Chemistry 434

Fall 2016

Advanced Analytical Chemistry - Instrumental Methods of Analysis

 

 

Course Organization, Lecture Syllabus and Other Important Information

 

Lectures:	Monday, Wednesday, Friday 1:50 to 2:40 pm
Location:	136 CEM
Recitation:	Friday, 9:10-10:00 AM,  183 CEM Friday, 3:00-3:50 PM,  136 CEM
Course Website:	http://www2.chemistry.msu.edu/courses/cem434/
Required Text:	D.A. Skoog, F.J. Holler and S.R. Crouch, Principles of Instrumental Analysis, 6th Edition, Thomson Brooks/Cole Publishers, 2007.
Instructor:	Professor Greg M. Swain 314 Chemistry Building Tel. 355-9715 x229 Email:  swain@chemistry.msu.edu
Instructor Office Hour:	Wednesday, 1:00 to 2:00 pm, 314 Chemistry, or by appointment.
TA:	Stephen Baumler baumler@chemistry.msu.edu
TA Office Hour:	TBA

                       

                                            

Course Description

This in-depth course covers the design, operational principles and practical application of modern instrumental methods used in chemical analysis. These methods are used in the separation, identification and quantification of the chemical components of natural and artificial materials. Using a combination of problem-based learning approaches, case studies and traditional lectures, the student will develop critical thinking skills in the areas of instrument selection, method development and data interpretation.

 

Course Objectives

·       Understand the basic design and operating principles of some modern instruments used in chemical analysis, specifically separations, optical spectroscopy, electroanalytical methods, material characterization and surface analysis techniques, analytical mass spectrometry and NMR.

·      Understand the basics of experimental design and the use of statistical analysis to evaluate measurement data.

·      Understand how to design experiments using these instruments to solve problems in chemical analysis.

·       Learn how to use databases to search for scientific literature and how to read a scientific paper.

·       Improvement of written communication skills through the preparation of a literature-based research paper on a current topic in analytical chemistry.

·      Improvement of oral communication skills through delivering an oral presentation, as part of a team, on an assigned case study.

 

 

Course Organization

Section A: Foundations (Analytical Chemist’s Toolbox)

Chapter 1	Method selection, detection figures of merit and response calibration
Chapter 5	Instrumental electronics and signal processing
	Experimental design and sample preparation (lecture notes only)
	Statistical data analysis (lecture notes only)

 

Section B: Separations

Chapter 26	Theory of separations
Chapter 27	Gas chromatography (environmental analysis)
Chapter 29	Normal- and reversed-phase liquid chromatography (bioanalysis)
Chapter 30	Capillary electrophoresis (single cell analysis)

 

Section C: Spectroscopy

Chapter 8	Atomic absorption spectroscopy
Chapter 9	Atomic emission spectroscopy – ICP (water quality analysis)
Chapter 13,14	Molecular UV/Vis spectroscopy
Chapter 15	Molecular luminescence spectroscopy (bioanalysis)
Chapter 16, 17	Infrared spectroscopy (forensics)
Chapter 18	Raman spectroscopy (polymer characterization)

 

Section D: Electroanalytical Chemistry

Chapter 23	Potentiometry and probes (biomedical analysis)
Chapter 25	Analytical voltammetry (chemical sensing)

 

Section E: Additional Topics

Chapter 21	Material and surface analysis techniques (polymers and nanoscale materials)
Chapter 20	Advanced topics in mass spectrometry: understanding the experiment (biomolecules)
Chapter 19	Advanced topics in NMR: understanding the experiment (biomolecules)

 

 

Exam Schedule

October 5th	(Exam 1 – in class)
October 31st	(Exam 2 – in class)
November 30th	(Exam 3 – in class)
December 12th	(Final Exam – 12:45-2:45 PM)

                               

Grading

There are a total of 800 points available for this course:

 

Ten weekly quizzes   Given during Recitation	(10 pts. each, 100 points total)
Three 1-h exams worth 100 points each	(300 points total)
Final Exam  Comprehensive	(200 points total)
Term Paper	(100 points total)
Oral presentation	(100 points total)

                                         

                                       

The scale indicated below is based on the number of total points accrued being converted to a percentage of the total points available.  These grade cut-offs are based on historical experience with this course and they may be relaxed by a small amount, at the instructor’s discretion, based on the class exam results.  In no event shall the grade levels be made more stringent than indicated below.

 

 

 

Lecture Schedule

Lecture notes will be posted on the course website.

 

It is expected that the Required Reading for each week will be completed prior to the start of that week’s class. All exams will cover material in the text, some of which may not be extensively discussed in the lectures, case study material, assigned problems and lecture notes!!

 

 

 

 

 

Course Syllabus

  

 

Research Paper

Your first task will be to select a topic of interest to write about. You can get ideas from the literature, for example, a feature article in the journal, Analytical Chemistry, or a related analytical measurement journal. One you have identified a current topic in analytical measurement science, you will need to search the literature for  articles on that topic to use to develop your paper. DO NOT SEARCH GOOGLE!! Search the scientific literature databases (Scifinder, Scopus, Web of Science and or Pubmed) through MSU Libraries for important articles on your topic. The main article for the paper should be one published within the past three years. However, there may be background literature on the topic that dates back more than the three years. Use of this material is fine.

 

After gathering and reading the appropriate literature, you will need to do some critical thinking and write your thesis statement down in one sentence. Your thesis statement is like a declaration of your belief. What is the purpose for the report?  The main portion of your report will consist of arguments to support and defend this belief or position.

 

You will then prepare an outline for the paper and have this reviewed by me before Oct. 3^rd. The purpose of an outline is to help you think through your topic carefully and organize it logically before you start writing. A good outline is the most important step in writing a good paper. The outline should include: (i) Introduction – brief comment leading into the subject matter, (ii) Body of the paper – (a) experimental approach and instrument design, (b) experiments performed, (c) data analysis, and (iii) Conclusions – summary of key points from the main paper.

 

You will then write a 10-page literature-based research paper (Times Roman, 11 point, 1.5 line spacing) on the topic. The paper should utilize at least five references. The term paper should have the following sections: Motivations for the Instrumental Method (what is it good for, what types of analyses are possible, and how does having the method benefit science?), Basics of the Instrument Design and Theory of Operation, Example Data and Interpretation, and Conclusions and Future Prospects. All figures are to be scanned and embedded into the text. All text used in your paper and written by another author should be appropriately cited. All papers are due on or before October 28^th.

 

The term paper should have the following sections:

1)  Motivations for the Instrumental Method (what is it good for, what types of analyses are possible, and how does having the method benefit science?)

2)  Basics of the Instrument Design and Theory of Operation (instrument design and function)

3)  Example Data and Interpretation (at least three pieces of key data)

4)  Conclusions and Future Perspectives

 

All figures are to be embedded (copy and paste) into the text. You can usually copy the figures directly from the pdf version on the journal website. Use the text wrap-around feature. The figures should generally be no more that 3 x 3 in². Any text excerpted from another work should be cited appropriately.

 

Use the following reference or citation format.  J.E. Jones and P. A. Barnum, Anal. Chem. 1997, 75, 206-212.

 

 

 

Presentation (Case Study)

You will be assigned to a group (4 students) and the team will prepare and present a lecture on an assigned case study. The case studies will be assigned by me and are listed on the website. You will discuss the purpose for the work, the design of the instrumental method used and its operational principles, the data presented and the conclusions reached. See the syllabus for your presentation date.

 

Plan the presentation for about 40 min with 10 minutes for questions. This means about 25 slides. The presentation should be organized as follows: (i) describe the chemical problem, why the analysis is needed and the motivation for the work, (ii) present details of the measurement method (how everything is fit together and how it works), (iii) indicate any theoretical principles that relate the instrument/method response to an analyte concentration, (iv) present and discuss the measurements made and the data presented, (v) review the conclusions from the paper and (vi) offer your perspectives about what the future holds for the measurement method and what chemical or biochemical problems it could be used to help solve.

 

As you read through the paper, it may be necessary for you to obtain other literature in order to understand and explain the work presented. This is fine. Also, note that when you find the article on the journal website, there is very often is supplemental information that you should access and use in your presentation. At the end of your presentation, list the citations you used. Your textbook or another textbook could be one of these citations.

 

 

Religious Observances/ Other Absences from Class

It is the responsibility of students who plan to be absent from class at certain times throughout the semester, due to religious holidays or other reasons, to make arrangements in advance with the instructor. Course notes or handouts may be obtained from the instructor if these conditions are met. If a make-up exam is required, the instructor retains the right to determine the content of the exam and the conditions of administration, giving due consideration to equitable treatment.

 

 

Academic Honesty

Academic dishonesty at Michigan State University is defined by the General Student Regulations as conduct that violates the fundamental principles of truth, honesty, and integrity. The following conduct is specifically cited:

 

o    Supplying or using work or answers that are not one's own.

o    Providing or accepting assistance with completing assignments or examinations.

o    Interfering through any means with another's academic work.

o    Faking data or results.

 

You are expected to complete all course assignments, including homework, quizzes, tests and exams, without assistance from any source. You are expected to develop original work for this course; therefore, you may not submit course work you completed for another course to satisfy the requirements for this course.  Also, you are not authorized to use the www.allmsu.com or similar web sites to complete any course work in this course.

 

Students who violate these rules WILL be assigned a failing grade for the course.

 

 

 

Social Media Policy

As members of a learning community, students are expected to respect the intellectual property of course instructors. All course materials presented to students are the copyrighted property of the course instructor and are subject to the following conditions of use:

 

1)  Students may not record lectures or any other classroom activities and use the recordings only for their own    course-related purposes without permission from the instructor.

 

2)  If granted permission, students may share the recordings with other students enrolled in the class. Sharing is limited to using the recordings only for their own course-related purposes.

 

3)  Students may not post the recordings or other course materials online or distribute them to anyone not enrolled in the class without the advance written permission of the course instructor and, if applicable, any students whose voice or image is included in the recordings.

 

4)  Any student violating the conditions described above may face academic disciplinary sanctions.

 

 

Special Requests

 

https://www.rcpd.msu.edu/

 

Michigan State University is committed to providing equal opportunity for participation in all programs, services and activities. Requests for accommodations by persons with disabilities may be made by contacting the Resource Center for Persons with Disabilities at 517-884-RCPD or on the web at the link shown above. Once your eligibility for an accommodation has been determined, you will be issued a verified individual services accommodation (“VISA”) form. Please present this form to me at the start of the term and/or two weeks prior to the accommodation date (first test date). Requests received after this date will be honored whenever possible.

 

 

Lecture Notes

Lecture 1

Extra Lecture 1

Lecture 2

Lecture 3 –Chap 5. Signals and Noise

Lecture 4 – Sample Preparation

 

Chapter 26 – Intro to Separations

Chapter 27 – Gas Chromatography Lecture 1

Chapter 27 – Gas Chromatography Lecture 2

Chapter 28 – Liquid Chromatography Lecture 1

Chapter 28 – Liquid Chromatography Lecture 2

 

Basic Statistics 1

Basic Statistics 2

Supplemental Material from Granger and Granger (Statistics)

 

Chapter 30 – Capillary Electrophoresis

 

Chapter 8 and 9 – Atomic Absorption Spectroscopy

Atomic Absorption Extra Notes

Chapter 10 – Atomic Emission Spectroscopy (ICP)

Chapter 13 & 14 – Molecular Absorption Spectroscopy

Chapter 15 – Molecular Fluorescence Spectroscopy

Chapter 16,17 & 18- IR and Raman Spectroscopy

IR Spectroscopy Summary

Raman Spectroscopy

Chapter 22 – Introduction to Electrochemistry

Chapter 23 - Potentiometry

Chapter 25 - Voltammetry

Chapter 21 – Material Characterization

Statistical Analysis

Chapter 20_Analytical Mass Spectrometry_Lecture1

 

 

Case Study Articles

Group 1	September 16th	Case Study 1
Group 2	September 23th	Case Study 2
Group 3	September 30th	Anal. Chem. 79 (2007) 6903-6911
Group 4	October 14th	Anal. Chem. 88 (2016) 8433-8440
Group 5	October 21st	Anal. Chem. 79 (2007) 4215-4221
Group 6	October 28th	Anal. Chem. 85 (2013) 9469-9477
Group 7	November 11th	Anal. Bioanal. Chem. 387 (2007) 97-105
Group 8	November 18th	Electrochem. Comm. 56 (2015) 6-10
Group 9	December 2nd	Environ. Sci. Technol. 42 (2008) 8841-8848
Group 10	December 9th	Case Study #10

                                                                                                               

Homework  and Quiz Answer Keys and Supplemental Material

Internal Standard and Standard Addition Method Ex

Excel Spreadsheet_mean and variability

Excel Spreadsheet_Linear Regression_LOD

 

Chapter 1 AK                           Quiz 1AK                Exam 1 AK

Chapter 5 AK                            Quiz 2 AK                 Exam 2 AK

Chapter 26 AK                          Quiz 3 AK                 Exam 3 AK                     

Chapter 27 AK                          Quiz 4 AK

Chapter 28 AK                          Quiz 5 AK  

Chapter 8, 9 & 10                      Quiz 6 AK

Chapter 13,14 & 15                   Quiz 7 AK 

Chapter 16                                 Quiz 8 AK

Chapter 22                                 Quiz 9 AK

Chapter 23

Chapter 25