Department of Chemistry

DEPARTMENT OF CHEMISTRY CCNY

Chem 24300 3DG - Quantitative Analysis SPRING 2008

COURSE SYLLABUS

A: LECTURES

INSTRUCTOR: Professor Teresa J. Bandosz

Office : MR-1316; Telephone: (212) 650-6017;

E-mail: tbandosz@ccny.cuny.edu

CONSULTING HOURS: Tuesday, and Thursday: 11-12 or by appointment.

TEXT BOOK: Analytical Chemistry: An Introduction, 8^th ed. by D.A. Skoog, D. M. West, F. J. Holler and S.R. Crouch (2007) ISBN 0-03-020293-0

PREREQUISITE: General Chemistry 10401

Hours/Credits: 7 hours per week, 3 LECT., 4 LAB - 4 credits

Catalog Description: Volumetric, spectrophotometric and Electrometric analyses

GENERAL OBJECTIVE: This course intends to introduce the bases of analytical chemistry for chemistry and biochemistry majors. The emphasis is put either on understanding the theoretical aspects of quantitative analysis or problem solving skills.

Blackboard website: Please follow CUNY PORTAL at http://portal.cuny.edu/portal/

LEARNING GOALS:

Students should:

· Know the physical bases for analytical methods discussed during the course and understand them

· Be aware of the sources of errors and have knowledge how to avoid them

· Know how to calculate the amount of analyte in the specific application of each method

· Know how to obtain calibration curve and how to use it for an analytical purpose

· Know the criteria, which are used for choosing the methods for a particular analysis.

CONCEPTUAL THINKING OBJECTIVES:

· Reading: cause-effect logic, hypothesis testing, summarizing logic

· Writing: cause-effect links, objective designing, experiment planning

· Data analysis: relevant data sources, data treatment, qualitative and quantitative evaluation, data consistency, error analysis

· Models: cause-effect, correlation, trends

The objectives of this course contribute to the following departmental educational outcomes:

Dept outcome letters

Define the physical and chemical principles of volumetric, gravimetric, electrochemical and basic spectroscopic methods (AA, AE, FTIR).
Identify which analytical method should be used to quantitatively determine certain level of a target analyte in various matrices.
Define the principles and goals of analytical separations including chromatographic techniques ( GC, HPLC),
Understand multiple equilibria in solutions and effectively use chemical equilibrium toward determination of the target analyte conc.
Understand the significance of the random and systematic errors, know the ways to minimize/ avoid them, and use the basic statistical evaluation of errors (standard deviation, variation, t-test, Q-test).
Understand and apply the purpose, principle and significance of calibration techniques for quantitative determination of analyte.
Describe in terms of chemical reactions and equilibrium constants all steps used to quantitatively determine the concentration of analyte
Successfully perform volumetric, gravimetric, spectroscopic and chromatographic determination of the target analyte concentration and evaluate the experimental error.
Write a laboratory report including data and error analysis.

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LEARNING ACTIVITIES:

· Text reading

· Class-time (lecture)

· Hand on experience (laboratory)

· Group discussion

· Computer-aid instruction

· Problem solving (individual)

· Student-instructor consulting

HOME ASSIGNMENT: The course requires extensive reading and understanding of each chapter covered during the lecture. Students are encouraged to solve the problems and find answers to all theoretical questions after each chapter.

QUIZZES: Before each lecture starts the students will be asked to find an answer to one question or solve the problem (5 minute quiz) dealing with the material discussed during the previous lecture. The grading from quizzes will consist of 10% of the total grade.

ATTENDANCE: Students are required to attend all lectures and laboratories. After 3 absences the instructor will ask the Registrar to withdraw the student from the course with WU.

GRADING:

No INCOMPLETE Grade

Final - 30%

Laboratory 30%

Best three scores of the four in class examinations 30%

Quizzes 10%

NO make up exams

Academic integrity: The CCNY policy on academic integrity will be followed. Document is posted on the CCNY website (CUNY policy on academic integrity—link is at the bottom of the home page). Make sure you have read the details regarding plagiarism and  cheating, in case you are not clear about the rules of the college. Cases where academic integrity is compromised will be prosecuted according to these rules.

A: SCHEDULE OF LECTURES

DATE CHAPTERS and High priority areas

Jan 28 5, 6: Introduction, Errors in Chem. Analysis, Random Errors in Analyses

· types of errors

· sources of errors

· standard deviation, variation

Jan 30 7: Application of Statistics to Data Treatment

· t-test

· Q-test

· least square method to derive calibration curve

Feb. 4 11: Titrimetric Methods of Analysis

· the principles of titration (definitions of terms)

· volumetric calculations

Feb. 6 4: Aqueous Solution Chemistry

· chemical equilibria

· solubility product

· common-ion effect

· acid-base dissociation constants

Feb. 11 9: Effects of Electrolytes on Ionic Equilibria

· thermodynamic and concentration based equilibrium constants

· ionic strength (calculations)

· salt effect

· activity and activity coefficient (Debye-Huckel equation)

Feb. 13 10: Application of Equilibrium Calculations to Complex Systems

· steps used for solving complex equilibrium problems

· calculation of solubility using mass balance, charge balance and equilibrium constants

· separation of ions by precipitation

Feb. 20 EXAMINATION 1

Feb. 25 12: Theory of Neutralization Titration

· how an indicator work

· calculations of titration curves for strong acids and strong bases and vice versa

· definition of buffers, their preparation and basic calculations (pH, volumes)

· titration curves for weak acids with strong bases or weak bases with strong acids

Feb. 27 13: Titration Curves for Complex Acid/Base Systems

· titration curves for mixtures of strong and weak acids (strong and weak bases)

· buffers based on polyfunctional species

· titration curves for polyfunctional acids with understanding of the mechanism of the processes in each pH range

March 3 14: Application of Neutralization Titration

· standards and standardization

· carbonates and carbonate mixtures

March 5 15: Precipitation Titrimetry;: Complex Formation Titration

· titration curves in precipitation titration (for individual ions and mixtures)

· definition of terms in complex formation titration

· form of EDTA in solution and their properties

· calculations of the metal concentration based on EDTA titration

March 10 EXAMINATION 2

March 12 16: Introduction to Electrochemistry

· redox reactions (balance, oxidant, reductant)

· schematic representation of the electrochemical cell

· electrode potentials (standard electrode potential)

· electrolytic and galvanic cells

· Nerst equation

March 17 17: Application of Standard Electrode Potential

· thermodynamic potential of the cell and its determination

· calculations of redox equilibrium constants

· redox titration curves and equilibrium point potential

· K constant calculations

March 19 18: Application of Oxidation/Reduction Titration

· standard oxidants and reductants

· their applications

· calculation based on redox reactions

March 24 19: Potentiometry

· reference electrodes

· indicator electrodes

· diagram of glass/calomel cell for the measurement of pH and definition of all potential playing role in the system

· the principle of working of glass membrane electrode

· standard addition method for calculation of ion concentration based on the cell potential

· potentiometric titration

March 26 20: Other electroanalyical methods

· sources of polarization

· potential selectivity in electrolytic methods

· coulometric methods for calculation of the amount of the analyte

· comparison of coulometric and conventional titrations

· volammograms, i_d, E_1/2

· dependence of limiting current on concentration

· calculation of the amount of analyte based on the diffusion current

March 31 EXAMINATION 3

April 2 21: Introduction to Spectrochemical Methods

· properties of electromagnetic radiation

· electromagnetic spectrum

· mechanism of absorption of radiation (atoms and molecules)

· transmitance and absorbance

· Beer Law

April 7 23: Molecular Absorption Spectroscopy

· mechanism of absorption by organic and inorganic molecules

· charge transfer absorption

· characteristics of spectrophotometic methods

· standards addition methods to calculate the concentration of analyte

· principles of photometric titration

April 9 23: IR and atomic spectroscopy

· IR spectroscopy

· calculation of concentration of components of the mixture based on the absorption of radiation

· preparation of samples for measurement

· function of flame

· differences between AAS and AFS

· sources of interferences and how to avoid them

April 14 EXAMINATION 4

April 16 24: Analytical separations

· Filtration

· Distillation

· Ion exchange

April 28 24 F: An Introduction to Chromatographic Methods

· elution in chromatography

· how to increase separation

· partition ratio, capacity factor

· column efficiency: N, H

· column resolution

April 30 25A: Gas-Liquid Chromatography

· main parts of GC

· FIT and TCD

· properties of solid support

· types of columns

May 5 25BC: High Performance Liquid Chromatography

· main parts of LC

· application of liquid chromatography

· normal and reverse phase chromatography

May 7 26A: High Performance Liquid Chromatography

· ion chromatography

· advantages of SFC over HPLC and GC

· comparison of GC and HPLC

May 12 Summary of Analytical Methods

· criteria for choosing an analytical method

· steps in sample preparation

· water in solids

· methods used for the decomposition of samples

May 14.. SUMMARY

FINAL-covers all material

CCNY DEPARTMENT OF CHEMISTRY

Chem 243 SPRING2008

B: LABORATORY

TIME: Monday: 2:00 – 5:50

INSTRUCTOR: TBA

Office: MR-1209

CONSULTING HOURS: Monday 11-12 am

HOME ASSIGNMENT: Before each lab read carefully the experiment description and refer to the chapter in the text book dealing with the particular chemistry content objectives

QUIZZES: Before each laboratory starts the students will be asked to find an answer for one question or solve the problem (15 minute quiz) dealing with the experiment which they are about to do. The grading from quizzes will consist of 10 % of the total laboratory grade.

Student are required to start their laboratory experiments on time

ATTENDANCE:

You are required to come to the lab on time. Attention: their will be a lateness penalty (10 points out of 100) of you show up later than 2:15 p.m. Moreover, if you are late you will not get your quiz points (10%). If you do not show up at all, your grade will be zero

PERFORMANCE:

· Always prepare for the lab, so you can do the experiment efficiently.

· Handle the equipment and chemical with care. Attention: safety glasses must be worn while working with chemicals - you will not be allowed to work if you do not bring them.

· Keep your workplace clean

· Record the measurements, calculations and results in a bind book.

· Before you leave the lab, the instructor should see your results and sign there (you may have to show the original results to the instructor later, so do not lose your notebook). At that time ask any questions you have about carrying out the calculations, doing the report, etc.

REPORT:

The lab report should be typed or hand written legibly on white 8.5 x 11 format paper and handed in to the instructor on week after the experiment. Late reports will not be accepted (no kidding!!!).

The report should include:

· Theoretical part (do not write too much-it should not take more than one page)

· Experimental procedure

· Data analysis: detailed calculations using significant figures and correct units. If there are any graphs, they should also be included in this section. The graph should be done using computer programs. If computer is not available, graphs can be done on an accurate graph paper. In both cases linear regression analysis is to be used to analyze data if linear dependence is expected.

· Discussion: discuss your results and analyze sources of errors that might have occurred during your experiment. Explain how these errors could have been avoided.

· Answer to questions if there were any.

GRADING:

The lab grade carries 30% of the final score. Each experiment is graded on the scale from 0 to 100 points.

GRADING:

Quiz 10%

Performance in the class 10%

Form of the lab report 10%

Calculations 50%

Discussions 20%

To arrange a make-up of the lab a note from a doctor, etc. HAS TO be shown.

SUGGESTED TECHNIQUES:

· Before filling a pipette or burette always rinse it with small portions of solution.

· In reading meters and burettes, be careful to avoid parallax.

· Always read your burette to the second decimal.

· Never weight either a hot or a cold sample

· never put a pipette into a bottle of stock reagents. You can contaminate the solution and ruin every determination made with it. Instead, pour some of the solution into a dry beaker and pipette from the beaker. Discard the residue

· Use graduated cylinder only for measuring approximate volumes

SCHEDULE OF LABORATORY EXERCISES

AND CHEMISTRY CONTENT OBJECTIVES

DATE : Exercise # TOPIC and chemistry content objectives

Jan. 30 1. Introduction to EXcel