox titration. During the reaction either water-insoluble bromine addition products or water-soluble bromine, substitution products are formed.
✓ Dichrometry
• Dichromate titrations with potassium dichromate in acidic solutions are based on the conversion of the dichromate ion-containing hexavalent chromium into the trivalent chromium ions.
✓ Titrations with potassium iodide
• Potassium Iodated AR is used as a primary standard. Titrations in which potassium Iodated is used, Involved the reaction with potassium iodide in an acid solution to liberate Iodine (I2).
✓ Conductometry
• Conductometry is the determination of the conductance of an electrolyte solution using a conductometric. When solutions of the electrolyte are subjected to an electric field, then they conduct electric current by migration of the ions. This conductance process obeys Ohm’s law.
• Conductance is of three types specific conductance, equivalents conductance and molar conductance.
✓ Potentiometry
• Different electrode systems are used in combination with measuring the potential or pH of a solution. A pair of electrodes is commonly required for measurement.
• Two electrodes are the indicator electrode and the reference electrode. For understanding the mechanism you should know about the electrode potential and its measurements also.
✓ Polarography
• Polarography is the study of the current-voltage relationship using the polarographic apparatus. This term is applied to the current-voltage curves when the dropping mercury electrode is used as an indicator electrode.
• Polarography is the essential electrolysis on a micro scale for the solution of the substance in a concentration range of 10-6 to 10-2 M.
✓ ILkovic Equations
• The diffusion current at the DME is known as the ILkovic equation. The equation is id = 607n D1/2 cm2/3 t1/6
Where, id = Average diffusion current during the life of drop, n= Number of electrons Involved in the electrode reaction, D= Diffusion coefficient of the substance, c= Concentration of the substance, m= Rate of mercury flowing through the capillary, t= Drop time in seconds.
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