CHEM 4553Experiments in the Instrumental Analysis of Organic Compounds
1:20-4:20PM Tu-Th in lab 302 Williams Hall, 108 Choppin and other in instrumental facilities
PROFESSOR: Dr. Kresimir Rupnik (201 Choppin Hall office /lab 302 Williams Hall)
578-2945 205-1353 cell
WEBSITE: Moodle class page link
TEACHINGASSISTANTS: TBA
REFERENCE TEXTS. Your CHEM 1201 and 2001 textbook (–Harris)will be most helpful and needed.Analytical textbooks and web links will be assigned.You will learn how to do literature search and use it in the class NOTE: At the beginning of the semester you MUST FIND PROTOCOLS for your independent project.
HELPFUL WRITING BOOKS (see scientific paper format): ACS.org website, Elements of Style, Strunk and White, ACS Style Guide, Dodd, Editor (check the ACS website: acs.org)Writing the laboratory notebook, Howard M. Kanare
CLASS FORMAT and CxC:This course provides students with hands-on experience with chemical instrumentation, protocols and analytical chemistry (and QA) report writing. The course will also focus on preparing the student to conduct chemical research in various laboratory settings. CxC: The analytical chemistry report work is intimately related to the excellent communication skills. We received the formal recognition of this course as the Communication Intensive by the Communication across the Curriculum Program for writing and oral presentations. You will receive specific instructions related to those requirements. More than 50% of the oral and written reports will be subject to direct CxC procedures, feedback and grading.
TENTATIVE EVALUATION***
Scale
Core labs,4. Reports and Practice* 30%
Midterm (lab #4, Unknowns)10%
Project Proposaland Preparations15%
Project Work and Written Report20%
Project Oral Report15%
Written Final Exam**10%
GRADES: A+ 100 – 97, A 96-93, A- 90-92, B+ 89 – 87, B 86-83, B- 82-80, C+ 79 – 77, C 76-73, C- 72-70, D 69 – 60, F below 59
*The grade includes basic hands–on instrument operation skills based on the training provided in the class.If you need additional help let TA (or me) know before completing the lab assignment.
** Material on the tests, quizzes and final is taken from the work in this semester.
*** IMPORTANT: your lab notebooks are mandatory! They will be used for grading. You MUST have all the DATA recordedand available for inspection at all times!!!Graduate and undergraduate students will be graded on the same scale.At the end of each assignment, it is your responsibility to understand the instrument, data analysis method and the interpretation of your results in all work in this lab. Prerequisites for this class include basic instrumental methods (1212, 2002) and analytical methods (1201/02 and 2001). You may want to review that material before work in this lab.Violation of attendance (more than 3 classes missed), no data available or logged, serious safety violations, serious ethics violations (data manufacturing , etc. ) will bring your grades down or worse.
Remember, you will use very expensive and sophisticated instruments in this laboratory. You must learn (1) how the instruments work, (2) how to use them and (3) how to correct basic failures and how to repair them using the available parts. You must always treat the instruments properly. Abuse of equipment will result in failure of the course. You are responsible for the operation of instruments and you should be able to report the possible failure of an instrument.
ATTENDANCE (report any absence by e-mail)
DURING CORE EXPERIMENTS. Attendance will be taken each day. If you are not here, you will be marked absent and receive a zero for the laboratory notebook report. If absent, you are forbidden to copy your partner's data and turn in a report.Doing so will result in disciplinary action. There is a make-up lab session available if needed.You may be reassigned to another group.
DURING INDEPENDENT PROJECT EXPERIMENTS. You are expected to be in the laboratory at the scheduled time. If you have to leave campus, you must check in with your Teaching Assistant or me before leaving.
EXPERIMENTS:
(1)CORE LABORATORY EXPERIMENTS
The core experiments will provide experience with some of the instruments typically used by professional chemists. The core experiments at the beginning of the semester will help you to establish basic skills necessary for the project experiments. During the core laboratories, you will also learn how to maintain a professional research notebook and write lab reports.
Below is a summary of experiments that will be performed in this lab course. Some may be added or changed. This list may change due to the technical needs and other needs.
Experiment 1 (~100 pts)
High Performance Liquid Chromatographic Separations (training and measurement)
Experiment 2 (~100 pts)
Fluorescence Determination of Quinine in Tonic Water (training and measurement)
Experiment 3 (100 pts)
Flame Atomic Absorption of Metals in Food (training and measurement)
Experiment 4: ( ~points TBD) Protein concentrations etc.
Experiment 5: ( ~points TBD) GCMS analysis of standards
Experiment 6 – MIDTERM (200 pts) (experiments)
Identification of a set of unknown organic compounds using FTIR, GC-MS, and NMR (or additional instruments).
(2)INDEPENDENT PROJECT EXPERIMENTS
The major emphasis of this course is for you to think independently to assess a chemical problem, propose a hypothesis to solve the problem, consult the literature to learn how to conduct experiments that will allow you to prove or disprove your hypothesis, perform experiments carefully, successfully, and safely, and evaluate the results of experiments. It is also an opportunity to apply quality control (QC) standards and practices, much as would be required in professional laboratories to ensure high-quality, accurate and reproducible results. To facilitate this training, your team will be able to choose a project using the techniques which you find most interesting. The list of topics for projects was derived from reading the newspaper, Chemical and Engineering News, and other journals. You probably have questions regarding some chemical topic that is of an analytical nature during your life. This is an opportunity to pursue such a question. In addition to the topics below, we are open to suggestions from you. However, your ideas must not be too grandiose due to the short time available during this semester.
BEFORE starting independent project you will be asked to find a protocol for an ASSIGNED experiment. This and literature search course will give you a better idea about how to start your independent project.
You and your lab partner (if assigned) should discuss the topics that you are considering for your project with the teaching assistants and the professor. YOUR INDEPENDENT RESEARCH TOPIC MUST BE APPROVED BY the PROFESSOR!!!! Once your topic is approved, your team will write a ~five (5) page proposal (not including bibliography) that will outline your proposed project experiments. Include which instruments will be used and how.These completed proposals will be due by the middle of second month (date will be assigned) , giving you about <~ six weeks to construct the proposal and TEST it. It is important that you begin researching this proposal at the beginning of the course, because the proposal and oral and written reports must be complete and they account for 50% of your semester grade! (That means if you do not complete them you can fail the class. )
Previous Topics used for 4553 Analytical Projects. DO NOT COPY PREVIOS WORK! (LSU guide for ethical behavior). This is NOT the list of suggested topics!
1. Plasticizers, antibacterials, and babies, 2. Metals, pots, pans and crystalware, 3. Odor removers and you, 4. Fabrics, plastics and forensics, 5. Cracking catalysts and failure, 6. Artwork, pottery and non-destructive analyses, 7. Herbal remedies and you, 8. Chocolates, 9) Wines, 10) Organic products (chemistry agriculture), 11) makeups, 12) Pharmaceuticals), 13) vitamins, 15) Proteins 16) Plastics and macromolecules everywhere.17) Forensics (drugs, metabolic products, explosives (LIMITED) Etc.
Flow of the Course/tentative schedule
- Safety, assignments, Lab Check-in, introduction with syllabus, group assignments, introduction to instruments, some pretesting
- Literature, library search, assigned protocol searches
- Introduction instrument training
------
3. Completion of hands on instrument operation and adjustment/repair training
4. Core Experiments (Fluorescence, AAS, HPLC, GCMS, FTIR , NMR etc)
------
5. Midterm Lab (Analysis of an unknown compound using FTIR, GC/MS, NMR)
------
5. Discussion of independent proposal with instructor, after preliminary tests
A. Topic pre-approval
B. Submit a list of chemicals or glassware that are needed
C. Write proposal, include a timeline for tasks planned each week
6. Implementation of Proposed Plan
7. A. Written Research Report
B. Oral Research Presentation in Class
YOURWORK MUST BE COMPLETED a WEEK before final /dead week
8. Final
LABORATORY PARTNERS
The core experiments will be done in groups with individual reportsand the midterm will be done individually. The independent proposals will be done in groups with individual reports. Your research partner(s) will be assigned to you the first day of class. You may be moved to another group if you do not keep up. That may influence your grade.
LABORATORY REPORTS MUST BE WRITTEN INDIVIDUALLY. If you do not write your lab reports individually, you will be reported to the Dean of Students Office and your case will be dealt with according to the LSU Code of Student Conduct. Possible penalties for plagiarism include a failing grade for the laboratory exercise, failing grade for the course, and dismissal from the university. The LSU Code of Student Conduct defines plagiarism in Section 5.1.16:
"Plagiarism is defined as the unacknowledged inclusion of someone else's words, structure, ideas, or data. When a student submits work as his/her own that includes the words, structure, ideas, or data of others, the source of this information must be acknowledged through complete, accurate, and specific references, and, if verbatim statements are included, through quotation marks as well. Failure to identify any source (including interviews, surveys, etc.), published in any medium (including on the internet) or unpublished, from which words, structure, ideas, or data have been taken, constitutes plagiarism."
*** LSU websites
LABORATORY PREPARATION – “Check-in”
You must prepare to do the experiment before arrival. Review the material contained in the 4553 Laboratory manual, appropriate reference books and primary literature sources that you obtain yourself, and the specific instructions on operation procedures for the instrument to be used before the scheduled time of the laboratory. This will be reviewed during "check-in" time. In addition, your notebook and your work area must be inspected before departure during "check-out” time. Failure to participate in the check-in and check-out procedures will result in a grade of zero for the particular core laboratory write-up, or loss of credit on your project report.
SAFETY
Wear safety glasses at all times in the laboratory. You are not permitted to wear contact lenses in this laboratory. If you have eyeglasses, you may wear them instead of safety glasses if they conform to good laboratory practice protocols. If you are found without protective eyewear three times during the semester, you will receive a grade of F for the entire course. No open-toe shoes, shorts, or tank tops are allowed.Long sleeves, pants and shirts are mandatory. Also, no eating, drinking, or smoking is allowed in the laboratory at any time - this includes chewing gum and the use of smokeless or regular tobacco products. Never work in the laboratory unless a TA or professor is present. You may not "come and go" either . Violation of any of these rules will result in serious consequences that will be decided on a case-by-case basis.
IMPORTANT: After the completion of Safety Introduction you MUST sign the SAFETY FORM and date it. DO NOT continue work before you sign that form.
LIBRARY RESOURCES
Due to the heavy requirement for library work associated with this laboratory, you must be familiar with the SciFinder, Sadtler index, Chemical Abstracts, and other reference material. There are a number of journals which publish general reviews periodically pertaining to specific topics in chemistry. A good example is the Fundamental Reviews in Analytical Chemistry which is published every two years. The library staff can be of great assistance in helping you find what you need. You will attend a training course in the Library.
THE LABORATORY NOTEBOOK and your MANUALS
1. The experimental procedures, your manuals (where needed or assigned) and data must be neatly and concisely recorded in black ink in a scientific notebook. You must use a black, permanent ink, ball-point pen. Do not record data on loose pieces of paper. You must have a Table of Contents in your notebook; allow 4 pages for this at the beginning of the notebook. You can use electronic notebook with dated files.
2. Spectra, chromatograms, and other data from computers should be neatly attached to pages of your notebook (using glue or similar) or insert the electronic image into the electronic file-report. Keep in mind, the ability to write a good report will depend upon how well you organize data in the notebook. The teaching assistants or professor will check your notebook to make sure the data are entered properly and that your notebook shows professional quality work. Failure to maintain a proper notebook will result in serious consequences.
3. Unknowns will be given to you for some experiments. Make sure when you are given an unknown that you record the identifying number in your notebook and clearly state the unknown number on the front page of the laboratory report. Failure to do so in either case will result in a grade of zero for the laboratory report. (There is no other way to do it.)
4. At the beginning of the laboratory period you must provide a procedure for the laboratory experiment of the day that describes how you will do the experiment (written in your laboratory notebook). You must also understand how the instrument works, know how it is operated and how to fix problems that appear when instrument is used. The procedure should be detailed enough to allow you to carry out the procedure without referring to the 4553 Laboratory Manual or other literature. In addition, you must obtain information from a materials safety data sheet (MSDS) for the chemicals that you will use in the experiment from sources such as the internet or the chemical library. Any special handling techniques, precautions, incompatibilities, or waste disposal issues must be noted in the procedure. Any additional questions you have regarding the procedure must be directed to the teaching assistants before/ during the laboratory period. You also should have written out in your notebook procedure the chemical structures of all chemicals to be used in the experiment, noting their chemical characteristics that you might need for the experiment.
The teaching assistants will check everyone's notebooks at the beginning of the class period for the procedure. If it is not present or is incomplete, you will receive a grade of zero for the laboratory report and will be sent away. We will call this checking of notebooks the "check-in."
5. At the end of the laboratory period, you must find the teaching assistant and have them sign and date your notebook at the point you stopped for that period. Data acquired manually must be recorded in the notebook. This will ensure your keeping up the notebook on a daily basis and should help you obtain a good grade for the notebook portion of your course grade. In addition, your work area will be checked to make sure that you have cleaned the lab bench areas. If you do not have your notebook "checked out" you will receive a zero for the laboratory report.
TENTATIVE GRADING FOR LABORATORY NOTEBOOKS
The following section describes the assignment of points and the format for written lab reports. Also included are important points and concepts that should be included in each section of the write-up. You must use the following format. All sections must be included in the write-up or you will lose points.
- General Information /Purpose/Introduction/Theory Mandatory (~5 pts)
- Instrument use (~15 points)
- Experimental Procedure(~10 points)
- Data and Results (~30 points)
- Discussion and Analysis of Results and Questions (~30 points)
- Bibliography (~Mandatory)
- Additional Questions (~10 pts)Total – 100 pts
FORMAT (NOTE – points are not strictly assigned, they provide a general guideline)
General Writing Aspects
Technical writing demonstrates your scientific and literary proficiency. Consult The ACS Style Guide, The Elements of Style, and a dictionary as needed. Use the standard ACS format for citing references. The report here is focused on experimental results, not on the broader theory.
1. General Information Mandatory (5 pts)
Title of experiment
Date experiment started (As noted by teaching assistant)
Date experiment completed (As noted by teaching assistant)
Date write-up completed
