Introduction to Instrumental Methods of Analysis

CHE-309 Spring 2003

Instructor: Dr. J. Mullin Phone: x2538

Office: Decary 347; Lab: Alfond 339/340 E-mail:

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Philosophy: This course will present you not only with a clear description of the principles, applications, and operation of selected, important instrumental analytical techniques, but also will encourage you to learn to think and solve challenging, new problems involving the applications of analytical chemistry in a variety of fields which depend on the accurate measurement of chemical composition. To this end, you will be expected to be fairly independent and creative. In a course at this level you will be expected to carry out reading and problem assignments on your own, in a timely fashion, and to be well-prepared for class and especially for laboratory. You also will be expected to acquire both teamwork and management skills that will be important to you in professional settings later on. This course should provide a good opportunity for you to apply some of the chemical knowledge you have accumulated.

Texts: The basic course text will be Principles of Instrumental Analysis, 5th Ed. (Saunders, 1997), by  Skoog, Holler and Nieman. A very useful reference will be Harris, Quantitative Chemical Analysis, 6th Ed. (Freeman, 2003), from which frequent reading assignments will be made (everyone should have a copy from CHE-307). While this book covers a great deal of the material we will explore and is well-written, it is not truly an Instrumental Analysis text, and therefore is incomplete. Some of its descriptions lack sufficient depth, and some material is not included at all (e.g., electronics), yet it serves as good introductory reading for many techniques.

Class Time: T & Th 8:00-9:20 a.m., Marcil 217. Attendance will be taken, but will not be figured directly into your grade, unless there are excessive (>4) absences. Please note that in this course, much of what will be discussed in lecture will not be available in the course texts, so attendance is recommended very strongly.

Communication: Electronic mail will be used extensively for outside-of-class communication between students and the instructor and between student lab partners. It is essential that you check your e-mail account regularly (e.g., daily) so you do not miss important announcements, assignments, etc. Failure to check your e-mail will not be an acceptable excuse for missing deadlines, announcements, assignments, etc.

Exams: Three "regular-season" exams will be given, as well as a comprehensive final. Please note that make-up exams will NOT be given, so be sure you don't miss exams. If there is a serious problem, make sure you contact the Fearless Leader in advance. Exam questions may be drawn from material discussed in class, material in assigned readings (whether discussed in class or not), and any laboratory experiments completed by all prior to the test date. Topics outlines will be provided in advance of all exams.

Office Hours: A schedule will be posted outside Decary 347 and Alfond 340, but you may stop in anytime or set up an appointment. Most weeks, an open lab will be held Thursdays, 2:00 - 5:00 p.m, should extra lab time be desired.

Homework Problems: Homework problems will be assigned regularly, and sometimes will be collected and graded. You are encouraged to work on the problems regularly; don't leave them until the night before an exam.

Course Prerequisite: This course carries a prerequisite of CHE-307 (Quantitative Analysis). It is expected that you are familiar with topics such as the statistical treatment of analytical data and chemical equilibrium.

Literature Assignments: Each month you will be required to read and submit a written summary of an article from the current or a recent (within two years) issue of the journal Analytical Chemistry. These reviews will be due on the 30th of each month (starting with January). Details will be given in class. They are to be submitted electronically as WordPerfect or MS Word files. The journal is available in the UNE Library. Individual issues also may be borrowed from the instructor.

Oral Presentation: Each student will present a 20 minute talk, mostly likely during the last scheduled lab period on May 6. The talk essentially will be an extended report on one of the experiments performed during the semester, presented to be understandable to students who have not taken this course. Details will be provided in class.

Computer Use: You will be expected to use microcomputers for all of your data manipulation, graphing, and report preparation and submission. Quattro Pro, WordPerfect, Excel, and Word are available on the campus network and in the Chemistry labs. ChemDraw (chemical structure drawing package) is available in the Chemistry labs. No formal instruction in the use of application software will be given. See the instructor if you need help.

Evaluation: Course grades will be determined by the total number of points accumulated (on a percentage basis), according to the following tentative distribution:

Exams (3 @100 pts each) 300

Comprehensive Final Exam 150

Literature assignments (4 @ 20 pts) 80

Homework, quizzes & misc. 50

Oral Presentation 80

Lab Reports ~450

Note: This tentative distribution and list of assignments is subject to revision by the Management.

Laboratory Role-playing Model: With the exception of the first three electronics experiments, the laboratory will be run using a role-playing format wherein each student is assigned a specific function determined by the role played during that experiment. The roles, defined as Principle Investigator and Staff Scientist, have carefully structured responsibilities, and the thorough attention to the fulfillment of these responsibilities will have a major impact on both the ease with which you can complete an experiment and the grade you receive for the lab report. The role-playing model is described in more detail in the Laboratory Handbook, and will be discussed in class before the fourth experiment; the goal of this approach is to give valuable insights into the importance of teamwork and experience in the application of good management skills.

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Introduction to Instrumental Methods of Analysis

Course Outline

CHE-309 Spring 2003

Please note: Reading assignments in Skoog/Holler/Nieman (SHN) and Harris are indicated. You are expected to keep up with the assigned reading without constant reminders. Recommended homework problems will be assigned regularly.

I. Introduction; Electronics in Analytical Chemistry

A. Introduction (SHN 1A-1D)

    1. Overview of Instrumental Analytical Methods

    2. The Analytical Process; Data Domains

B. Measurement of Electrical Signals; Definitions (SHN 2A-2B)

C. Basics of Analog Electronics (SHN 2C-2E)

    1. Ohm's Law; circuit diagrams; series and parallel resistors

    2. Kirchoff's laws

    3. Equivalent circuits

    4. Current and potential measuring devices

    5. Voltage dividers

    6. Voltage source loading

    7. Capacitors; RC circuits & filters; noise

    8. Semiconductor devices: diodes and transistors

D. Operational amplifiers in Analytical Instrumentation (SHN 3A-3E)

    1. Op-amp basics

    2. Useful op-amp circuits

E. Introduction to Digital Electronics (SHN 4A-4E)

    1. Digital signal encoding

        a. binary, octal, hexadecimal, BCD

        b. serial/parallel values

    2. Logic gates

    3. Latches & registers

    4. Simple counters

    5. Microcomputer basics; communication with laboratory instruments

II. Instrumental Methods Basics

A. Instrument Response Functions (SHN 5A-5C)

    1. Sensitivity and detection limit

    2. Instrument noise and methods of dealing with it

    3. Interferences (instrumental and chemical)

B. Analytical Calibration Methods (Harris, 5.1 - 5.4)

    1. External standards and blanks; Calibration curves

    2. Internal standards

    3. Standard Additions

    4. Pre-separation and pre-concentration

III. Spectroscopic Methods

A. Electromagnetic Radiation and its Interactions with Matter (Harris, 19.1 - 19.2; 19.5; SHN 6A-6D)

B. Molecular Spectroscopy & Instrumentation: UV-Vis and IR

    1. UV-Vis Absorption (Harris, 19.3-19.4; 20.1-20.3; 21.1-21.7)

        a. origin of the analytical signal (SHN 13A)

        b. instrumentation (SHN 7A-7H; 13A; 13D)

        c. quantitative relationships: Beer's Law (SHN 13B-13C)

        d. applications (SHN 14A-14-D)

    2. Luminescence (Harris, 19.6; 20.6; 21.7)

        a. fluorescence and phosphorescence (SHN 15A)

        b. instrumentation (SHN 15B)

        c. analytical applications (SHN 15C)

        d. chemiluminescence (SHN 15D)

    3. IR Absorption (Harris, 21.8; SHN 7I; 16A-16C)

        a. vibrational spectra

        b. theory and instrumentation for Fourier Transform IR spectroscopy

        c. selected applications (SHN 17A)

    4. Raman Spectroscopy (SHN 18A-18C)

C. Atomic Spectroscopy (Harris, 22.1 - 22.5)

    1. Atomic Absorption, flame and furnace atomization (SHN 9A-9D)

    2. Atomic Emission: Flame, arcs, sparks, & plasmas (SHN 10A-10C)

IV. Chemical Separations

A. Introduction: Phase Equilibria and Extractions (Harris, 23.1)

B. Chromatographic Methods (Harris, 23.2 - 23.5)

    1. Chromatography theories: Plate theory and Rate theory (SHN 26A-26F)

    2. Chromatographic Systems

        a. gas chromatography (Harris, 24.1 - 24.7; SHN 27A-27E)

            i. packed column

            ii. capillary column

            iii. GC-MS (SHN 20A-20E for MS background)

        b. liquid chromatography; HPLC (Harris, 25.1 - 25.4; SHN 28A-28E)

        c. ion exchange; ion chromatography (Harris, 26.1 - 26.2; SHN 28F)

        d. thin layer chromatography (SHN 28H)

        e. size exclusion chromatography (Harris, 26.3; SHN 28G)

        f. supercritical fluid extraction and chromatography (SHN 29A-29C)

        g. capillary electrophoresis (Harris, 26.5; SHN 30A-30C)

V. Electroanalytical Chemistry

A. Basics of Electrochemistry (Harris, 14.1 - 14.6; SHN 22A-22F)

    1. Electrochemical cells

    2. Cell and electrode potentials

    3. The Nernst Equation

B. Potentiometric Methods (Harris, 15.1 - 15.7; SHN 23A-23G)

    1. Reference electrodes

    2. pH electrodes and other ISE's

    3. Instruments for measuring cell potentials

C. Voltammetry (Harris, 18.1 - 18.6; SHN 25A-25F)

    1. polarography

    2. anodic stripping voltammetry

    3. cyclic voltammetry

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Laboratory Policies and Schedule

Laboratory Times and Scheduling: All students will perform the three electronics experiments in self-selected pairs during the regularly scheduled lab period (Tuesdays, 2:30 - 5:20 p.m.). For other experiments, scheduled times will be arranged for each experiment by that experiment's Project Director in consultation with the Captain. Normally, this will be the regularly scheduled lab period for any given week, although occasionally it will be necessary to schedule alternative or additional times by mutual agreement. You sometimes will be required to work in the lab outside of the normally scheduled lab period if you are inefficient or come to lab unprepared. Delays in completing an experiment that result from your mistakes or the need to make minor instrument repairs will not extend lab report deadlines- it is your responsibility to complete the experiment in a timely fashion so that the report may be submitted on time. Please be aware that instrument malfunctions sometimes do occur; while the instructor will make every effort to effect repairs as quickly as possible, some delays may be unavoidable. Remember that typically there will be four different experiments going on simultaneously, but there is only one instructor, and as skilled as he is, he can only be in one place at a time. Since you will be working in groups, you must show up on time and prepared for every lab session, so your partner is not left waiting. It sometimes may be possible to start lab earlier than the scheduled time (e.g., 1:00 p.m.) if this is arranged in advance with the instructor.

Lab Reports: Details on how to prepare lab reports will be provided in class and in the Laboratory Handbook. Except for the Electronics experiments, lab reports are not written and submitted by individuals. Subsequent to the electronics experiments, lab reports are written by the Principle Investigator (PI) and submitted by the group. The Staff Scientist will be responsible for submitting completed calculation spreadsheet files simultaneously to the PI and Instructor no later than the Tuesday following the scheduled lab in which the experiment was scheduled. Lab reports will be due as specified on the back of this sheet (typically the Tuesday two weeks after the experiment is scheduled to be performed). Late lab reports carry a 10% per week late fee. In any case, lab reports will not be accepted after 6:00 p.m. on May 9. Failure to complete all experiments and lab reports will result in automatic course failure. Specific details about the responsibilities of Principle Investigators and Staff Scientists, and on the grading mechanisms to be used, will be supplied in the Laboratory Handbook and discussed in lab.

Safety Glasses: Approved eye protection must be worn at all times in the lab, unless the instructor is lecturing and no lab work is being conducted.

Laboratory Notebooks: You must invest in a bound laboratory notebook (preferably graph-ruled) into which will be entered all raw data, experiment notes and observations, following the rules discussed in class and in the Laboratory Manual. You also may wish to consult Writing the Laboratory Notebook by Howard M. Kanare. It is perfectly acceptable for you to continue to use the lab notebook you used in Quantitative Analysis. Laboratory notebooks occasionally will be inspected, without warning, by the Captain. Poorly kept notebooks not only will make it much more difficult for you to write lab reports, but will result in loss of lab report points if (a) the Captain conducts a random inspection or (b) if the notebook must be consulted as a result of questions generated in reviewing the lab report. No work may be done in the lab (other than washing glassware or drying samples) if you do not have your lab notebook. Scraps or loose sheets of paper never should be used for recording data. Any such papers will be confiscated by the management and will not be returned.

Late Work Penalties:

Late lab reports are subject to a late fee of 10% per week as noted above, and will not be accepted after 6:00 p.m. on May 9. If it's not in on time, points will be deducted unless you have a physician's statement of your incapacitation, at which point appropriate alternative arrangements will be made. Why the draconian approach?

1. The load is constant -- if you fall behind, it's just going to get worse. So at the due date, turn in what you have and keep moving.

2. The instructor has a life outside CHE-309 (well, he doesn't really, but he has other work to do, at least). Everyone comes out ahead if grading activities can be managed with foresight. The instructor will endeavor to return graded lab reports in a timely manner.

3. In The Real World, if it's late, it's useless. You might as well get used to deadlines having consequences.

4. You get no chance for feedback if you hand in all lab reports at the end, thus, diminished opportunity to learn.

5. Since your lab partner's grade will suffer as well as your own, you are responsible for those ramifications.

6. You really do not want to face a frantic end-of-semester rush.

Lab Report Due-date Schedule:

Please note that after the electronics experiments, different groups will be working on different experiments during any given week. Thus, experiments are referred to in this schedule by number, rather than by name. This means that, for example, "The Determination of the pKa of an Acid/base Indicator by UV-Vis Spectrophotometry" may be "Experiment 4" for one group and "Experiment 5" for another group. Also, note the section "Laboratory Times and Schedule" above, and remember that while some experiments may be performed at other times by mutual agreement of all staff and the captain, such adjustments do not change the report due-date.

Lab Day Experiment Report Due

Jan 21 Expt. 1: Basic Electronic Measurements Tues, Jan 28

Jan 28 Expt. 2: Analog Electronics Tues, Feb 4

Feb 4 Expt. 3: Digital Electronics Tues, Feb 11

Feb 11 Experiment 4 Tues, Feb 25

Feb 18 Experiment 5 Tues, Mar 4

Feb 25 Experiment 6 Tues, Mar 11

Mar 4 Experiment 7 Fri, Mar 28

Mar 11 Experiment 8 Tues, Apr 1

Mar 18 Spring Break -----

Mar 25 No Lab (ACS Meeting) -----

Apr 1 Experiment 9 Tues, Apr 15

Apr 8 Experiment 10 Tues, Apr 22

Apr 15 Experiment 11 Tues, Apr 29

Apr 22 Experiment 12 Tues, May 6

Apr 29 Experiment 13 Tues., May 13

May 6 No Lab Experiments (talks)

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