DRUG ANALYSIS I

Alphabetic division AC-DL-MQ-RZ

Course Sheet

Course code:

00011

Academic Year of enrolment:

2020

Year of supply:

2022/2023

Divisions:

Cognomi H-Z

Type of Course:

Characterising

Degree:

Course of Single Cycle Degree 5 years in PHARMACY

Disciplinary Sector:

Pharmaceutical Chemistry

Is part of:

DRUG ANALYSIS I

Location:

CHIETI

Credits:

Programme Year:

Professor and Collaborators:

CAMPESTRE Cristina

Cycle:

First semester

Obligatory attendance:

Yes

Minimum hours of attendance:

Hours of classroom activity:

120

Individual study hours:

205

Prerequisites:

Organic Chemistry
Analytical chemistry and analytical chemistry laboratory

Objectives

The aim of the course is to provide the theoretical and practical knowledge necessary for the quantitative determination of substances of pharmaceutical interest, using both chemical and instrumental methods, reserving particular attention to substances registered in the Official Pharmacopoeia.
At the end of the course the student will be able:
- to work safely in a chemical laboratory
- to understand and correctly apply the analytical procedures for the quantitative determination of substances of pharmaceutical interest, as reported in the Official Pharmacopoeia;
- to carry out in practice the quantitative analysis of substances of pharmaceutical interest, using chemical and/or instrumental methods
- to process the data obtained and critically evaluate the results

Contents

VOLUMETRIC ANALYSIS
- General aspects
- Laboratory equipment, materials and reagents
- Titration methods
- Acid-base titrations in aqueous solution
- Acid-base titrations in non-aqueous medium
- Precipitation titrations
- Complex-formation titrations
- Redox titrations

INSTRUMENTAL ANALYSIS
- Potenziometry
- Conductimetry

LAB PRACTICE SCHEDULE

Extended Syllabus

VOLUMETRIC ANALYSIS

General aspects
Introduction to quantitative pharmaceutical analysis. Classification of analythical methods. Qualitative and quantitative analysis. Sources of impurities in pharmaceutical products. General operations of the quantitative pharmaceutical analysis. Medicines and codes of purity. Italian Official Pharmacopoeia and European Pharmacopoeia.

Laboratory equipment, materials and reagents
Analytical and technical balance. Operations related to weighing. Errors in weighing. Volumetric glassware. Materials and reagents. Safety in the chemical laboratory.

Titration methods
General aspects. Volumetric titration. Reactions in volumetric analysis. Requirements for volumetric analysis. Primary standard and secondary standard. Standard solutions. Calculating the concentration of a standard solution. Equivalence point and end point. Titration curve. Titre of a solution. Equivalent weight. Titration procedure. Calculations in volumetric analysis. Concentration units. Errors in volumetric analysis.

Acid-base titrations in aqueous solution
Aqueous solutions and acid-base equilibria. Strength of acids and bases. pH calculation. Acid-base indicators. Titration curves: strong acids and strong bases, weak acids and weak bases, mixture of two acids, polyprotic acids and polyfunctional bases. Acidimetry and alkalimetry. Examples of acid-base titrations according to E.P.

Acid-base titrations in non-aqueous medium
General aspects. Classification of solvents. Leveling effect and differentiating effect. Autoprotolysis constant. Dielectric constant. Examples of acid-base titrations in non-aqueous medium according to E.P.

Precipitation titrations
General aspects. Solubility and solubility product constant. Titration curves. End point determination. Argentometric methods (Mohr, Fajans, Volhard methods). Examples of precipitation titrations according to E.P.

Complex-formation titrations
General aspects. Titrations with monofunctional ligands. Chelometry: EDTA, pH influence. Conditional formation constant. Titration curves. End-point determination. Selectivity of EDTA titrations: pH, auxiliary complexing agents, masking agents. Metallochromic indicators. Titration methods using EDTA. Examples of complexometric titrations according to E.P.

Redox titrations
General aspects. Scale of redox potentials and Nernst equation. Calculation of cell potential and equlibrium constan. Titration curves, equivalence point potential. Redox indicators. Applications of redox titrations: permanganomety, cerimetry, bichromatometry, iodimetry, iodometry, bromatometry. Examples of redox titrations according to E.P.

INSTRUMENTAL ANALYSIS

Potenziometry
Introduction to electrochemistry. Principle of potentiometer. Reference electrode and indicator electrode. Glass electrode. Potentiometric titrations and end point determination. Examples of potentiometric titrations according to E.P.

Conductimetry
General aspects. Electrical conductivity of solutions. Kohlrausch law. Conductivity measurement. Ionic migration. Conductimetric titrations.

LAB PRACTICE SCHEDULE

- Safety in laboratory.
- Volumetric glassware, analytical and technical balance.
- Preparation and standardization of a HCl solution.
- Acidimetric determinations of some substances according to E.P..
- Preparation and standardization of a NaOH solution.
- Alkalimetric determinations of some substances according to E.P..
- Preparation and standardization of an EDTA solution.
- Complexometric determinations of some substances according to E.P..
- Preparation and standardization of a KMnO4 solution.
- Permanganometric determinations of some substances according to E.P..
- Potentiometric titrations.
- Conductimetric titrations.

Recommended Bibliography

- Holler, Crouch: Fondamenti di Chimica Analitica di Skoog e West, (EdiSes, Napoli);
- Porretta: Analisi di preparazioni farmaceutiche, (CISU, Roma)
- Hage, Carr: Chimica Analitica e Analisi Quantitativa (Piccin, Padova)

Teaching Methods

The course consists of approximately 72 hours of lectures, including numerical exercises, and about 48 hours of single-seat laboratory exercises.
- The lectures provide for the projection of slides, with a detailed explanation of the content, and the carrying out of numerical exercises for each of the topics covered, as well as the resolution of some exam tasks. All supplementary teaching material is available.
- The laboratory exercises are carried out in parallel with the theoretical lessons, so that the student can adequately deal with the experimental experience. The exercises are single-seated, and each student is constantly followed by the teacher for the correct execution of the analysis. Each student is given a "guide to the exercises" paper that shows the individual procedures to be followed for both the volumetric and the instrumental part. The preparation of the titolating reagents, the titrations and the quantitative determinations are carried out individually and the student presents a complete report of the calculations performed to arrive at the final result required.

Evaluation methods

Verification of learning:

The exam includes a written test and a subsequent oral exam.
The written test and the subsequent oral examination have as their object the topics covered during the lessons or laboratory exercises.
The written test, lasting 80 minutes, consists of two numerical exercises, each with at least two questions; the candidate is admitted to the oral examination with a minimum score of 15/30.
The oral exam includes a review of the written test, in which the student is informed about the correction criteria, and subsequently a thorough check of his / her knowledge regarding the teaching topics. The questions can also include the laboratory exercise methods and have the purpose of verifying the mastery of the different topics.
The written and oral tests, both in thirtieths, have equal weight in determining the final grade; the practical skills acquired during laboratory exercises are also evaluated.

Contacts/More Information

The teacher is available every day by appointment requested by e-mail, for clarifications concerning the theoretical and practical part of the course.

Università degli Studi
"G. d'Annunzio"

Chieti - Pescara

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