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Home , Instrumental chemistry

CHEM 300 – Spring 2012

Instrumental and Analytical Methods

Lectures: Monday, Wednesday, Friday 11 – 11:50 AM, Beaven 118

Instructor: Professor Amber Hupp Office: Haberlin 335 Telephone: 508-793-2502 Email: [email protected] Office Hours: Tuesday 1 – 3 PM, Wednesday 1 – 2 PM, Thursday 2 – 3 PM, Friday 2 – 3 PM, or by appointment

Laboratory: Monday 1 – 5 PM OR Tuesday 8 AM – 12 PM, Haberlin 319

Lab Supervisor: Antonet DeSouza-Goding Office: Haberlin 312 Email: [email protected] Office Hours: Monday 9:30 – 10:30 AM, Thursday 1 – 2 PM

Required Course Material: Principles of Instrumental Analysis, 6th Ed., by Skoog, Holler, & Crouch

Chemistry 300 Laboratory Manual (available on Moodle)

Bound laboratory notebook (carbon-less are okay)

USB flash drive (for lab data)

Scientific Calculator (graphing type are okay)

Moodle is accessible from: http://www.holycross.edu/login/

Course goals: This course will focus on key concepts of quantitative and instrumental methods of analysis. Students will learn about molecular and atomic , , separation science, and . Lecture and laboratory work will emphasize major analytical methods of analysis, instrumental design, and some method development. Students will learn how and why instruments are designed to operate according to specific criteria and should be able to make intelligent choices among several possible ways of solving an analytical problem.

Prerequisites: Chemistry 231, Physics 111 or Physics 115 with laboratory (may be co-requisite)

1 Quizzes and Examinations: There will be two quizzes, three hourly examinations, and one final cumulative examination. See attached schedule for dates. Quizzes and exams will focus on lecture material, however, due to the integrated nature of the course, concepts and content from the laboratory portion will be included. Quizzes and exams are equally important, yet generally quizzes will cover a smaller amount of material and be held in a shorter amount of time than exams.

Laboratory: There will be eight laboratory experiments designed to provide comprehensive details concerning instrumental methods of analysis. It is expected that you will come to lab prepared, having read the laboratory experiment, recorded pertinent experimental information, and completed any necessary calculations in your laboratory notebook ahead of time.

Each week, a series of questions regarding the previous weeks lab will be given. The answers to these questions should be typed and are due as a group at the beginning of the lab. Three full laboratory reports will be written throughout the semester, two as a group and one individually. More details concerning these lab reports are located in the Chem 300 Laboratory Manual on Moodle and will be discussed in lab. See attached lab schedule for assignments and due dates.

In the final weeks of the laboratory, an independent laboratory project will be completed. Your group of 2 students will be given a chemical problem and be in charge of determining the proper analytical technique (from data pretreatment to instrumental system to data analysis) to quantitatively analyze your sample. More details about the laboratory project will be given in class during the week of March 12.

The laboratory notebook should be maintained over the course of the semester. To evaluate the notebook, two laboratory notebook quizzes will be given at the mid and end points of the semester during lab time. Guidelines for the lab notebook can be found in the Chem 300 Lab Manual.

Attendance: While attendance at lecture is not required, it is expected. Partial lecture notes will be available on the Moodle course website. However, these notes will contain only an outline with significant graphs, figures, or diagrams, and do not substitute attending lecture. Attendance at all laboratories is required. An unexcused absence from lab will result in receiving a zero for that laboratory, as well as a 10% overall reduction in the laboratory grade. Please contact the instructor regarding any missed laboratories.

2 Missed Assignments: Make-ups for labs and exams will only be allowed with a Dean’s excuse, and must be arranged in advance if possible. If sickness arises, a Dean’s excuse will be required. In this case, please contact the instructor as soon as possible to arrange for a make-up.

Late Policy: All laboratory assignments will be due at the beginning of lab. A penalty of 20% will be assigned for each day (24 hour periods, including weekends) that the assignment is late. After 4 days, no assignment will be accepted, and the student will receive a zero for that assignment.

Re-grading: Please let the instructor know as soon as possible if you would like a re-grade or if your score is incorrect. No re-grades or grade corrections will be allowed more than one week after your assignment is returned to you. Academic Dishonesty: All work submitted for this class must be your own. Any student caught cheating or plagiarizing work will receive a zero for the assignment or for the course, depending on severity of academic dishonesty. In addition, all instances of academic dishonesty will be reported to your Class Dean and put in your file.

Evaluation: Grades will be assigned based on the following scheme:

Quizzes (2) 100 points ~ 12% Hourly Exams (3) 300 points ~ 38% Final Exam 150 points ~ 19% Laboratory 250 points ~ 31%

Total 800 points 100%

3 Tentative Lecture Schedule

Week Date Lecture Topic Other

Jan 25 1 Ch 1 – Basics of Instrumental Analysis Jan 27 Statistics for Jan 30 Propagation of Error, Significant Figures 2 Feb 1 Ch 5 - Noise

Feb 3 Quiz 1 1, stats, 5

Feb 6 Ch 6 – Introduction to Spectroscopy

3 Feb 8 Ch 7 – Components of Optical Instruments Feb 10

Feb 13 Chs 13 & 14 – UV-Vis Spectroscopy

4 Feb 15 Catch-up and Review 1, stats, 5, 6, 7, Feb 17 Exam 1 13, 14 Feb 20 Ch 15 – Luminescence Spectroscopy

5 Feb 22 Ch 16/17 –

Feb 24 Ch 18 –

Feb 27 Ch 8 – Introduction to Atomic Spectroscopy 6 Feb 29

Mar 2 Ch 9 – Atomic Absorption Spectroscopy

Mar 5, 7, 9 No Class – Spring Break

Mar 12 Ch 10 – Atomic Emission Spectroscopy Discuss Lab Projects 7 Mar 14 Catch-up and Review 15, 16, 17, 18, Mar 16 Exam 2 8, 9, 10

4 Week Date Lecture Topic Other

Mar 19 Ch 22 – Introduction to Electrochemistry 8 Mar 21

Mar 23 Ch 23 – Potentiometry

Mar 26 Ch 23 (con’t)

9 Mar 28 Ch 25 –

Mar 30 Quiz 2 22, 23, 25

Apr 2 Ch 26 – Introduction to Separation Science 10 Apr 4

Apr 6 No Class – Easter Break Apr 9 No Class – Easter Break Prelab proposal Apr 11 Ch 26 (con’t) 11 approval due Apr 13 Ch 27 – Gas

Apr 16 Ch 27 (con’t)

12 Apr 18 Ch 28 – Liquid Chromatography Apr 20

Apr 23 Ch 30 – Capillary

13 Apr 25 Catch-up and Review

Apr 27 EXAM 3 – Separation Science 26, 27, 28, 30

Apr 30

14 May 2 Chs 11 & 20 – Mass Spectrometry

May 4

15 May 7 Final Review

5 Laboratory Schedule

What’s Due? When’s it Week Date Laboratory Experiment G = Group due? I = Individual Introduction to Lab and Expectations for Reports 2 Jan 30, 31 Lab 1: UV-Visible Absorbance Spectrometry

3 Feb 6, 7 Lab 1 con’t Full Report (G) Feb 13, 14

Lab 2: Spectrometer Lab questions in 4 Feb 13, 14 Components Feb 13, 14 notebook (I) ** Lab Quiz 1**

3 Week Rotation (3 groups – A, B, C)

Lab 3: Fluorescence (Group A) Typed lab 5 Feb 20, 21 Feb 27, 28 Lab 4: questions (G) Infrared/Raman (Group B)

Lab 5: Atomic Absorption (Group C) Rotation con’t

Lab 3: Group B Typed lab 6 Feb 27, 28 Mar 12, 13 Lab 4: Group C questions (G)

Lab 5: Group A Mar 5, 6 Spring Break – no lab

Rotation con’t

Lab 3: Group C Typed lab 7 Mar 12, 13 Mar 19, 20 Lab 4: Group A questions (G)

Lab 5: Group B

8 Mar 19, 20 Lab 6: Electrochemistry Full Report (I) Mar 26, 27

6 What’s Due? When’s it Week Date Laboratory Experiment (G = Group due? I = Individual) 2 Week Rotation (2 groups – A, B)

Lab 7: Typed lab 9 Mar 26, 27 Apr 2, 3 (Group A) questions (G)

Lab 8: Liquid Chromatography (Group B) Rotation con’t Typed lab 10 Apr 2, 3 Lab 7: Group B Apr 16, 17 questions (G) Lab 8: Group A Apr 9, 10 No lab – Easter Break

Independent Lab Projects – 11 Apr 16, 17 Week 1

** Lab Quiz 2**

Independent Lab Projects – 12 Apr 23, 24 Full Report (G) May 7, 8 Week 2

Apr 30, Independent Lab Projects – 13 May 1 Week 3 (only if needed!)

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