Dr. Scott Russell, 664-6870, srussell@chem.csustan.edu
Dr. Koni Stone, 667-3570, koni@chem.csustan.edu
When sending electronic mail, please put CHEM 4100 in the subject line, for speedy assistance. When leaving a voice mail message, be sure to clearly state your phone number.
Douglas A. Skoog, F. James Holler, Timothy A. Nieman
Principles
of Instrumental Analysis
5th Edition © 1998
ISBN: 0030020786
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 world wide web is an excellent source of information for the instruments you will be using. It is highly recommended that you make use of this resource.
Grades will be assigned based upon your performance on three
equally-weighted exams and 7 experimental reports and 6 background
reports. Experiment report grades will be based
on the quality of your results as well as the quality of your report
presentation.
| Graded Course Elements | Points for Each | Total |
| Exams (3) | 100 | 300 |
| Experimental Reports (7) | 25 | 175 |
| Background Reports (6) | 25 | 150 |
| General Unknown | 50 | 50 |
| Library Exercise | 25 | 25 |
| Lab notebook maintenance | 25 | 25 |
| Total | 725 |
| Grade | % | Points |
| A | 90 | 652.5 |
| B | 80 | 580 |
| C | 70 | 507.5 |
| D | 60 | 435 |
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. It is definitely to your advantage to complete a lab report before the exam as the process of writing the report helps immensely in pointing out weaknesses in your comprehension of course content. 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.
Normal laboratory safety rules will be followed. These include:
| Appropriate eye protection must be worn whenever working in the lab. Contact lenses are not considered eye protection. These can, in fact, be very dangerous and their use in the laboratory should be avoided. |
| No smoking, eating, or drinking in the lab. |
| If you want to work in the lab at times other than the normal laboratory hours, you must have permission from the instructor beforehand. Generally, this practice is discouraged, but may be necessary to allow equal access to all the instrumentation. |
| Please familiarize yourself with the location of the safety equipment in the laboratory. |
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 the instructor who is responsible for the instrument for clearance. 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!
| Atomic Absorption/Flame Emission Spectrometer (Stone) |
| Fourier Transform Infrared Spectrometer (Stone) |
| Ion Chromatograph, Electrochemical Analyzer & Bromide Electrode (Stone) |
| High Pressure Liquid Chromatograph (Russell) |
| Gas Chromatograph-Mass Spectrometer (Russell) |
| Nuclear Magnetic Resonance Spectrometer (Stone) |
| UV-Visible (Russell) |
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. If you wish to propose other experiments which might be more interesting and consistent with the goals of the course, please feel free to suggest them. 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. Advance 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!
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:
These notebook elements should be used to create the graded Experimental report (discussed below).
You will turn in a report for each experiment on or before the due date. Reports may be submitted electronically. Late reports will be penalized 10% for every day they are late.
Do not expect extensive help the last days before a report is due. Complete the reports in a timely fashion as expected of all professionals. No reports will be graded until all students have turned in that report. Reports must be type-written using a word processor in Analytical Chemistry manuscript style. (The directions to authors are found in the first issue of the journal each year.) All reports should have an abstract, introduction, experimental methods, results & discussion, conclusion, and references sections. Here is a brief summary of what is expected in each section of the experimental reports:
Abstract: A brief overview of the experiment conducted and the significant results obtained (approx. 100 words).
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 interpretted 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.
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. Sheets of rough mathcad calculations are not found in professional journals, so they will not be tolerated in your final reports. However, you can put your Mathcad calculations in your notebook and an appendix to the report. Explain your results to the reader. Error analysis is important in determining how significant your results are. Use error analysis to report the 90% confidence range of your unknown determination; also, use error analysis to determine how many significant figures to report. Do not hand in pages of error analysis with your report, put these pages in your notebook.
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.
Typically, a scientific journal paper will include an introduction or purpose which places the work in context. Reports must be type-written using a word processor in Analytical Chemistry manuscript style. Related research that has been previously reported is often briefly summarized and used to underscore or define the significance of the research being reported. Along this line of thinking, you will be required to write Background Reports for six of the experiments that you conduct this semester. These will be done separately from the actual Experimental Reports and have their own due dates.
Each report should be submitted on or before the due date. Reports may be submitted electronically. Late reports will be penalized 10% for every day the report is late.
A good Background Report will be 2-3 pages (11 point Arial font) long. It will be well organized and free of grammatical, spelling and syntax errors. Each Background Report must provide two primary elements:
(1) A thorough discussion of the background theory describing how an instrument functions including describing the nature of the physical phenomenon and the manner in which the instrument responds to the phenomenon. This will likely come from lecture, your course textbook, and other reference materials. However, you should not simply copy (i.e. Plagiarize) from these sources nor should you quote from them. Part of the intent of this assignment is for you to summarize the information in your own words; If you understand it then you can do this quite readily. This discussion will go well beyond what you would likely encounter in a published journal article introduction, but it has important educational value.
(2) A summary of the literature that relates to the significance and the theoretical basis of the experiment. Find at least one paper in the literature that makes use of this technique (instrumentation) and include a discussion of it (them). Be sure that you are not using the same paper(s) as one of your classmates. There are thousands of examples in the literature, so there is no need to use the same ones. You should provide enough detail that the experiment and its results can be generally understood, but not so exhaustive a report that every nuance of the experiment is detailed. Provide a synopsis of the critical parts of the paper as they apply to your topic. Be sure to cite all references used.
An oral presentation of each General Unknown will take place during the final exam week (times to be announced in lecture). Presentations should be a maximum of 20 minutes in length. Expectations for the presentations will be discussed in class. While you will not write a full length report for this assignment, you will submit a synopsis of the oral presentation with all the supporting data on the day of the presentation.
Your instructors will be inviting other professionals from our academic community. We will help you prepare any materials necessary for your presentation (data viewers, overheads, etc.) but you must ask us well (at least 2 days) in advance.