Advanced Analytical Chemistry The University of Toledo Department of Chemistry and Biochemistry CHEM 4305 001/6300 001/8300 001 Instructor: Emanuela Gionfriddo Email: emanuela.gionfriddo@utoledo.edu Office Hours: M,W,F 3-5 pm or by appointment Office Location: WO 2268 Office Phone: 419-530-1508 Term: Fall Class Location: Memorial Field House 2210 Class Day/Time: T, Th - 2:30 pm - 4:20 pm Credit Hours: 4 COURSE/CATALOG DESCRIPTION The course offers a comprehensive survey of analytical extraction strategies used for the preparation of a variety of samples, such food, environmental and biological matrices, for targeted and non-targeted extraction of analytes (e.g. volatile, semi-volatile, nonvolatile organic compounds, metal ions, DNA, RNA and nucleic acids). Moreover, the course will provide the basics of analytical instrumentation used for qualitative and/or quantitative analysis of analytes using the specified sample preparation strategy. COURSE OVERVIEW The purpose of this course is to present the fundamentals and practical aspects of the most commonly used sample preparation approaches and describe various associated analytical instrumentation. The course is divided into various sections describing sample preparation methods for different types of matrices and targeted analytes. STUDENT LEARNING OUTCOMES The Advanced Analytical Chemistry course is devoted to enhancing the students deeper understanding of both fundamental and practical aspects of sample preparation strategies. After completion of the course the students will be able to: - Classify and describe principles of operation of the most common sample preparation strategies used for analysis of volatile, semi-volatile, non-volatile organic compounds, metal ions, DNA, RNA and nucleic acids. - Critically select the appropriate and best sample preparation method for isolation of a group of targeted analytes from a given matrix and the proper corresponding analytical instrumentation to use for qualitative and/or quantitative analysis. TEACHING STRATEGIES This course consists of in-class lectures. Additional literature and links to online learning tools and videos will be provided to support the course material. Discussion during the in-class lectures is highly encouraged. Some active learning activities likely to involve project work presentations will also be arranged. PREREQUISITES AND COREQUISITES For undergraduate students: Instrumental analysis 1
REQUIRED TEXTS AND ANCILLARY MATERIALS Sample Preparation Techniques in Analytical Chemistry, Somenath Mitra (Editor), 2003, Wiley, ISBN: 978-0-471-32845-2 Additional material will be provided by the instructor during in-class lectures. TECHNOLOGY REQUIREMENTS A laptop computer is recommended for access to online videos and tutorials that support in-class lectures, and for interactive learning activities. For tests and final exam, the use of a scientific calculator is required. UNIVERSITY POLICIES The University is an equal opportunity educational institution. Please read The University s Policy Statement on Nondiscrimination on the Basis of Disability Americans with Disability Act Compliance. Academic Accommodations The University of Toledo is committed to providing equal access to education for all students. If you have a documented disability or you believe you have a disability and would like information regarding academic accommodations/adjustments in this course please contact the Student Disability Services Office. ACADEMIC POLICIES Students are expected to follow the guidelines of student conduct as outlined in the Student Handbook (http://www.utoledo.edu/student affairs/pdfs/studenthandbook.pdf) Academic Dishonesty: The academic honesty policies, as stated in the 2017- UT Catalog will be strictly enforced. Any student found violating the UT academic honesty policies will be penalized in accordance with these policies. COURSE EXPECTATIONS Attendance to the in-class lectures is mandatory. An absence will be excused in accordance with the University Missed Class Policy upon notification to the instructor by email or voicemail prior to the beginning of the class. It is the student s responsibility to independently study the topics covered during the missed class. During the in-class class lectures, with the exception of student s laptop or relevant hardcopy books, usage of all other forms of electronic gadgets is not allowed. The only exception for the use of mobile phone is during some of the interactive learning activities; the instructor will give necessary information/instruction. In case of emergency situations, the students are invited to discuss with the instructor, prior to the beginning of the class, temporary use of mobile phones during the lecture but strictly outside the classroom. Each student found to disturb or interrupt the lecture will be gently invited to leave the classroom with the only purpose of guaranteeing a proper learning experience for other students attending the lecture. The students are highly advised to arrive on time! The student should keep in mind that the course notes have the sole purpose of facilitating the in-class lectures and are not meant to be the sole source of learning material. The textbook and additional material provided by the instructor should be considered as the reference learning material for this course. 2
GRADING Course points: please refer to the following table for the distribution of points that will contribute to the final grade for the course Test #1 Test #2 Final Exam 300 points 300 points 400 points 10 bonus point will be granted after completion of the course evaluation at the end of the semester Final Grading Final grading will be calculated based on the percentage of total points acquired from tests, project work presentation and final exam. Please refer to the following table to relate the calculated percentages to the final grades. A 92% A- 87% B+ 83% B 79% B- 75% C+ 71% C 67% C- 63% D+ 59% D 55% D- 50% F < 50% COMMUNICATION GUIDELINES The students are welcome to communicate with the instructor (by email or appointment, or during office hours) about any aspect of the course, including concerns and factors that might limit student s success. All email communications need to be addressed to Dr. Gionfriddo (emanuela.gionfriddo@utoledo.edu) and contain the course name and student s name in the email object. Emails will generally be answered within 24 hours. STUDENT SUPPORT SERVICES The students are welcome to discuss with the instructor, by email or in person, any concern or support needs. 3
Week #5 Week #4 Week #3 Week #2 Week #1 COURSE SCHEDULE Class schedule Aug 28, Aug 30, Sept 4,6, Sept 11, 13, Sept 18, 20, Sept 25, 27, Topics Introduction to the Advanced Analytical Chemistry course SAMPLE PREPARATION: AN ANALYTICAL PERSPECTIVE The Measurement Process Errors in Quantitative Analysis: Accuracy and Precision Method Performance and Method Validation Preservation of Samples Post-extraction Procedures Quality Assurance and Quality Control during Sample Preparation PRINCIPLES OF EXTRACTION AND THE EXTRACTION OF SEMIVOLATILE ORGANICS FROM LIQUIDS Principles of Extraction Liquid Liquid Extraction Liquid-Solid Extraction Solid-Phase Extraction Solid-Phase Microextraction Stir Bar Sorptive Extraction EXTRACTION OF SEMIVOLATILE ORGANIC COMPOUNDS FROM SOLID MATRICES Soxhlet and Automated Soxhlet Ultrasonic Extraction Supercritical Fluid Extraction Accelerated Solvent Extraction Microwave-Assisted Extraction EXTRACTION OF VOLATILE ORGANIC COMPOUNDS FROM SOLIDS AND LIQUIDS Volatile Organics and Their Analysis Static Headspace Extraction Dynamic Headspace Extraction or Purge and Trap EXTRACTION OF VOLATILE ORGANIC COMPOUNDS FROM SOLIDS AND LIQUIDS (continued) Solid-Phase Microextraction Liquid Liquid Extraction with Large-Volume Injection Membrane Extraction 4
Week #6 Week #7 Oct 2, 4, Oct 9, Oct 11, PREPARATION OF SAMPLES FOR METALS ANALYSIS Wet Digestion Methods Dry Ashing Solid-Phase Extraction for Preconcentration Sample Preparation for Water Samples Precipitation Methods Preparation of Sample Slurries for Direct AAS Analysis Hydride Generation Methods PREPARATION OF SAMPLES FOR METALS ANALYSIS (continued) Colorimetric Methods Metal Speciation Contamination during Metal Analysis Fall Break! Week #8 Oct 16, Test #1 Week #9 Week #10 Oct 18, Oct 23, 25, Oct 30, Nov 1, SAMPLE PREPARATION IN DNA ANALYSIS DNA and Its Structure Isolation of DNA from Bacteria Isolation of Plasmid DNA Genomic DNA Isolation from Yeast DNA from Mammalian Tissues SAMPLE PREPARATION IN DNA ANALYSIS (continued) DNA from Plant Tissue DNA Amplification by Polymerase Chain Reaction Assessment of Quality and Quantitation of DNA SAMPLE PREPARATION IN RNA ANALYSIS RNA: Structure and Properties RNA Isolation: Basic Considerations Phenol Extraction and RNA Recovery Guanidinium Salt Method Isolation of RNA from Nuclear and Cytoplasmic Cellular Fractions 5
Week #14 Week #13 Week #12 Week #11 Nov 6, 8, Nov 13, SAMPLE PREPARATION IN RNA ANALYSIS (continued) Removal of DNA Contamination from RNA Fractionation of RNA Using Chromatography Methods Isolation of RNA from Small Numbers of Cells In Vitro Synthesis of RNA 324 Assessment of Quality and Quantitation of RNA Storage of RNA TECHNIQUES FOR THE EXTRACTION, ISOLATION, AND PURIFICATION OF NUCLEIC ACIDS Methods of Cell Lysis Isolation of Nucleic Acids Chromatographic Methods for the Purification of Nucleic Acids Automated High-Throughput DNA Purification Systems Nov 15, Test #2 Nov 20, TECHNIQUES FOR THE EXTRACTION, ISOLATION, AND PURIFICATION OF NUCLEIC ACIDS (continued) Electrophoretic Separation of Nucleic Acids Capillary Electrophoresis for Sequencing and Sizing Microfabricated Devices for Nucleic Acids Analysis Nov 22, Thanks Giving! Nov 27, 29, SAMPLE PREPARATION FOR MICROSCOPIC AND SPECTROSCOPIC CHARACTERIZATION OF SOLID SURFACES AND FILMS Microscopy of Solids Spectroscopic Techniques for Solids Sample Preparation for Microscopic Evaluation Specimen Thinning for TEM Analysis Sample Preparation for Surface Spectroscopy 6
Week #16 Week #15 Nov 4, 6, SURFACE ENHANCEMENT BY SAMPLE AND SUBSTRATE PREPARATION TECHNIQUES IN RAMAN AND INFRARED SPECTROSCOPY Raman Effect Fundamentals of Surface-Enhanced Raman Spectroscopy Attenuated Total Reflection Infrared Spectroscopy Fundamentals of Surface-Enhanced Infrared Spectroscopy Sample Preparation for SERS Sample Preparation for SEIRA Potential Applications December 11, Final Exam 7