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Introduction & Review Notes Part 2

This document provides an overview of different instrumental methods of pharmaceutical analysis classified based on the chemical reactions involved. The main classifications discussed are neutralization, reduction-oxidation reactions, complexation/compleximetry, and precipitation titrations. Specific examples are given for each method including details about the primary standards, analytes, indicators used, and endpoints. Common techniques like acidimetry, alkalimetry, permanganometry, iodimetry, cerimetry, and argentometric titrations are described.

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Jean Ganub
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62 views1 page

Introduction & Review Notes Part 2

This document provides an overview of different instrumental methods of pharmaceutical analysis classified based on the chemical reactions involved. The main classifications discussed are neutralization, reduction-oxidation reactions, complexation/compleximetry, and precipitation titrations. Specific examples are given for each method including details about the primary standards, analytes, indicators used, and endpoints. Common techniques like acidimetry, alkalimetry, permanganometry, iodimetry, cerimetry, and argentometric titrations are described.

Uploaded by

Jean Ganub
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Pharmaceutical Analysis 2: Instrumental Methods of Analysis

(Review of Analysis 1 and Introduction)

Classifications of Analysis Base on the Reactions Involved

I. Neutralization
A. Acidimetry –measurement of base by a standard acid
Aqueous
Direct Titration: Assay of Sodium bicarbonate (VS: HCl/H2SO4; Primary Standard/Analyte: Na2CO3)
Residual Titration: Assay of ZnO; Assay of Milk of magnesia
Non-aqueous
Direct Titration: Standardization of 0.1N HClO4 (VS: HClO4; Primary Standard/Analyte: Potassium biphthalate)
B. Alkalimetry –measurement of an acid via a standard base
Aqueous
Direct Titration: Assay of Hydrochloric Acid (VS: NaOH; Primary Standard/ Analyte: HCl)
Residual Titration: Assay of Aspirin Capsules
Non-aqueous
Direct Titration: Standardization of 0.1N Sodium Methoxide (VS: Na methoxide; Primary Standard/ Analyte: Benzoic Acid)

II. Reduction-Oxidation Reaction


A. Permanganometry
-involves oxidation process (K permanganate serves as a reducing agent in the process)
VS: KMnO4 Primary standard/ Analyte: Sodium oxalate Indicator: None (VS is self-indicating) Endpoint: Slightly pink
Examples: Direct- Assay of H2O2 Solution, Assay of Cherry Juice for Malic Acid
Residual –Assay of Sodium Nitrate; Standardization of 0.1N Oxalic Acid
B. Iodimetry
-assay for iodine; involves oxidation process (Iodine serves as an oxidizing agent (also the VS) in the process undergoing reduction)
VS: Iodine Solution Primary standard/Analyte: Arsenic trioxide Indicators: Starch T.S.; ChCl3&/ CCl4 Endpoint: Starch-colorless to blue; ChCl3&/ CCl4-colorless to
Purple
Examples: Direct- Assay of Vitamin C; Standardization of 0.1N Iodine Solution;
Residual- Assay of Methionine; Assay of Na bisulfide
C. Iodometry
-assay of oxidizing agent (sample) and iodine serves (VS) as reducing agent (undergoing oxidation process)
VS: Sodium thiosulfate Primary Standard/Analyte: Potassium chromate Indicators: Starch T.S.; ChCl3&/ CCl4 Endpoint: Starch- blue to colorless; ChCl3&/ CCl4-purple to
Colorless
Examples: Direct- Assay of Cupric sulfate; Assay of Sodium hypochlorite Solution
Residual –Assay of Phenol; Assay of Thyroid Hormones
D. Cerimetry
-involves the use of cerium salts
VS: Ceric sulfate Primary standard/Analyte: Arsenic trioxide (new)/ Iron fillings (old) Indicator: Orthophenanthroline Endpoint: blue violet
Examples: Assay of Ferric sulfate tablets

III. Complexation/Compleximetry
-aka “Chelometry”
VS:EDTA(ethylenediaminetetraacetic acid Primary standard/Analyte: CaCO3 Indicator: eriochrome black T- Mg analysis; hydroxynaphthol blue-Ca analysis; Dithiazone-Al analysis
Examples: Direct- Assay of CaCO3
Residual- Bismuth content of glycobiarsol
Special Technique
“Masking” –determination of a metal in the presence of another metal
1. Triethanolamine- Fe3+, Al3+, Mn2+
2. Thioglycols-Ag2+, Cu2+, Bi3+, Pb2+
3. CN-1- Zn2+, Co2+, Ni2+, Cu2+
4. Ammonium F-Mg2+,Al3+, Ca2+

IV. Precipitimetry
-aka Volumetric Precipitation
-most common: Argentometric Titrations
-determination of halides
A. Volhard Method
VS: Ammonium thiocyanate Primary standard/ analyte: Silver nitrate Indicator: Ferric alumn Endpoint: blood red precipitate
B. Mohr Method
VS: Silver nitrate Primary standard/ analyte: NaCl Solution Indicator: K chromate T.S. Endpoint: brick red precipitate
C. Fayan’s Method
VS: Silver nitrate Primary standard/ analyte: NaCl Solution Indicator: Dichlorofluorescein Endpoint: green  pink

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