Instrumental Analysis
CHEM 4100: Fall 2021
Instructors:
Dr. Scott Russell, N365,664-6870, (Office Hours: TR 5:00-6:30pm in via zoom)
Dr. Koni Stone, N358, 667-3570, Office Hours: by appointment, see Canvas to sign up)
Email is the best way to get a hold of us, go to canvas home page for our email addresses. When sending email, please put CHEM 4100 in the subject line.
Text:
Optional: Douglas A. Skoog, F. James Holler, Timothy A. Nieman
Principles of Instrumental Analysis
6th Edition © 2007
ISBN: 13: 978-0-495-01201-6
or
Douglas A. Skoog, F. James Holler, Stanley R. Crouch, Principles of Instrumental Analysis
7th edition, © 2018
ISBN-13: 9780357709276 Ebook = $31.49
ISBN-13: 9781305577213. Hardcove = 159.95
Grades:
| Assessement Device | points | total points | Dates |
|---|---|---|---|
| Exams | 3 x 100 points each | 300 | September 17, October 26, December 9 |
| Lab reports | 5 x 40 points each | 200 | See Canvas for dates |
| GRFP proposal | 20, 20, 60 | 100 | Sept 13, Sept 27, Oct 11 |
| Presentations: Build a spectrophotometer (Guidelines & Rubric), GRFP research proposal | 100 | 200 | Sept 30 and December 15, 11:00 am - 1:50 pm |
Grades are assigned with the following minimums: A= 90%, B= 80%, C= 70%, D=60%
This is a WP course, thus you must pass the Lab reports and exams with a 70% average, to receive a C and earn WP credit towards graduation. You will receive feedback on your reports that will help you improve your writing.
CHEM 4100 Web Site: http://chem4100.wikidot.com
This site has suggested readings, homework problems, examples of old exams and other useful information. You should check this page on a regular basis. The internet is an excellent source of information for the instruments you will be using. It is highly recommended that you make use of this resource.
Calendar:
The calendar for the class has important due dates and the lecture topics for each lecture class.
coming soon
Exams & Homework:
Homework problems may be assigned but not collected. These questions may come from the textbook or the instructor. Exam questions will be based upon the lectures, laboratory material, and homework problems. Several computer tutorials are also available (IR including Diffuse Reflectance, PMR, CMR, UV-Vis, and Mass Spec.) and will aid in both understanding the background theory and spectral interpretation for these instruments which will tested on the exams.
If you have extenuating circumstances, then please contact one of your instructors as soon as possible to determine an appropriate plan.
Safety:
Normal laboratory safety rules will be followed. These include:
- Appropriate eye protection must be worn whenever working in the lab.
- Appropriate clothing and closed toe shoes must be worn in the lab.
- No smoking, eating, or drinking in the lab.
- Please familiarize yourself with the location of the safety equipment in the laboratory.
- You must complete your work during your regularly scheduled lab period. You may be approved to use an instrument outside of lab time, but you will never be granted time to prepare samples. If you request access to an instrument outside of your lab time, your lab instructor must approve it, and a faculty member must be available to supervise you.
More detailed comments regarding laboratory safety are found here: Laboratory Safety
Instrument Proficiency:
You are required to be certified by the instructor on each instrument before you may use it. You should have a basic background in how to operate the instrument safely and how to obtain useful data from the instrument. After you have read the appropriate background information such as theory from your textbook and the appropriate sections of the instrument manual, and understand the experiment you plan to conduct, you should be able to demonstrate your proficiency with each instrument on the list below. When you are ready, please contact your instructor. You must clear this proficiency check on all of the instruments listed below to pass the class. It is NEVER okay to let someone else run your experiments for you.
Experiments:
The list of experiments for the laboratory portion of the course has a brief description of each experiment and links to pages with more details. Each person will work independently and analyze his/her own samples. Please consult the lecture and lab schedule for the start dates and due dates for each experimental report.
You must properly plan your experiments before coming to the laboratory. Simply reading the procedure will not be enough preparation. Carefully read the experiment and plan your laboratory work in advance to make the best use of the time available. Advanced planning will allow you to begin procedures that require large blocks of time at the beginning of the laboratory period. Also, you must be cleared to use an instrument BEFORE you can begin working on it. Each student must be checked out on an instrument by the instructor before using it. Consult with the instructor before starting an experiment.
Most of the instruments are quite expensive and consequently we only have one of each. This can present availability problems. For this reason, a sign-up sheet will be posted in the laboratory if necessary. Those people signing up for an instrument have it reserved for that time block. As a courtesy to your colleagues, please reserve instruments only for the time you will need them, not while you are preparing solutions, etc. Time limits will be placed on the amount of time you can use the instrument while others are waiting for it.
The unfortunate reality of working with advanced instrumentation is that they tend to break down more often. Aside from your understanding, please aid your instructors in taking good care of the instruments and not abusing them. Maintenance can be extremely time consuming and expensive. This is frustrating for everyone.
Notebook:
A permanently bound notebook will be provided and must be used. You should consecutively number each page and include a table of contents. All data, observations, and conclusions must be recorded directly into the notebook in ink. Do not record raw data on scraps of paper. All work must be dated, and signed by an instructor each day you are in lab. Your notebook record should include:
Purpose: Identify the fundamental scientific reason(s) the experiment is being conducted, and the general type of data that will be collected (instrumentation, components, design, etc.) to address the purpose.
Experimental Section: This section should describe how you obtained the data (and not how you manipulated or interpreted the data). Describe the experimental method that you used, including any unusual circumstances. Anyone following your experimental section should be able to repeat your experiment precisely. It will not suffice to "refer to the hand-out" nor should you copy the hand-out. Use your own words, as there is zero tolerance of plagiarism. Include sample calculations for solution concentrations or other related calculations as well as mass and mole values of quantities used. Report information on instruments used and the source of chemical reagents. Note any warnings from material safety data sheets (MSDS) on particularly dangerous chemicals and attach MSDS copies as an appendix to your report.
Data: Include all data "collected in lab", written in ink, in the notebook. The exceptions are spectra and chromatograms. You may paste those into your notebook in the Results section. You must have your data signed by your instructor on the day that it was collected.
Data analysis: Show all sample calculations, including statistical analysis of your data. Clearly explain what you are calculating and why. This section should be neat, organized and succinct.
Results and Discussion: This section will include your outcomes, expected and unexpected. Calculations of any result from your collected data should be reported here. All results must be introduced in the text and displayed in well organized tables and graphs. Each table and graph should be explained in the text, tell what it is, how you got the results and explain the significance of these results. Explain your results to the reader. Error analysis is important in determining how significant your results are. When appropriate,use error analysis to report the 95% confidence range of your unknown determination; also, use error analysis to determine how many significant figures to report.
Conclusion: Summarize your fundamental results and how they relate to the expected (literature) results. Be sure to include the uncertainty of your final data and report your data with the correct number of significant figures. Also, you must state any unknown numbers in the conclusion. References: Include all sources cited and use the ACS style for citing references.
Labs are due at midnight on the due dates. Late labs are penalized 10% per hour that they are late. (Do not be late.)
1. UV/VIS: Build a spectrometer, analyze an unknown and analyze a data set for a two component mixture.
2. IR:
3. NMR: A complete structural assignment of a compound using NMR data
4. Chromatography:
5. Mass spectrometry: Proteomics and spectral interpretation of small molecules.
GRFP Research Proposal Presentation:
Due: Dec 15th. More details are available as the semester progresses. You will turn in a summary of the project to turnitin.com, on or before the due date.