Experimental Methods in Chemistry
Experimental Methods in Chemistry
5.35
Section 1
1.1 Executive Summary
1.2 Course Policies and Information
1.3 The first and the last day in the
Laboratory
1.4 Grading
1.5 Notebooks and Reports
1.6 Academic Honesty
1.7 Required Books
Section 2
2.1 Introduction
2.2 Safety Training
2.3 Laboratory Safety Equipment
2.4 Safety Rules and Guidelines
2.5 More On Safety in the MIT
Undergraduate Laboratories
2.6 Environmental Consequences of
Laboratory Operations
2.7 Procedures for Handling Hazardous
Chemical Wastes
2.8 Hazardous Materials
2.9 Responsible environmental practices
Section 3
Experimental Modules
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1.1 EXECUTIVE SUMMARY
For most of you, 5.35 will be the first formal laboratory course you will take at M.I.T.
It is the first part of a modular sequence of increasingly sophisticated (and challenging)
laboratory courses required of all Course V majors: 5.35, 5.36, 5.37 and 5.38. The
objectives of 5.35 are:
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1.2 COURSE POLICIES AND INFORMATION
(1) THE UNDERGRADUATE LABS OPEN AT 1:00 p.m. for Chemistry 5.35
students. Students may NOT arrive earlier and may NOT to do any work until his/her
TA is in the lab.
(2) THE UNDERGRADUATE LABS CLOSE AT 5:00 p.m. TAs must remain in the
lab until his/her last student has left for the day.
(3) 5.35 students SCHEDULED for MW Labs CANNOT COME INTO THE TR
Labs TO WORK AT ANY TIME, AND VICE VERSA.
Students who need to work on a scheduled Friday afternoon must see the Lab Director
by 5:00 p.m. on WEDNESDAY AFTERNOON (for MW labs) and on THURSDAY
AFTERNOON (for TR labs).
(5) ANY absences from lab due to illness or other unforeseen emergencies or
circumstances require a note from S^3 sent to the Lab Director. Absences from lab due
to sports or other extracurricular activities need to be discussed with the Lab Director
well ahead of time (1 week MINIMUM). If you have any weekly conflicts with your lab
schedule, the lab takes priority. No accommodations will be made.
(6) At the end of each laboratory day, glassware and equipment must be cleaned and
stored in your desk. Although students do not pay a lab fee, a fee will be charged at the
end of the semester for lost, broken or stolen glassware and equipment.
(7) All requests for an extension of assignment due dates and oral reports in
5.35 should be directed to the Lab Director. Extensions are only given for excused
absences and other crises beyond the reasonable control of students and are solely at
the discretion of the Lab Director.
(8) Please make a special effort to take extremely good care of the balances
and other instrumentation so that they will perform well throughout the semester.
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1.3 FIRST AND LAST DAY OF LAB
A. CHECK-IN PROCEDURE
Your desk assignment will be determined at check-in. At your desk you will find the
following items:
1. Laboratory desk inventory sheets listing the equipment contained in the desk.
2. EH&S CLEARANCE FORM, which must be signed and returned to your TA
during your first work day in the lab.
3. 5.35 Laboratory Manual. Additional copies of the 5.35 Lab Manual may be
purchased from the Chemistry Stockroom
A key for the lock on your assigned desk will be distributed during the afternoon.
Check the equipment in your desk against the inventory; the items in your desk may
not be arranged as outlined on the sheet. For convenience in checking-in and checking-out,
arrange your desk equipment conform to the organization of the sheet. Immediately report
any discrepancies to your TA, who will give you a replacement slip to be used in obtaining
the missing item from the Laboratory Stockroom . When your equipment is in order,
sign the check-in sheet and return it to your TA. You will not be registered for the course
until the check-in procedure is completed. Once you have checked into the laboratory, you
are responsible for the items in your desk, and even if the course is dropped the following
day, it is your responsibility to check-out of the laboratory.
B. CHECK-OUT PROCEDURE
Students will check out of the lab on the day designated in the course schedule.
Students who do not check-out as scheduled, will be checked out by the Laboratory
Stockroom Personnel. For this service, the charge of $50 will be billed to the
student’s MIT account. If you DROP the course, you are STILL required to complete
the check-out procedure, and you may arrange with your TA to check out at the time
when you are leaving the course.
All glassware and other equipment must be replaced, if necessary, by purchase from the
Laboratory Stockroom. Desk items will be checked against the check-in sheet.
C. LABORATORY EQUIPMENT
In addition to the equipment in your desks, other items may be checked out from
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the Laboratory Stockroom on presentation of a withdrawal slip.
Returnable equipment
These may be obtained from the Laboratory Stockroom for a limited period of
time. Most items are in short supply and must be returned at the end of EACH laboratory
period. You will be notified if a returnable item may be stored in your desk for the duration
of an experiment. You will be charged only if the equipment is not returned or is damaged.
Only those items issued to you will be accepted for credit. Fill out and submit a return slip
with each item returned to the Stockroom.
Non-returnable Items
Bring the empty container or worn out item (filter paper box, septa, etc.) to the
Laboratory Stockroom for refill or replacement.
D. LABORATORY CHARGES
You will be charged only for your purchase of “breakage,” i.e., all returnable
items you fail to return to the Laboratory Stockroom and desk items that are replaced during
the semester or while checking out. Do not indiscriminately purchase non-returnable items
from the Laboratory Stockroom without consulting your TA to determine whether you will
need them.
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1.4 GRADING
A detailed overview of the URIECA program can be found online from the Dept of
Chemistry’s web page.
5.35 is composed of three separate lab modules. Each module has similar grading schemes
differing principally in the format of the final report (see below). You will receive a distinct
letter grade for each module upon completion of the module and after marks have been
tabulated. Once you have completed all three modules (not necessarily in the same
semester), you will receive an overall letter grade for 5.35 that is based on an equal
weighting of your grades for each of the three modules
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Laboratory Quizzes: 5 minute quizzes will be conducted at the beginning of most lab
periods, as determined by the instructor or TA. These quizzes are solely designed to
determine if you have read the lab manual and have prepared yourself and understand
the experiments you will do that day.
The Factual Record: Data, procedure signed and dated. It is important to develop good
habits in keeping a notebook. Students must submit carbon copies of their notebooks to
their TAs at the end of each lab period.
Techniques, Safety:
The staff will use the following guidelines for assessing each student’s
laboratory technique, proper waste disposal, safety, etc.
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Waste Inventory Sheets:
Waste inventory sheets require you to track the chemicals you use in each experiment and
their ultimate destination at the experiment’s completion. For labs that include this, you
must keep track of your consumption after each lab day. Waste management is an
important aspect of modern chemistry. These will be graded based on the quality of the
tracking of chemicals and wastereduction ideas. Ideas will be considered for future
incorporation into 5.35.
The TA responsible for the experiment will grade the notebooks and reports(see also
Section 1.6). Your TA should discuss the comments and evaluations with you. Questions,
suggestions, comments, and complaints not being handled by the TA’s should be directed
to the course faculty or laboratory director.
Each experiment will be graded based on the quality of the laboratory work and the
write-up. All of the categories listed below will be considered in grading, but the relative
weight will depend on the nature of the experiment (your TA will provide more details and
advice). Your final grade for each experiment will be based on:
Laboratory reports and any other written assignments are due on the dates
announced in lab . All written reports must be turned in by the report
due date to obtain a grade in the course.
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1.5 NOTEBOOKS AND REPORTS
1) Notebook
A. General
The colored duplicate copy of the factual record of each dayʼs work must be
handed in to your TA after each page has been signed and dated by your TA at
the end of each lab day.
1. Duplicate pages work best with a ball point pen (black or dark blue ink), press
hard.
2. Write on one side only.
3. No erasures or whiteout:
• If you make a mistake, cross it out neatly so it still can be read.
• Write the correct entry on top or side.
• If the entire page is incorrect, cross it out with a single diagonal line and
state the reason why it is believed incorrect.
• Under NO circumstances should any original page be removed from a
notebook.
4. Record all data and results with units and experimental error directly into
your notebook:
• Data may NOT be transferred. Never record anything on scraps of paper,
your hand… Plan to have your Notebook with you wherever you will make
a measurement of observation.
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• If circumstances force you to record data remote from your notebook;
date, sign and tape it into your notebook.
5. Start a new page for each experiment and each new major section:
• Write the title of experiment, date, your name and your TAʼs name at the
top of each page.
• Indicate if the page is continued from previous page.
• NEVER skip a space for later additions. Always record data is a serial
fashion except when it is appropriate to record it in a table.
6. Be neat! Do not overcrowd a page:
• If handwriting is large skip a line.
• Write legibly. If you canʼt write legibly then PRINT. Illegible notebooks
may receive a grade of zero. Other things being equal a neat and well
organized notebook is far preferable to a messy or poorly organized one,
although neatness and organization are distinctly secondary to legibility,
accuracy and completeness.
1. Title, date, your name and your TAʼs name on each page.
Record all data and results. The crude yields of products or product mixtures
should always be recorded. If the product is separated into crude acidic, basic,
and neutral fractions, the weight of each crude fraction should be recorded. If
any of the crude fractions is a solid, its crude melting point should be recorded. It
is extremely important to make every effort to account for all of the reactants in
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the various fractions of crude products. Thus, for a chemist to begin a reaction
with 1.0 moles of a reactant and then to describe only the isolation of 0.13 moles
of a product at the end of the reaction is inexcusable. The fate of the remaining
0.87 moles of material should be indicated, even if no additional pure substance
can be isolated.
Note: always report both the weight and physical constants for the crude and
pure products.
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• Show a sample calculation, substituting the number in with appropriate
units.
• If the calculation needs be repeated, it may be shown in tabular form.
Graphs:
• Use fine paper graph paper if the rulings in notebook are not sufficient.
• Provide a reference to the data in tabular form, e.g., STC-I-42A.
• Attach the graph to the notebook
• Label axes and title with units.
Spectra:
• Attach the spectra to your laboratory notebook.
• Label axis with units.
• Provide a reference to the spectra in the procedure section of your
notebook, e.g., STC-I-42A.
5. Data Analysis and Errors.
• Perform appropriate error analyses
• Examine and discuss the accuracy and precision of data.
• Is the precision of your result reasonable based on the uncertainties of the
original measurements?
• Discuss possible systematic and random errors.
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2) Written Report
(1) Title. The title should be a brief, clear description of the subject of the report.
(2) Abstract. The abstract is a concise statement of the major results obtained
and should consist of no more than 2 to 4 complete sentences. It should be
prepared after the rest of the report has been completed.
(3) Introduction. The second page of the report should begin with the
Introduction, which is record of the experiment. The Introduction should contain
a brief statement of the experiment to be performed with balanced chemical
equations where relevant, and a statement about the goal of the experiment. DO
NOT just regurgitate the laboratory write up.
(5) Summary of results. All data, yields, calculated results, etc. should be
presented, in tables or graphs if applicable.
(7) Analysis of Data and Errors. ALL ANALYSIS OF DATA MUST BE DONE
INDIVIDUALLY. The reproducibility and precision of data should be examined
and the major sources of errors identified. Although detailed statistical analyses
of error are rarely called for, you should at least attempt to distinguish between
systematic and random error.
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(8) Discussion, Interpretation. The outcome of each experiment should be
quantitatively and qualitatively discussed in relation to the goals of the
experiment as stated in the introduction. You should:
(9) Conclusion. A very brief (1-3 sentence) statement based on the data
collected and analyzed.
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3. ORAL REPORT
After completing the last experiment, you will present your results and
analysis to your TA in the form of an INFORMAL ORAL REPORT. In this oral
report, you should tell your TA briefly:
Much of the preparation for your Oral Report will be the same as for a Written
Report, described above. In particular, the data analysis, graphing and plotting,
error analysis, etc. should be carried through to completion and the results
should be presented in an appropriate form (tables, plots, etc.) for efficient
communication.
YOUR PRESENTATION
You should plan on discussing your experiment for no more than 15-20
minutes. Be aware that it is impossible to present everything that you know
about the experiment. Therefore, you should selectively plan what you have
chosen to present. Throughout the time, your TA will ask questions pertaining to
your experimental work.
The objectives of the oral are to encourage you to learn as much as possible,
and to find out how much you know in an efficient manner. In an informal exam
of this type there is no substitute for knowing the material.
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After analyzing your data and mastering the material, organize your
presentation. You will almost surely want to use some notes, especially to guide
you through theoretical discussions. You may use a blackboard if you wish. You
may also just show your (neatly written) notes to your TA on occasion, rather
than transcribe them onto the board. (This is especially convenient if there are
many equations.) Do whatever makes you most comfortable, without wasting
time. You will surely need to show your TA spectra, plots, etc. As always,
attention should be paid to the presentation of data and results so that they are
easily understood. Write neatly, label the axes of plots, indicate units, errors,
etc. Some students find it helpful to use a poster format to avoid shuffling
papers.
You should come prepared to “take the initiative” and guide the oral exam.
Otherwise your TA will be forced to take the initiative by asking you question after
question, likely venturing into territory you prefer not to explore. Be prepared to
give an informal but well organized presentation. Your presentation should
include the following elements, in sequence:
• Introduction;
• Background (why you did it);
• Experimental (what you did);
• Results (what happened);
• Discussion;
• Conclusions;
Ordinarily, you will not turn in your original data. However, you must do so if your
TA so requests after your oral exam. Your grade will reflect your ability to
convince the TA that you understand the most important aspects of the
experiment. The experiment grade sheet will be used by your TA as a guideline
for determining your grade.
The schedule for the oral reports will be posted in advance on the course bulletin
board. It is your responsibility to check the day, date, time and topic of your oral
report.
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1.6 ACADEMIC HONESTY
The expected behavior in the laboratory courses and the consequences of not following these
standards.
Every decision has its ethical component. While it may appear that in a
laboratory course such as 5.35 it's really not difficult to tell right from wrong, there
is always the potential for ambiguity or miscommunication on these issues: hence
this perhaps overly long statement. The MIT policy on academic misconduct is
very strict. "MIT assumes that all students come to the Institute for a serious
purpose and expects them to be responsible individuals who demand of
themselves high standards of honesty and personal conduct. Cheating,
plagiarism, unauthorized collaboration, deliberate interference with the integrity of
the work of others, fabrication or falsification of data, and other forms of
academic dishonesty are considered serious offenses for which disciplinary
penalties can be imposed."1
Where does ethical conduct come into the picture? Experimental scientific
work requires, among other things, background knowledge (why do we want to
do the experiment, what do we want to get out of it), experimental skills (how do
we do it), scientific ethics (what are we going to do with the information we obtain
from it, what if the experiment fails, etc.), and a large dose of motivation
(motivation to study, motivation to learn, motivation to discover, or even
motivation to obtain a good grade). Lack of motivation is one of the principal
causes of failure in experimental work, especially in a laboratory subject. This
1
"MIT Policies and Procedures", (http://web.mit.edu/policies)
2
"On Being a Scientist. Responsible Conduct in Research", 2nd. Edition, Committee on Science,
Engineering, and Public Policy, NAS, NAE, IOM, National Academy Press, Washington, D.C., 1995.
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lack of motivation is usually accompanied by weak background preparation, lack
of experimental techniques and skills, and in several cases, unethical behavior.
Motivation is very personal and cannot be provided or taught. On the other hand,
the background knowledge you need to perform an experiment is mostly built
during your lecture subjects. It is in laboratory subjects such as this one where
you learn experimental skills as well as the basis of ethical scientific behavior.
3
For examples of experiments which failed on multiple occasions, just recall NASA's 1998 Mars Climate
Orbiter and Mars Polar Lander missions. For details, consult the NRC report at
www.nap.edu/catalog/9796.html.
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Unlike in the lecture subjects, your actions in a laboratory subject can affect,
and they usually do affect, the performance of your classmates. Imagine that
by accident you contaminate a solution of a reagent that your classmates will
use after you. Would you inform your TA at the risk of losing your "technique"
points? Or would you keep silent and let your classmates perform the
experiment with a contaminated reagent?
In some cases unethical behavior seems to be the easy way out, and some
students think they can get away with it. That is certainly not the case, and
we will do our best in defending the effort of those students who honestly
work toward academic excellence.
Examples of conduct in 5.35 that would fall in the category of academic
dishonesty, and would result in severe penalties
• CHEATING on a lab quiz, including having your lab manual or notebook open
during a closed book quiz, will result in a grade of zero for that experiment.
• COPYING into your lab report any section of another student's lab report
(from the current or a previous year) will result in a grade of zero for that
experiment, could result in a grade of F for the course, and could result in the
case being referred to the MIT Committee on Discipline.
• MAKING UP and/or ALTERING DATA will result in a grade of zero for that
experiment and could result in a grade of F for the course and the case being
referred to the MIT Committee on Discipline.
• Adding a grade sheet or other materials to the written report after submission
for grading will be considered academic dishonesty unless the submission
date is adjusted and the late report penalty is taken.
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1.7 REQUIRED ITEMS
Required Items:
A USB Flash Drive will be needed to collect data files. The U Lab is also outfitted
for wireless web/e-mail connectivity for your laptops. However, lab computers are
to be solely used for data collection and are not connected to the network.
A laboratory research notebook with numbered duplicate pages (i.e., each white
page being followed by a colored page, perforated for easy removal).
Carbonless copy pages are preferable to those requiring carbon paper. Most
students will require a notebook with 100 duplicate pairs of pages. Notebooks
with 50 duplicate pages are available; however, a second notebook may be
required to complete the course.
You are allowed to bring your lab manuals for use during the lab period.
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