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Lecture Notes and Other Resources

CHEM2041 - Chemical and Spectroscopic Analysis

Files for Downloading

All downloadable files are available from this web page.

Overview

The following notes are extracted from the laboratory manual. The manual contains more information.

Description

Subject Coordinator: Dr J. Justin Gooding
UOC6 S1 HPW6
Prerequisites: CHEM1011 or CHEM1031, and CHEM1021 or CHEM1041; MATH1021 or MATH1231 or MATH1241 or MATH1031
Note: Excluded CHEM2849

The CHEM 2041 course is an introductory course in Analytical Chemistry. The course covers spectroscopy and the analytical applications of spectroscopic methods; the application of equilibrium calculations to analytical problems concerned with the isolation/separation and quantitative analysis of components of mixtures; and the theory and practice of electrochemical potentiometric analysis. The course also includes the statistical analysis of data.

CHEM 2041 is offered in Session 1 for chemistry majors. CHEM 2849 is offered in Session 2 and is designed for servicing students from a range of courses. At present the two courses are very similar. Any variation in the course as presented in the manual will be clearly explained at the beginning of the session.

A substantial part of the course is devoted to practical work in which the student will be expected to carry out real analyses as well as gain a better appreciation of the theory and application of chemical and spectroscopic analysis. In the laboratory, assessment will be based on the quality of analytical results and on clarity of understanding of the related theory.

A tutorial section has been incorporated in the laboratory manual to help students to master some essential skills in "chemical arithmetic". Your lecturer may use a session as a tutorial and work through some of these problems. We recommend that you attempt these problems during the course of the session.

Towards the end of session, attempting past papers is recommended as a way to prepare for the final examination. The manual contains sufficient past papers for students to attempt under both study and self-imposed exam conditions.

Laboratory Work

Laboratory work for CHEM2041 consists of these experiments:

Introduction to ion exchange, Acid Base titrations, Complexiometric titrations, Determination of fluoride in toothpaste, Spectrophotometric determination of copper in tap water, Spectrophotometric determination of manganese in steel and Determination of vitamin C in citrus juices; Introduction to spectroscopy, Infra-red spectroscopy, Atomic spectroscopy, Magnetic resonance spectroscopy, and Ultraviolet spectrophotometry.

All laboratory classes are in room 132 in the Chemical Sciences Building. Attendance at laboratory classes is compulsory and absences must be satisfactorily accounted for.

Students should consult the schedule displayed in room 101 to ascertain the four week period during which they will be rostered to the Spectroscopy Laboratory.

Syllabus

Data analysis (7 Lectures)

UNCERTAINTY AND ERROR. Random uncertainty and the normal distribution. Mean, median, standard deviation, variance, relative standard deviation (coefficient of variation), degrees of freedom.

STUDENT T DISTRIBUTION. Calculation of confidence intervals.

HYPOTHESIS TESTING. Statistical treatment of outliers; two-group experiments; comparison of two means; paired data tests. Fisher F-test for variances. ANOVA.

CALIBRATION. Linear regression. Detection limits and limit of determination. Analysis by standard addition.

SPREADSHEETS for statistical and chemical calculations.

Chemical and analytical spectroscopy (14 Lectures)

ATOMIC SPECTROSCOPY Atomic spectroscopy; atomic spectra of H, He and alkali metals, spectral series, selection rules. Analytical applications of atomic spectroscopy; Atomic emission spectroscopy. Atomic absorption spectroscopy (AAS), in detail.

MOLECULAR ELECTRONIC SPECTROSCOPY Orbitals and energy levels, electronic transitions and selection rules, vibrational structure. Organic and inorganic chromophores. Typical instrument layouts. Beer Lambert Law; calibration. Fluorescence and phosphorescence; quantitative fluorescence analysis.

INFRARED ABSORPTION SPECTROSCOPY Vibrational energy levels, simple harmonic oscillator model; harmonic vs. anharmonic vibrations; Infra-red spectroscopy, selection rules. Group frequencies and the interpretation of spectra. IR instrumentation, sample handling, analytical applications.

NUCLEAR MAGNETIC RESONANCE Nuclear spin; spin and magnetic quantum numbers; NMR active nuclei and natural abundances. NMR transitions, relaxation. Chemical shift; 13C and 1H NMR. Spin-spin coupling; analysis of simple first order spectra. Introduction to instrumentation, sample handling and applications.

Titrimetric and potentiometric analysis (12 Lectures)

ACID BASE TITRATIONS (Competition for protons) Titration curves and titration feasibility, indicator choice; polyprotic systems and mixtures of acids/bases.

COMPLEXOMETRIC TITRATIONS (Competition for metal ions) Ligands and chelate stability, EDTA titrations, conditional formation constant K'f - feasibility; manipulating K'f for selectivity, indicators.

POTENTIOMETRIC ANALYSIS Survey of electrochemical principles. Nernst equation. Ion selective electrodes and microelectrodes. Ion selective field effect transistors (ISFETs). Gas sensing membrane electrodes. Enzyme electrodes. Measurement of pH by ISE and redox electrodes.

REDOX TITRATIONS (Competition for electrons) monitoring electrode potential, self-indicating redox reagents, redox reagents and applications. Conductiometric titrations.

Separation techniques (9 Lectures)

PHASE EQUILIBRIA: SOLVENT EXTRACTION. Phase equilibria: partition coefficient, distribution ratio, extraction efficiency, extraction of metal complexes.

CHROMATOGRAPHY Overview of chromatography; stationary and mobile phases; column performance and resolution. GC instrumentation : injectors, column ovens, detectors (thermal conductivity, flame ionisation, electron capture) Examples of GC separations.

Assessment - WHAT IS EXPECTED OF YOU

Assessment for CHEM 2041 is based upon written examination (70%), laboratory mark (20%) and laboratory assignment mark (10%).

Marks

Candidates for CHEM 2041 must demonstrate a satisfactory performance in both laboratory work and the written examination. A mark of fifty percent is regarded as the minimum acceptable performance in the laboratory. Students who do not attain this mark in their laboratory work may not be awarded a pass in the subject irrespective of their performance in the examination.

Attendance

Unless a specific exemption is granted by the School, a minimum attendance rate of eighty percent in each component of the course (Lecture, Laboratory and Tutorial) is required before a candidate can be considered for a pass in the subject.

Exemptions

Students who are repeating the subject at the first opportunity may make a case for full or partial laboratory work exemption. If such an exemption is granted by the Course Coordinator, marks for the exempted components will be taken from the best previous attempts. Exemptions must be applied for formally by approaching the Course Coordinator and, if granted, a form stating which exercises have attracted an exemption must accompany the student's record card in the laboratory. Students in this category are advised to keep a copy of this form.

Note: Non-exempt experiments must be completed otherwise laboratory work will be incomplete and a grade of WD may be awarded.

Safety

While in the laboratory students are required to comply with all School and University safety policies. Safety spectacles and covered footwear must be worn. Laboratory coats are strongly recommended. Failure to comply with safety rules (for example by refusing to wear eye protection) will result in access to the laboratory being denied. Demonstrators will advise and remind students of their safety responsibilities.

The laboratory notes for each experiment in the manual contains risk assessment and safety material. Students must read the section carefully before commencing the experiment and refer to it as necessary during the experiment.

Material safety data sheets (MSDS) are available for consultation.

If there is any doubt about safety procedures ask a demonstrator.