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THE UNIVERSITY OF THE WEST INDIES CAVE HILL CAMPUS Department of Biological & Chemical Sciences CHEM3950 –BASIC PROJECT IN CHEMISTRY CHEM3955 – RESEARCH PROJECT IN CHEMISTRY LABORATORY MANUAL ACADEMIC YEAR: 2021-2022

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ACADEMIC INTEGRITYCAVE HILL CAMPUS
CHEM3950 –BASIC PROJECT IN CHEMISTRY CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
LABORATORY MANUAL
CHEM3950 – BASIC PROJECT IN CHEMISTRY Academic Year: 2021-2022 CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
Page 1
Guidelines for Students 6
– Research Notebook Management 8
On Writing Reports 10
Reference style 14
Contents 18
Form 18
Delivery 19
Academic Integrity 21
Emergency procedures in the chemistry laboratory 30
Policy for exposure to hazardous materials during pregnancy 34
General laboratory safety reminders 34
Notes on Laboratory Technique 35
Column preparation 35
Column chromatography 35
Chloroform recovery 35
Distillation 35
CHEM3950 – BASIC PROJECT IN CHEMISTRY Academic Year: 2021-2022 CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
Page 2
Recrystallization 36
Refrigerators 36
Vacuum distillation 37
Reaction Yields 39
Cleanup and Checkout Procedure for all Project Students 41
Chemistry Research Project Laboratory Safety Regulations Agreement 42
APPENDIX 43
CHEM3950 – BASIC PROJECT IN CHEMISTRY Academic Year: 2021-2022 CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
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OFFICE OF THE BOARD FOR UNDERGRADUATE STUDIES
COURSE OUTLINE FORMAT
COURSE TITLE: BASIC PROJECT IN CHEMISTRY COURSE CODE: CHEM3950 LEVEL: III SEMESTER: I & II NO. OF CREDITS: 3 PRE-REQUISITE(S): CHEM2715, CHEM2700, CHEM2705, CHEM2710, CHEM2730
COURSE DESCRIPTION/RATIONALE
This course consists of a research project carried out under the supervision of a member of staff. It is meant to provide the necessary training and skill development in the different areas of chemistry.
LEARNING OUTCOMES
At the end of the course the student should be able to:
1. Complete research goals as defined by the supervisor 2. Make independent and critical assessments 3. Independently perceive, formulate and solve problems 4. Effectively search the literature for information pertaining to specific topics
CONTENT
TEACHING METHODOLOGY
Students who have been admitted to the course have the right to receive tuition and/or supervision for the duration of the time period.
ASSESSMENT
REQUIRED READING
Journal articles and reference books as determined by the supervisor.
CHEM3950 – BASIC PROJECT IN CHEMISTRY Academic Year: 2021-2022 CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
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OFFICE OF THE BOARD FOR UNDERGRADUATE STUDIES
COURSE OUTLINE FORMAT
COURSE TITLE: RESEARCH PROJECT IN CHEMISTRY COURSE CODE: CHEM3955 LEVEL: III SEMESTER: YEAR LONG NO. OF CREDITS: 6 PRE-REQUISITE(S): CHEM2715, CHEM2700, CHEM2705, CHEM2710 and CHEM2730 AND
the permission of the Department. Preference will be given to students double majoring in Chemistry.
COURSE DESCRIPTION/RATIONALE A practical project carried out under the supervision of a member of staff. The project will run throughout the academic year and students are expected to spend at least 144 hours on laboratory work. Each student will be required to give a seminar on completion of the project as well as submit two typed and bound copies of a written report. Enrolment will be limited to those students who have demonstrated good practical skills and an aptitude for research.
LEARNING OUTCOMES
CHEM3505 is an eight credit course in which final year undergraduate students pursuing a major in Chemistry engage in research under the guidance of a member of staff in the Department of Biological and Chemical Sciences. The goal of the course is for students to actively participate in state-of-the-art research in chemistry. In so doing, the student will be exposed to research problems of current interest. They will also receive instruction and gain experiences in:
• Using modern research tools
• Carrying out research investigations
• Increasing their understanding of the scientific method
• Reading and evaluating scientific journal articles
• Developing experimental skills and techniques
CONTENT
CHEM3950 – BASIC PROJECT IN CHEMISTRY Academic Year: 2021-2022 CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
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TEACHING METHODOLOGY Students who have been admitted to the course have the right to receive tuition and/or supervision for the duration of the time period.
DECIDING ON A CHEM3955 PROJECT
Students are encouraged to begin their undergraduate research as soon as their course schedules allow. CHEM3955 projects are offered in both semesters. In making a decision on a CHEM3955 research project, students should look over the list of projects being offered in the preferred semester and fill out the form attached at the end of the lab manual. This form should then be handed in to Ms. Shirley Jones in the Departmental Office. You will be contacted at a later date informing you of the project that you have been assigned to. Students are strongly encouraged to meet with the project supervisors and postgraduate students before deciding on projects.
ASSESSMENT
REQUIRED READING
Journal articles and reference books as determined by the supervisor.
CHEM3950 – BASIC PROJECT IN CHEMISTRY Academic Year: 2021-2022 CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
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Guidelines for Students pursuing CHEM3950/CHEM3955
During your project you will conduct an investigation under the guidance of a project
supervisor(s). You will develop specialised practical/research skills and you are required to
utilize the knowledge that you have acquired in your course of study to solve problems. Your
success is heavily predicated on your motivation and attitude. To help you to successfully
navigate this course, the guidelines as presented below have been created.
1. Fill out the application form at the back of the CHEM3950/3955 lab manual clearly
listing your 1st, 2nd and 3rd choices. Every effort will be made to assign you to your
preferred project, however at times it may be necessary to assign you to your 2nd and 3rd
choices and in some cases, an option not noted on your application form.
2. Submit your completed application form to Ms. Shirley Jones in the Departmental Office
by Friday, September 10, 2021 (semester 1) or by Friday, January 28, 2022 (semester
2).
3. When you have received your assignment to a project and a supervisor, make an
appointment to see your supervisor(s) as soon as possible. During the meeting with your
supervisor(s) ensure that you fully understand:
- What it is you are trying to achieve in your project
- The relevance/importance of what you are trying to achieve
In addition, establish a timetable that lists the times that you will meet with your
supervisor, deadlines for drafts etc.
4. Subsequent to the meeting with your supervisor(s) and prior to the commencement of any
practical work you should write a summary (no longer than one page) detailing the aims
and objectives of the project and submit to your supervisor(s) for approval.
5. You must attend the library session and a safety session, the dates of which will be
communicated to you.
6. “Mini-workshops” may be held during the first hour of the timetabled lab session. You
are required to be in attendance for all sessions scheduled, the dates of which will be
communicated to you.
7. Try not to exceed 72 hours on your investigations. If you do, it may have an adverse
effect on your studies.
8. All data, procedures, calculations etc. associated with the project must be recorded in a
lab book.
10. Be courteous to the technical staff.
11. Once you have commenced practical work:
- Be neat and be considerate of other researchers in the laboratory.
- Read and follow the assorted notes and memos on how to do research and
how to conduct yourself in the laboratory.
- Respect and take care of equipment and glassware, most of which are
extremely expensive. Many long hours are spent sourcing funds to buy
equipment which you will be using. In other words, DO NOT BREAK
STUFF!
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- Work hard and become “emotionally involved” with your project. You will
gain independence and self-confidence as you progress but should keep in
close touch with your supervisor about your project.
12. After your practical work is finished you must:
- Clean all glassware including sample vials, test tubes etc. that were used by
you and return them to their correct storage area.
- Clean and wipe down your workbench as well as the working surfaces of the
communal areas (balance room, fume hood etc.) that you used.
- Return apparatus (general or specialised) that was borrowed from the
technicians, other lecturers etc.
- Dispose of all chemicals appropriately and safely using the waste bottles
and/or containers provided in the lab. If you are unsure of how to safely
dispose of a chemical please consult with your supervisor, technician - Mr.
Kenville Grimes or Senior Technician - Mr. Lionel Sobers.
13. If your project does not require laboratory work, you will be required to take a safety test.
See your supervisor and coordinator.
14. You are required to submit TWO (2) copies of your project report (THREE (3) in the
case of CHEM3955) to the Departmental Office by the deadline date (will be
communicated to you). The last page of the report must contain a summary report
generated by the TURNITIN software which can be accessed on the myElearning
website. You must have a copy of your report present at the oral presentations.
15. You are required to prepare an oral presentation (10 minutes for CHEM3950 and 15
minutes for CHEM3955) based on the work done on your project.
16. Your electronic file should be uploaded to the computer BEFORE the start of
presentations on the day of the oral presentations.
17. A corrected, bound copy of your report should be submitted to the Departmental Office
no later than one month after the date of the oral presentations.
18. The Assessment of Oral Presentation forms along with the rubric used by the examiners
are located in the Appendix.
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RESEARCH NOTEBOOK MANAGEMENT
The notebook is the fundamental record of experimental research. It is to be used for recording
all laboratory operations and observations. It should provide in ink and account of what was
done, how it was done, and what happened. This includes the apparatus used, the sequence of
steps, all measurements, significant time intervals, changes in appearance, and all other relevant
data. It is essential that the salient operations, observations and measurements be recorded
insofar as possible as they are done or made. An ex post facto scrapbook of recollections and
miscellaneous jottings is exactly what a research laboratory notebook is not to be. It is also not to
be used as a record for literature searched (a separate notebook or card index better serves this
purpose) and must not be a verbatim transcription of a literature procedure.
This set of guidelines is designed:
a. To increase the efficiency of the researcher to do research.
b. To enable succeeding researchers to exactly reproduce experimental results reported by
the original researcher.
c. To allow the research adviser quick and painless access to samples, spectra and other data
for publication or other purposes.
An index should precede the main body of the notebook. Therefore leave at least 2 pages
(depending on the size of your writing) for it. The index should list a given synthetic
transformation in structural format, i.e. graphics only! It is wise to write the index parallel to
writing the experimental; it is tedious and boring to have to write the index after the book is
complete and it is only too easy to find excuses not to do it. Yields should also be indicated here.
Record the date for each reaction at the top of your notebook page (Month, day, year). All
entries are to be made in the dark ink; never use pencil. In industry, each page must be signed by
the researcher and by a witness! Although we don’t think we need to be this precise, you
absolutely must record the date, including the year, the reaction (showing structures) and what
you did.
You must include the amounts (weight, volume, moles) of substrates, reagents, and solvents, the
reaction times, temperatures, and other conditions, the workup procedure, and purification
procedure(s). Normally, since it changes, the recrystallization solvent volume is not recorded,
and the weights of drying agents are normally not cited. Try to remember to record the volumes
of extraction and washing solvents that you employ during reaction workups, and the volume
and/or weight of the workup medium (e.g. saturated ammonium chloride, ice, etc.). Of course,
these can be approximate. The quantity of drying agent need not be specified. The concentrations
of aqueous washing solutions should also be noted (e.g. 6N NaOH, saturated aqueous sodium
carbonate, 2% HCl, etc.).
Think carefully about significant figures when you are planning a reaction. Thus, it is absurd to
weigh out a reagent to three or four significant figures when it is to be used in large excess in a
reaction. For example, it is illogical to weigh out 5.37 g (0.141 mol) of sodium borohydride for
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use in reducing 2.83 g (0.0141 mol) of a ketone. Thus, if a ten-fold excess is required, then
weigh out 5.4 g or even 5 g. Also watch your use of significant figures in calculating and
reporting yields. Thus, it is incorrect to report the weight of a product to four figures if you only
weighed your starting material (assuming this to be the limiting reagent) to two or three figures.
Thus, 1.42 grams of starting compound can give 1.23 grams of product but not 1.234 grams of
product even if you weighed the product more carefully than you did the starting material! The 4
milligrams is meaningless here because your 1.42 gram starting weight implies a reproducibility
of 0.01 grams and not 0.001 grams. (Note that 0.0005 has one significant figure while 2.00400
has six). Remember that % yields are normally reported to only two significant figures.
Other important data for your notebook: source of all starting materials and reagents, reference to
previous reactions (yours or literature), reaction temperatures and times, other reaction
conditions (inert atmosphere? Mechanical stirring?), observations (colour changes?
Exothermic?), cautionary notes, selected spectral data, chromatographic and other purification
information.
Other important data for your experimental writeups (research report): TLC and other
chromatography data (solvents, adsorbents), spectral data (IR, NMR, UV, MS), physical data
(melting or boiling points), elemental analytical data for new compounds (staple the results in
your notebook), X-ray data. You must indicate in the notebook what spectral information you did
record for a particular experiment or compound, and, of course, reference it to that relevant
notebook page number.
References should go in the notebook as should all important (or all) spectral data.
Summary
1. Record grams and moles of everything you use.
2. Record the number and volume of each extraction that you use in a workup.
3. Weigh the product(s) from a reaction and calculate the percent yield. You should weigh both
crude product and purified product.
4. Record all temperatures and pressures for distillations, sublimations, dryings.
5. Record concentrations of reagents and the source of all chemicals used (except common
stuff).
6. Recording 1H-NMR (and 13C-NMR if available) and IR spectral data (e.g. ten strongest
peaks) in your notebook saves time later when you write your report. This applies to all other
chromatographic information if you obtained these.
7. Record TLC data (solvent system, plate type, Rf, developing system). The same applies to
column chromatography.
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8. For a recrystallisation, of course you would record the solvent(s), but also make note of the
crystal type (plates, needles, cubes, etc.), size (long, short, fluffy, etc.), and colour. Record
the weight of each crop and the melting point.
9. If you have an “authentic” sample of what you have just made, you should do the following:
a. TLC comparison, including spot-on-spot.
b. Run IR’s of both at the same time (or nearly so) and concentration. This is the
single best means of compound comparison.
c. Do an mp and a mixed mp (if sufficient material is available).
d. An NMR comparison is frequently useful.
10. If you do not have an “authentic” sample of what you have made, then you should try to
locate similar compounds in the literature and record their IR, NMR, UV, etc. data in your
notebook to convince yourself and your supervisor that you really made what you think you
have made.
11. All new compounds require an elemental analysis. This requires an extensive
recrystallisation sequence. Pass on your sample to your supervisor promptly. Non-distillable
liquids may be analyzed by HR-MS.
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ON WRITING REPORTS
Good writing requires time, effort and care. In writing theses and reports the objectives should be
clarity and conciseness. Always choose the simple expression rather than the unusual. A reader is
more favourably impressed by an easily understood report, than by an exhibition of fancy literary
style.
GENERAL FORMAT
Specific recommendations with respect to font, font sizes and other formatting requirements are
given below. They are to be followed and variations are subject to a penalty.
1. FONT TYPE
Acceptable font types include Arial, Helvetica and Times New Roman.
2. FONT SIZE
Headings should be bold and in size 12 or 14 point.
Normal text in the body of the report should be size 12.
3. SPACING
4. ALIGNMENT OF TEXT
All text should be justified.
A chemical report should contain:
a. Table of Content (May include list of Table and Figures)
b. Abstract
f. Experimental
g. References
ABSTRACT
This is a succinct (one paragraph) summary of the entire report. The abstract should briefly
describe the question posed in the report, the methods used to answer this question the results
obtained, and the conclusions. It should be possible to determine the major points of the report
by reading the abstract. Although it is located at the beginning of the paper, it is easiest to write
the abstract after the paper is completed.
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INTRODUCTION
This part should include a brief and clear statement of the purpose and objectives of the work
and a concise historical background. Remember, you are writing to inform not only your
research supervisor, but others who may not be at all familiar with your work.
RESULTS AND DISCUSSION
This section should contain a description of the work of the report but can be divided into two
separate sections. Do not be a slave to chronology, but organize the presentation for clarity.
Sentences should not be interrupted by structural formulas, which should be conveniently located
between paragraphs and assigned Arabic numerals in the order of appearance. These formulas
are referred to in the text by the numerals. The discussion should be self-sufficient, and should
describe the reactions performed, any unusual experimental conditions, yields of products, and
any particularly significant data for new products.
Avoid: (a) Verbosity, (b) unnecessary changes of tense – usually the past tense, passive voice is
preferred, (c) the use of atomic symbols in text, (d) the use of the verb to react in the transitive
form.
EXPERIMENTAL
This section should contain complete details of the laboratory operations, should be written in
the past tense, passive voice, and should be consistent in style throughout. It is usually
convenient to specify some general practices in a footnote at the beginning of this section, e.g.,
that 95% ethanol was used as solvent for all ultraviolet spectra.
1. Each experiment that is written up should be carefully checked.
2. Paragraph headings should be used for each preparation.
3. No procedure is entirely new. Therefore, each preparation should have introductory
sentences citing (with references) the precedent for the procedure that follows.
4. All major compounds should be given full and correct chemical names (IUPAC where
possible).
5. Write up experiments in past tense and passive voice. Right: “The compound was distilled at
reduced pressure, bp 170-175° (0.5 Torr).” Wrong: “I distilled the compound….”
6. Always give the source, method of purification and physical characteristics (as determined
by you) of starting materials used in all preparations.
7. Never start a sentence with a numeral. Wrong: “0.10 g of the ester was…” Right: “One-
tenth of a gram of the ester was…” Generally such sentences can (and should) be rearranged
so as to avoid starting with a number, e.g. “A solution of 0.10 g…” or “A 0.10 g sample
was…” Exception to the rule: sentences may be started with names of compounds which
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begin with numerals, e.g. “2-Methoxytetralin…” In this case, the first letter following the
numeral is capitalized.
a. mg for milligrams
b. mL for millilitres
e. % for percent
j. mol for mole and moles
9. Weights, volumes and lengths of time are expressed in numerals except when beginning a
sentence.
10. Tables should carry titles as well as numbers. See the J. Am. Chem. Soc. for the correct
format.
REFERENCES
A scholarly report will be well documented with appropriate references to support statements
and to provide precedents. For reporting references use the Chemical Abstracts abbreviations for
journals and the style used in the ACS Style Guide. Examples are provided below.
Reference Style Guidelines (http://pubs.acs.org/books/references.shtml)
1. Citing References in Text
Indicate references in text by superscript numbers, which appear outside the punctuation if
the citation applies to a whole sentence or clause. Number the references sequentially as they
occur in the chapter text. Do not combine references. Each reference number should refer to a
single source, except where a Chemical Abstracts reference is included. An example is given
below.
Oscillation in the reaction of benzaldehyde with oxygen was reported previously.3
2. Reference Style
Collect references in a list under the heading References at the end of the report. The References
section should consist of a numbered list of references, single-spaced. Begin this section on a
new page. Do not leave blank lines between references. Please see the ACS sample references,
CHEM3950 – BASIC PROJECT IN CHEMISTRY Academic Year: 2021-2022 CHEM3955 – RESEARCH PROJECT IN CHEMISTRY
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3. ACS Sample References
The following are examples of ACS standard forms for various types of literature citations and
should be followed. (For more examples and a thorough discussion of reference style, consult
The ACS Style Guide, Chapter 14.)
Journal
Author, A. B.; Author, C. D. J. Abbrev. 19XX, vol, xx-yy.
NOTE: No punctuation in journal abbreviations except periods. No conjunctions,
articles, or prepositions in journal abbreviations. No comma or semicolon before or after
journal titles.
e.g: Evans, D.A; Smith, T.E.; Cee, V.J. J.Am, Chem.Soc. 2000, 122, 10033-10046
Magazine with dates instead of volume numbers
Author, A. B.; Author, C. D. Magazine Abbrev. October 26, 1995, p. 20.
e.g: Manning, R. Wired, May 2004, p. 176
Article from an on-line journal
Author, A. J. Abbrev .(online) 19XX, vol, pp-pp http:// (accessed date).
e.g: Peacock-Lopez, E. Chem. Ed. (On line) 2007, II, 383-393 http://Chemeducator.org
/bibs/0011006/110603801b.htm (accessed August 23, 2007).
Book without editors:
Author, A. B.; Author, C. D. Book Title; Series Name and number; Publisher: City,
STATE (2 letters), year; Vol. 1, pp xx-yy.
Book with editors, no authors named:
Book Title; Editor, A. B.; Editor, C. D., Eds.; Series Name and number; Publisher: City,
STATE (2 letters), year; Vol. 2, pp xx-yy.
Book with editors and authors named:
Author, A. B. In Book Title; Editor, C. D.; Ed.; Series Name and number; Publisher: City,
STATE (2 letters), year; Vol. 3, pp xx-yy.
Patent
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Author, A. B. Ph.D. thesis, Institution Name, City, STATE, year.
e.g: Thoman, J.W.Jr. PhD. thesis, Massachusetts Institute of Technology, Cambridge,
MA, 1987.
Websites:
An example of an electronic reference is: About the Commercial Internet eXchange, URL
http://www.acs.org. followed by the accessed date.
Use Chemical Abstracts abbreviations for journal names. For books, edition follows title: Book
Title, 2nd ed;
The punctuation retains the style (e.g., roman, bold, or italic) of the character to which it is
attached. Include the state name for all U.S. cities except New York. Include the country name
for all non-U.S. cities except London and Paris.
For unpublished results, give author names and affiliations. Describe submitted material as
unpublished. Unless an article has been published, it is either unpublished or accepted, in which
case it is in press. Include the journal name and year.
When citing M.S. or Ph.D. theses, include the name of the school, city, and state (or city and country). Certain journals that have duplicate titles should be cited along with the city of publication. For example:
Science (Washington, D.C.) Nature (London) Nature (London) New Biol. Nature (London) Phys. Sci.
Certain journals do not have volume numbers:
Chem. Ind. (London) Chem Lett. J. Chem. Soc. J. Chem. Soc. Chem. Commun. J. Chem. Soc. Faraday Trans. 1 or 2 J. Chem. Soc. Perkin Trans. 1 or 2 Proc. Chem. Soc. London Tetrahedron Lett.
For a more detail listing you can see the following website:
Page 16
1. PREPARATION OF FIGURES AND SCHEMES
Representations of chemical structures form a major part of many chemistry reports and
presentations. Chemical drawing programs such as ChemDraw, Isis/Draw and ChemSketch have
revolutionized the field of chemistry reporting.
The following guidelines must be considered when preparing figures and schemes:
• Figures and schemes are consecutively numbered with Arabic numerals in the order they
are first cited in the report (i.e. Figure 1, Figure 2, etc.).
• The legends of figures and schemes should be positioned directly below the
corresponding graphic in the report.
• Figures and schemes should be cropped as closely as possible to minimize white space
surrounding the graphic.
• Individual compounds must be numbered with boldface Arabic numerals in the order in
which the compounds are first mentioned in the text. Boldface lower case letters may be
added to distinguish compounds that differ only in the identity of substituents.
• All figures and schemes must be embedded in the report after the paragraph where they
are first mentioned.
• All figures and schemes should be approximately the same size where possible.
• Do not scan diagrams from books or other paper sources. Such scanned images are
usually of low quality, and are in violation of the original copyright
Structure Drawing Guidelines
Chemical Structures should be prepared according to the guidelines given below. The parameters
are benchmarks which should be used to prepare chemical structures with chemical structure
editors such as ChemDraw, etc.
Drawing in ChemDraw
• Chain angle: 120 degrees
• Fixed length: 0.25 in
• Bold width: 0.0278 in
• Line width: 0.0139 in
• Margin width: 0.0139 in
• Hash spacing: 0.0347 in
• Atom labels: Arial 12 pt Regular Formula
• Bond angles and length: "fixed" is recommended
The recommended settings for slide presentations are as follows:
• Chain angle: 120 degrees
• Fixed length: 0.35 in
• Bold width: 0.0625 in
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Page 17
• Atom labels: Arial 16 pt Bold Formula
• Bond angles and length: "fixed" is recommended
Drawing in IsisDraw
IsisDraw is available free to educators and students (with registration) from MDLI.
Obtaining ISIS/Draw.
Go to the MDLI website at http://www.mdli.com/. [UK mirror http://www.mdli.co.uk.] Look for
the "Download no-fee software" link near the bottom of the page, under "Quicklinks". Choose
the appropriate version, and download it. Optional. While at the download site, you may also
want to download two additional items:
1. The AutoNom Standard add-in. This add-in allows you to name structures you draw, and is
discussed below under F. Additional useful features in ISIS/Draw. (If the AutoNom installer
detects an old version, it will ask you if you want to proceed. You probably want to continue,
and install the new version in the correct folder.)
2. The help file. The basic installation does not include a help file. For basic use the instructions
given here should be sufficient.
Installation.
To install the program, run the exe file that you have downloaded. If you downloaded either of
the optional items discussed above, install them by running their exe files.
For further assistance, refer to:
http://www.geocities.com/athens/thebes/5118/obc/isis.htm#Introduction
2. PREPARATION OF TABLES
• All tables must be inserted in the report text after the paragraph where they are first
mentioned. The following guidelines must be considered when preparing tables:
• Tables are consecutively numbered with Arabic numerals in the order they are first cited
in the manuscript text (i.e. Table 1, Table 2, etc.).
• Tables must be cell-based and thus should be created using the “Table object” in the
word processing program such as MS Word or WP. Cells should be aligned either centre
left or middle centre.
• Line returns and tabs should not be used within the cells.
• Above each table a sequential bold typed Arabic table number must be provided followed
by a short and concise title after a colon.
• All table columns must have a short and self-explanatory heading.
• Footnotes should be typed below the table using low case letter designations. They
should be referenced in the table with lower case superscript letters. The sequence of
letters should proceed by row rather than by column. An explanation of all non-standard
abbreviations used in a table as well as additional descriptive information to the table
content must be given in a footnote.
Page 18
CONTENTS
What is the exact definition of the topic? What is expected? Analyse, clarify and define the topic
for yourself, then talk to your supervisor about aspects that remain unclear.
Ask your supervisor for starting points in your search for material. What is central and what is
marginal to the treatment of the topic? You cannot present everything, but make sure you present
the core of the matter, the basics, the essentials. A short report can only present the gist of the
matter. Nevertheless, a compact five-minute presentation may provide more essential insights
than a thick book.
Which information, models and terms are new and need to be explained? Which new terms did
you encounter preparing the report? Recall your own state of relative ignorance at the beginning
of your research. Use this state as a starting point for your oral report. Should you happen to
know a lot about your topic, try to imagine the basics which everyone needs to know.
The content should be presented in a compact, dense manner, yet clarity and comprehension still
take precedence.
Explain the larger significance of your topic.
Reproduce names, dates and facts accurately. Put difficult terms and names on your handout or
on a slide or print them on the whiteboard in large letters.
Present the facts and the basic information but you may also include your opinion.
FORM
A good presentation needs a beginning that rouses interest while clearly introducing the topic
clearly, a body that allows listeners to discern and follow a chosen pattern and an ending that is a
climax to your efforts (in the form of a summary, a poignant final statement).
You might want to announce the individual steps of your presentation in the beginning so that
the listeners may follow along more easily. Otherwise you can include them in a handout.
Keep your report lively by choosing illuminating examples, quotes and comparisons.
Do not get carried away with theoretical ruminations – your listeners need to be able to
understand and follow you. Don’t try to impress them with your knowledge, rather share your
impressive knowledge.
DELIVERY
The speaker’s attitude should be professional. It is important to be open to the questions,
suggestions or comments from the audience. If a question is beyond the speaker’s ability to
answer fully, the best answer possible should be given. There is nothing wrong in admitting the
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limits of one’s knowledge, saying, for example, “We have not yet considered that…” or “That’s
a good point, we should go back and examine it in greater detail…” Criticism, when justified,
should be accepted gracefully and learned from. Incorrect criticism should be politely explained
away by clearly stating how the particular objection is inapplicable or can be remedied.
Be aware that you are preparing your report for a listening, not a reading audience.
Keep in mind that you need eye contact with your audience in order to keep them with you and
your argument.
You may speak freely from notes/cue cards or you may read freely from a manuscript as
newscasters do. Both forms need practice for an effective delivery. Choose the mode which is
most comfortable for you.
Watch the pace, rhythm and the pauses of your report. Take your time – the audience will be
grateful for a well-tempered delivery. Vary the pace throughout your presentation, going slowly
through compact parts and speeding up through easier sections.
Make sure that the beginning and the ending of the delivery are effectively marked. This is an
important aspect for the success of your report.
Under no circumstances should the report exceed the given time frame. You need to finish within the allocated time. After the time has expired, you will be interrupted so that other presenters will have sufficient time for their reports. Conceive of the time limit as a task and as an opportunity. Think of yourself as a professional journalist working for a newspaper (limited print space) or a radio or a television station (limited broadcasting time).
Practice at home. Keep track of time. Adjust your manuscript to stay within the limit.
Accept that in all likelihood you may be nervous. Consider the presentation as an opportunity for
yourself, not an examination. Even the most experienced talk show hosts and TV stars are
nervous each time they address an audience. Concentrate on the topic, not on your performance.
Think of the many situations in which you have succeeded. Don’t take it too seriously and don’t
think you need to be perfect. Even if you mispronounce words, lose track of your thoughts or
fumble facts; this is all part of the (ad)venture. If possible, relax and enjoy your presentation
once you get started.
Take the advice from experienced speakers: Make your report a KISS (Keep It Short Sweetie).
Fourteen minutes may be just perfect for a fifteen minute report but do not end your report after
eleven or twelve minutes.
REMEMBER
• The oral report allows the presentation of a diversity of speakers and opinions.
• It allows students to take charge and switch roles from being learners to being teachers.
• It allows you to actively shape and model your seminar.
• It provides background information.
• It allows you to practice your presentational skills within a manageable frame.
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Assessment forms and accompanying rubric are collected in the Appendix.
CHEM3950 students will be assessed on the following aspects of the written report, practical
skills and seminar:
Written Report / 55
a. Abstract / 4
b. Introduction / 10
d. Experimental / 7
e. References / 4
Practical Skills / 30
Seminar / 15
c. Ability to answer questions / 5
CHEM3955 students will be assessed on the following aspects of the written report, work and
seminar:
d. Results / 10
e. Discussion / 20
f. References / 5
Work / 15
b. Technical Skills / 5
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ACADEMIC INTEGRITY
INTRODUCTION
Integrity is not a conditional word. It doesn’t blow in the wind or change with the weather. It is
your inner image of yourself, and if you look in there and see a man who won’t cheat, then you
know he never will.
- Ralph Waldo Emerson
Developing the integrity of individuals is of similar if not greater importance than the
development of knowledge. All students are expected at all times to go about their work with
utmost integrity especially when research is being conducted. Unfortunately the subject of
integrity is not always understood and as a result students tend to run into difficulties at the end
of the day.
It is therefore of utmost importance that all students registered for CHEM3950 and CHEM3955
read and understand the following sections that deal specifically with the expectations of this
course. NOTE: Students are required to fill out, sign and return the form (to your
supervisor) at the end of this section that says that you have read, understood and agreed
to abide by the guidelines presented in this section.
Most of the ideas presented in the following sections have been adapted from Academic Integrity
at Princeton, Office of the Dean of the College, Princeton University, Princeton, New Jersey,
2003.
ORIGINAL WORK
We, the academic staff of the Department of Biological and Chemical Sciences, sincerely hope
that during you tenure at the University of the West Indies that you are exposed to the ideas,
scientific theories, and creative works of countless scholars, scientists, and artists. It is expected
that your thoughts and ideas will be shaped by the words and ideas that you encounter. The
intellectual challenge you face in your academic work is to go beyond what you learn in your
textbooks, in lectures, and in library – to evaluate, rethink, synthesize and make your own the
information, data and concepts you find in your sources. The greatest satisfaction of academic
work comes from making something original, genuine, and new out of the material you have
learned in your courses and discovered in your research. Doing original work is the most
demanding, but also the most rewarding part of your education.
Your original work – whether it is a lab report, project report or research paper – is also the basis
for your supervisor’s evaluation of your performance in a course. For that reason, intellectual
honesty is the cornerstone of our academic community. You must always distinguish your own
words and ideas from the words and ideas of others – including the authors of primary,
secondary, or electronic sources and faculty members, classmates, or friends. Making those
distinctions is not always easy and can be made even more difficult by less-than-careful research
habits or the time pressure of submission deadlines.
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Take the time now to learn to recognize when it is necessary to cite your sources and how to
provide adequate and accurate bibliographic information for your reader. In the following
sections you will find definitions, discussions and examples of terms such as Plagiarism,
Collaboration and Common Knowledge.
SOURCES
There are a variety of reasons for acknowledging the intellectual sources upon which you have
built your own work. They are:
• To acknowledge your dependence on another person’s ideas or words, and to
distinguish clearly your own work from that of your sources.
• To receive credit for the research you have done on a project, whether or not you
directly quote or borrow from your sources.
• To establish the credibility and authority of your knowledge and ideas.
• To place your own ideas in context, locating your work in the larger intellectual
conversation about your topic.
• To permit your reader to pursue your topic further by reading more about it.
• To permit your reader to check on your use of source material.
In all of these reasons, the essential element is intellectual honesty. You must provide your
reader with an honest representation of your work so that he or she may evaluate its merits fairly.
Proper citation demonstrates the depth and breadth of your reading – in effect, documenting the
hard work you have put into your research. Proper citation permits a reader to determine the
extent of your knowledge of the topic. And, most important, proper citation permits a reader to
more readily understand and appreciate your original contribution to the subject. In contrast, a
very well-informed, complex or sophisticated piece of work, without adequate or accurate
acknowledgement of sources, will only provoke your reader’s concern or suspicion.
Such intellectual honesty is important, not only for your reader, but also for you as the author.
For example, you may cite a paper diligently only to discover that you can hardly find an original
idea or sentence of your own. Then you will know you have more work to do in order to develop
a substantial original idea or thesis.
These sections will emphasize the positive reasons for properly citing your sources rather than
the negative consequences for failing to do so. However, you need to know that those
consequences can be severe. Failure to acknowledge the sources – textual, personal, and
electronic – upon which you have relied is a serious breach of academic integrity. Such a failure
can lead to the accusation of plagiarism – defined as the use of any source, published or
unpublished, without proper acknowledgement. Plagiarism is a very serious charge at The
University of the West Indies the penalty for which is stated below.
The UWI Examination Regulations deal with this subject in section (B) Cheating under
Regulation 73 as follows:
(i) Cheating shall constitute a major offence under these regulations.
(ii) Cheating is any attempt to benefit one’s self or another by deceit or fraud.
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(iii) Plagiarism is a form of cheating.
(iv) Plagiarism is the unauthorised and/or unacknowledged use of another person’s
intellectual efforts and creations howsoever recorded, including whether formally
published or in manuscript or in typescript or other printed or electronically
presented form and includes taking passages, ideas or structures from another
work or author without proper and unequivocal attribution of such source(s),
conventions for attributions or citing used in this University".
In these regulations, examination refers to any written material to be assessed as part of the final
mark for a course. This includes practical reports, essays and project reports.
The penalties for plagiarism are stated in Regulation 79 as follows:
".... the Committee shall disqualify the candidate from the examination in the course
concerned, and may also disqualify him/her from all examinations taken in that
examination session; and may also disqualify him/her from all further examinations of the
University, for any period of time, and may impose a fine ....".
The most important thing to know is this: whether you fail to cite your sources deliberately or
inadvertently, you will still be found responsible for the act of plagiarism. Ignorance of
academic regulations or the excuse of sloppy or rushed work does not constitute an acceptable
defence against the charge of plagiarism.
EXAMPLES OF PLAGIARISM
This set of examples provides a range of textual plagiarism from verbatim copying to through
paraphrasing. The comments that follow the examples offer guidance about how a source may be
used and when a source must be cited.
Original source (text)
Yale University Press, 1979. pp.102-103
From time to time this submerged or latent theatre in Hamlet becomes almost overt. It is close to
the surface in Hamlet’s pretense of madness, the “antic disposition” he puts on to protect himself
and prevent his antagonists from plucking out the heart of his mystery. It is even closer to the
surface when hamlet enters his mother’s room and holds up, side by side, the pictures of the two
kings, Old Hamlet and Claudius, and proceeds to describe for her the true nature of the choice
she has made, presenting truth by means of a show. Similarly, when he leaps into the open grave
at Ophelia’s funeral, ranting in high heroic terms, he is acting out for Laertes, and perhaps for
himself as well, the folly of excessive, melodramatic expressions of grief.
Text Example 1
Verbatim plagiarism, or unacknowledged direct quotation (lifted passages are in bold)
Almost all of Shakespeare’s Hamlet can be understood as a play about acting and the theatre. For
example, there is Hamlet’s pretense of madness, the “antic disposition” that he puts on to
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protect himself and prevent his antagonists from plucking out the heart of his mystery.
When hamlet enters his mother’s room he holds up, side by side, the pictures of the two
kings, Old Hamlet and Claudius, and proceeds to describe for her the true nature of the
choice she has made, presenting truth by means of a show. Similarly, when he leaps into the
open grave at Ophelia’s funeral, ranting in high heroic terms, he is acting out for Laertes,
and perhaps for himself as well, the folly of excessive, melodramatic expressions of grief.
Comment – Aside from an opening sentence loosely adapted from the original and reworded
more simply, this entire passage is taken almost word-for-word from the source. The few small
alterations of the source do not relieve the writer of the responsibility to attribute these words to
their original author. A passage from a source may be worth quoting at length if it makes a point
precisely or elegantly. In such cases, copy the passage exactly, place it in quotation marks, and
cite the author.
Text Example 2
bold)
Almost all of Shakespeare’s Hamlet can be understood as a play about acting and the theatre. For
example, in Act 1, hamlet adopts a pretence of madness that he uses to protect himself and
prevent his antagonists from discovering his mission to revenge his father’s murder. He also
presents truth by means of a show when he compares the portraits of Gertrude’s two husbands
in order to describe for her the true nature of the choice she has made. And when he leaps in
Ophelia’s open grave ranting in high heroic terms, Hamlet is acting out the folly of excessive,
melodramatic expressions of grief.
Comment – This passage, in content and structure, is taken wholesale from the source. Although
the writer has rewritten much of the paragraph, and fewer phrases are lifted verbatim from the
source, this is a clear example of plagiarism. Inserting even short phrases from the source into a
new sentence still requires placing quotations around the borrowed words and citing the author.
If even one phrase is good enough to borrow, it must be properly set off by quotation marks. In
the case above, if the writer had rewritten the entire paragraph and only used Alvin Kernan’s
phrase “high heroic terms” without properly quoting and acknowledging its source, the writer
would have plagiarized.
Text Example 3
Paraphrasing the text while maintaining the basic paragraph and sentence structure
Almost all of Shakespeare’s Hamlet can be understood as a play about acting and the other
theatre. For, example, in Act 1, hamlet pretends to be insane in order to make sure his enemies
do not discover his mission to revenge his father’s murder. The theme is even more obvious
when hamlet compares the pictures of his mother’s two husbands to show her what a bad choice
she has made, using their images to reveal the truth. Also when he jumps into Ophelia’s grave,
hurling his challenge to Laertes, hamlet demonstrates the foolishness of exaggerated expressions
of emotion.
Comment – Almost nothing of Kernan’s original language remains in this rewritten paragraph.
However, the key idea, the choice and order of the examples and even the basic structure of the
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original sentences are all taken from the source. Although it would no longer be necessary to use
quotation marks, it would absolutely be necessary to place a citation at the end of this paragraph
to acknowledge that the content is not original. Better still would be to acknowledge the author
in the text by adding a second sentence such as – “Alvin Kernan provides several examples from
the play where these themes become more obvious” – and then citing the source at the end of the
paragraph. In the case where the writer did not try to paraphrase the source’s sentences quite so
closely, but borrowed the main idea and examples from Kernan’s book, an acknowledgement
would still be necessary.
MISREPRESENTING ORIGINAL WORK
Failing to acknowledge one’s sources is not the only form of misrepresenting one’s academic
work. It is also a violation of University regulations to cite a source when in fact the material was
not obtained from that source. A student may resort to false citation if he feels obliged to
document outside sources that he did not really consult; such a violation is subject to the same
penalties as plagiarism. Fabricating or falsifying data of any kind is also a serious academic
violation. If, for example, you discover that the data you collected in a chemistry lab are
somewhat contaminated, useless, or wrong, you must contact the supervisor for guidance.
Perhaps you will receive permission to write your report based on data collected by another
student; perhaps you will be asked to figure out what went wrong with your own lab work. But
in no case should you fabricate data.
Without proper permission, submitting the identical or similar work in more than one course is
also a violation of university regulations.
THE QUESTION OF COLLABORATION
In many courses, particularly in the sciences, where you may work with a laboratory team or on
a group project, some of the work is done in collaboration with fellow students. In such courses,
some of your grade may be based on joint efforts with other students, and some of your grade
may be based on independent work on papers and examinations.
To avoid confusion and possible violations of academic regulations, you must clearly understand
what work must be done independently and what work may be done collaboratively. What is
considered permissible collaboration will vary from course to course. Some supervisors permit
students to do problem sets together and even to turn in an assignment together; other
supervisors allow students to discuss the problems but require them to write up their own
answers; still others prohibit any collaboration at all on take home assignments. The penalty for
copying weekly problem set solutions or assignments can be just as severe as plagiarism on a
major project report.
If you must turn in work and are not sure of the course policy, do your work independently.
Never assume that you have permission to do a problem set or report collaboratively. Given the
variability from supervisor to supervisor, it is also very dangerous to rely on the “rules” from
another course, even within the same department. Too many times, students have turned in
identical or similar problem sets, laboratory reports, or papers, only to discover that they were
operating under a false set of assumptions. The wise thing to do is to ask.
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WORKING HABITS THAT WORK
1. Take complete and careful notes. Whatever note-taking system you use, make sure to
distinguish carefully between any passages copied directly from your source, information
from your source, and your own ideas and comments. When copying passages verbatim from
a source, make sure to use quotation marks and to be precise about recording the page
number(s) of the source. You will save yourself much time and aggravation if you make your
notes accurately and completely the first time around. Students often get into trouble because
their notes are incomplete or confused, and they run out of time to go back to check their
sources.
2. Keep all of your notes until after you have had your graded papers returned to you. If any
question is raised about your work, it is much to your advantage to be able to document your
notes and preliminary drafts of your papers.
3. Be scrupulous in drafting and checking your papers to make sure all words borrowed from
your sources are placed in quotation marks or indented and that all ideas and necessary
information that require citation are followed by a footnote.
4. If you do all of your work − from note-taking to drafts to final version − on a computer,
be especially careful. The ease with which computer text can be copied and pasted, moved
around, and edited can make the work of writing a paper quicker and more efficient, but it can
also lead to serious errors. Make sure whatever notes you have taken from sources are clearly
marked. If you move a phrase, a sentence, or a paragraph from your notes into your paper, be
certain that you also move any quotation marks and citations. Create your footnotes as you go
− for both verbatim quotations and for information that must be attributed. Too often quotation
marks and citations can get lost or confused in the shuffle; don’t rely on your memory or
incomplete or cut-up note files at the end of the process.
A good practice is to keep computer files distinct and to label them well. Don’t start drafting
your paper at the beginning or end of your note file; create a new file. Rather than cutting and
pasting from note files to your paper file, use "copy and paste" instead so that your original
note files remain intact. Be sure to keep track of the file names of the various drafts of your
papers so that you don’t confuse them in the final rush to print and submit your work. Sloppy
work habits and the pressure of deadlines are not valid defences if you are charged with
plagiarism or another violation. It is also a good idea to print out a hard copy of your work
periodically, and to back up your files on diskettes, CDs, or memory keys, in order to avoid a
crisis if your computer fails. Develop a sensible plan to keep track of your work on the
computer and stick to it.
5. Understand the difference between primary and secondary sources, but know that you
must cite quotations, ideas, and information from both. Most students learn how to quote
from a primary source. For example, if you are writing a paper about The Joker of Seville or
the Laws of Barbados, you know to put any quotation from that primary source in quotation
marks. Too often, however, students are not trained to use secondary sources, such as an essay
of literary criticism on Walcott’s novel or a scholarly book on the Laws of Barbados. Students
in disciplinary hearings sometimes claim that they did not know that ideas or words from
secondary sources require citation, or that they thought such material was common knowledge.
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However, the principle is clear: you must always distinguish your own words and ideas from
the words and ideas of others, whether in primary or secondary sources.
6. Do not rely on a single secondary source when doing a research paper. Try to find
multiple sources that provide varying perspectives and draw different conclusions on your
research topic. Your paper will be better if you respond to a variety of sources, and you will
avoid any possibility of depending so much on a single source that you can be charged with
plagiarism.
7. Whenever possible, show all of your work in problems sets that require calculation.
8. Be sure you understand the supervisor’s expectations and guidelines for collaborating on
assignments such as lab reports, problem sets, and research projects. If the rules for the course
are not explicit, do yourself (and your fellow students) a favour and ask the supervisor to
clarify them.
9. Be extra careful to verify the accuracy or validity of information obtained from electronic
sources. Be sure to cite such sources just as you would print sources.
10. If you are unsure whether or not to cite a source, ask your supervisor. If that is not possible,
follow the basic rule: when in doubt, cite.
11. Be your own hardest critic. Reread your papers to see how much is your own and how
much is quotation or paraphrase from primary or secondary sources. If your paper is replete
with ideas and quotations from your sources, are you confident that you have found some
idea or thesis of your own to argue? If there are almost no citations, have you done sufficient
reading and research to be confident in your information and analysis?
12. Be sure you understand your supervisor’s expectations for your work. Are you supposed
to be summarizing a source or analyzing it? Are you expected to go beyond the assigned
readings? Are you expected to use two sources? Six?
13. Be cautious about using notes belonging to other students, even if you are in the
preliminary stage of writing your own paper or doing your own problem set. Keeping others’
ideas distinct from your own is an important way to protect the integrity of your own
academic work and to avoid unintended plagiarism.
14. If you do not understand an assignment or need additional time to complete it, ask your
supervisor. Students occasionally, out of desperation, make the wrong choice by plagiarizing
their sources rather than requesting an extension.
15. This last piece of advice is the hardest of all to follow: give yourself enough time to do
your work well and carefully. Proper citation takes time. Avoid last-minute rushes when
the pressure of the due date may tempt you to get sloppy or cut corners you know you
shouldn’t just to finish. At 5 a.m. after an all-nighter, you may not be thinking clearly enough
to make the right choices about properly acknowledging your sources. Not to mention that
you are hardly likely to be doing your finest work at that hour.
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These regulations regarding safe laboratory practice are intended to help students work safely
with chemicals. Safe laboratory practice is based on understanding and respecting chemicals, not
fearing them. These guidelines cover ordinary hazards and apply to any laboratory experiments
students will encounter. During laboratory lectures, the instructor will discuss specific safety
precautions relevant to any one experiment. The laboratory textbook or manual will point out
specific hazards and precautions. Before beginning an experiment, have this information on hand
and understand it thoroughly. Do not hesitate to consult if you have questions about an
experiment or these regulations.
It is the students’ responsibility to read and follow the safety regulations in this manual and to
keep it with them in the laboratory. Any other safety handouts or special precautions mentioned
during laboratory lecture must also be observed.
Failure to follow laboratory safety rules and procedures may cause injury to students or their
colleagues. Call unsafe practices by colleagues to their attention and (if necessary) to the
attention of the instructor.
I. Safety Regulations and Precautions
Accidents in the laboratory are the result of carelessness or ignorance by students or their
neighbours. Stay alert and pay constant attention to your own and to your neighbours’
actions. The safety precautions outlined below will be useless unless students plan every
experiment, understand every operation, and think through the consequences of every procedure
before they perform it. The following kinds of accidents are common: fire, explosion, chemical
& thermal burns, cuts from broken tubing & thermometers, absorption of toxic (but non-
corrosive) chemicals through the skin, and inhalation of toxic fumes. Less common (but
nonetheless dangerous) is the ingestion of toxic chemicals. Each of these accident types is
discussed in a general way below; more specific reference to certain hazards will be found in the
experiment information handouts.
1. Laboratory Use: Students may work in instructional laboratories only during regularly
scheduled times on authorized experiments with supervision by an authorized teaching
assistant or member of the faculty. Working alone in the laboratory is strictly forbidden.
2. Safety Equipment: It is the students’ responsibility to know the location and operation
of fire extinguishers, shower & eye wash stations, fire blankets, and any other safety
equipment provided in the laboratory.
3. Eye Protection: SAFETY GOGGLES MUST BE WORN AT ALL TIMES when in
the laboratory. Students who do not follow the eye-protection requirement will be asked
to leave the laboratory. It is more the rule than the exception for flying glass and
spattered chemicals to hit the face. Even if students are not conducting a reaction or other
operation, their neighbors are working and may have an accident which spatters
themselves or other students.
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4. Clothing: Long hair and billowy clothing must be confined when in the laboratory.
Shoes are mandatory; aprons are recommended. Sandals (or opened-toed shoes) and
shorts (or short skirts) are inappropriate.
5. Fire: Open flames are to be used only with permission in specified locations. Make it a
working rule that water is the only nonflammable liquid you are likely to encounter. Treat
all others in the vicinity of a flame as you would gasoline. Specifically - never heat any
organic solvent with a flame in an open vessel (such as a test tube, Erlenmeyer flask, or
beaker). Such solvents should be heated with a steambath (not a hotplate) and the
flammable vapors drawn off with an aspirator tube by working in a hood. Never keep a
volatile solvent (such as ether, acetone, or benzene) in a beaker or an open Erlenmeyer
flask. The vapors will creep along the bench, ignite, and flash back if they reach a flame.
It is the students’ responsibility to know where the nearest shower and fire extinguisher
are located and how to operate them. Always point an extinguisher at the outer reaches of
a flame and work inward. Call for additional extinguishers.
6. Explosion: Never heat a closed system or conduct a reaction in a closed system (unless
specifically directed to perform the latter process and then only with frequent venting).
Before starting a distillation or chemical reaction, make certain that the system is vented.
The result of an explosion is flying glass and spattered chemicals, both usually hot and
corrosive.
7. Chemical and Thermal Burns: Many inorganic chemicals (such as the mineral acids
and alkalis) are corrosive to the skin and eyes. Likewise, many organic chemicals (such
as acid halides, phenols, and so on) are corrosive and often toxic. If they are spilled on
the benchtop, in the hood, or on a shelf, clean them up before you leave the spill area.
8. Cuts: The most common laboratory accident is the cut received while attempting to force
glass tubing into rubber stopper or rubber tubing onto a stirring rod, a thermometer, or the
sidearm of a filtration flask. Lubricate the stopper and use a gentle rotating pressure on
the glass part. Severed nerves and tendons are common injuries caused by improper
manipulation of glass tubes and thermometers. Always pull rather than push on the glass
when possible. In addition to these safety precautions, remember to use caution when
inserting syringe needles into plastic tubing.
9. Absorption of Chemicals: Keep chemicals off the skin. Many organic substances are not
corrosive, do not burn the skin, or do not seem to have any serious effects; nevertheless,
they are absorbed through the skin and may have serious consequences. Other chemicals
will give a serious allergic reaction upon repeated exposure, as evidenced by severe
dermatitis. For the organic laboratory, it may be advisable to wear gloves when handling
some reagents. The best type of glove to wear depends upon the reagent used and specific
information will be given in lab lecture for individual chemicals. Gloves provide only a
temporary layer of protection against chemicals on your skin. If gloves become
discolored, develop holes, or begin to deteriorate, remove them immediately, wash your
hands thoroughly and get a new pair.
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10. Inhalation of Chemicals: Keep your nose away from organic chemicals. Many of the
common solvents are toxic if inhaled in any quantity or for any length of time. Do not
evaporate excess solvents in the laboratory; on the contrary, use the hood or a suitable
distillation apparatus with a condenser. Some compounds (such as acetyl chloride) will
severely irritate membranes in the eyes, nose, throat and lungs, while others (such as
benzyl chloride) induce eye irritation and tears. When in doubt, use the hood, or better
yet, consult the laboratory instructor about the chemicals required for a particular
experiment.
11. Ingestion of Chemicals: The following are common ways of accidentally ingesting
harmful chemicals:
(d) By using chemicals taken from the laboratory.
i. Pipettes must be fitted with suction bulbs to transfer chemicals.
Never use mouth suction.
ii. Wash your hands before handling anything (cigarettes, chewing gum or
food etc.) that goes into the mouth. Always wash your hands when you
leave the laboratory.
iii. Do not eat or drink in the laboratory. Use water fountains outside the
laboratory when thirsty - not laboratory faucets.
iv. Never use chemicals (such as salt and sugar) from the laboratory or
stockroom as food additives. The source containers may be contaminated
or mislabeled.
v. Never use laboratory glassware as food and drink containers.
vi. Never store food or drink in a laboratory refrigerator or ice machine;
Never consume ice from an ice machine.
12. Accident Reports: All accidents (including contact with chemicals, any cuts, burns, or
inhalation of fumes) must be reported to an instructor immediately. Any treatment
beyond emergency first aid will be referred to the Student Health Clinic. Severe
emergencies will be referred to the Hospital Emergency Room.
II. EMERGENCY PROCEDURES IN THE CHEMISTRY LABORATORY
Fire: 311
Ambulance: 511
Police: 211
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1. Critical Emergencies are rare. The first priority (besides yelling for help) is to reduce
or eliminate the hazard: turn off gas, open the windows, shut off the power supplies, and
so on. If the victim isn’t breathing, immediately do what you can to get breathing started.
Oftentimes, carefully straightening the victim’s neck (jutting the jaw slightly forward)
works effectively. If it doesn’t, start mouth-to-mouth resuscitation. If the victim is
breathing and out of immediate danger, you can wait for help to arrive. Call the
ambulance and describe as accurately as possible what happened. Whenever an
ambulance is called, someone should wait by the building entrance to guide the medical
crew to the accident site.
2. Report all accidents immediately to the laboratory instructor or a staff member. If
practical, the staff member should administer first aid. The suggestions given here are
meant for emergency use, that is, only when it is necessary to administer first aid. All
minor cuts and burns should receive medical attention. Always err on the side of caution.
3. In any accident involving one or more chemicals, make every effort to find out the
names of the chemicals so that appropriate measures can be taken at the hospital.
4. When medical attention is required, call the Emergency Room with information about
the injury and the chemical(s) involved. Accompany the victim to the hospital. If the
accident victim cannot be moved, call an ambulance.
(a) Eyes. Get help immediately! Chemicals in the eyes must be removed at once by
flooding with large quantities of water. Help the victim. Use the eye wash station
if possible. Otherwise, place the victim on the floor, by force if necessary. One
person should straddle the victim with knees on the floor, pouring a moderate
stream of water from a flask or beaker onto the bridge of the victim’s nose so that
both eyes are flooded. Another person should squat at the head of the victim and
roll back both eyelids; use the thumb and forefinger to spread the eyelids open;
the victim will not be able to do this voluntarily. Use several litres of water. When
it is reasonably certain that the excess chemicals have been washed away, take the
victim to the Emergency Room for immediate medical attention.
(b) Chemicals on the skin. All chemicals that come in contact with the body should
be considered toxic; they should be washed off completely with soap and water
even if they do not appear to be corrosive. Wash off corrosive substances by
flooding the skin with tap water, using the safety shower if necessary, and
stripping off any clothing and shoes that are soaked with chemicals.
Acids: After washing the skin thoroughly with water, rub on a paste of sodium
bicarbonate and water; do not use the paste on burns to the eyes.
Alkalis: After washing the skin thoroughly with water, apply a 1% solution of
boric acid (available in the laboratory).
Bromine: Work fast. Wash the excess bromine off the skin and immediately rub
the entire area with a generous amount of glycerine (available in the laboratory).
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(c) Inhalation of chemicals. Get fresh air. Report all incidents (to the Laboratory
instructor) when more than a smell is inhaled or when prolonged exposure to
laboratory fumes has induced faintness or a headache.
(d) Ingestion of chemicals. Call the Poison Centre for recommended treatment.
Vomiting can be dangerous if the vomit gets into the lungs; most serious
poisoning problems are best treated in the Hospital Emergency Room. If
necessary, induce vomiting by having the victim swallow as much warm water as
possible, as rapidly as possible. Adding one or two teaspoons of table salt per
glass of warm water will help. Vomiting should be encouraged by having the
victim swallow additional water until the vomited liquid is clear.
(e) Cuts: Serious bleeding should be controlled by applying direct pressure to the
wound with clean gauze or a cloth pad. Minor cuts should be washed with tap
water, allowed to bleed briefly, pressed with a clean cotton pad or piece of gauze,
and then covered with gauze to keep the wound clean. More sever cuts (especially
those involving glass or other objects in the wound) require medical attention.
(f) Clothing fires. Call for help and a blanket. When someone’s clothing catches
fire, the flame and smoke can rise and be inhaled. Unless a shower is immediately
available or can be reached without inhalation damage, place the victim prone on
the floor (forcibly if necessary) and roll in a blanket. Put out the flames with your
hands or smother them with heavy garments.
(g) Thermal burns. Any burn that is extensive, severe, or involves the eyes of face
should be considered serious. A burn involving the respiratory tract could be
critical. Call the ambulance. Minor burns should be treated by washing the
burned area with cold tap water. Wrapping the burned area lightly with a clean
wet cloth reduces pain. Do not use ointments or salves unless instructed by a
physician.
(h) Faintness. If the victim is conscious, have that person sit down and place the head
between the knees. Give support to prevent a fall. If the person is weak or has
fainted, lay the victim on the floor; raise the feet and legs a little above the level
of the head. Call for medical assistance if the victim fails to regain consciousness
within half a minute. Insist that the person remain quiet (sitting or lying down) for
a few minutes after recovery unless it is necessary to take the victim to the
hospital for treatment.
Note: All people have some reaction to being injured; often they become faint. Always require a
person to be seated while being examined or receiving treatment. One should not add a fractured
skull to the original injury as a result of the victim falling over in a faint.
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DURING PREGNANCY
The Department of Biological and Chemical Sciences acknowledges that some laboratory
environments may present possible medical hazards to an unborn child. The Department
of Biological and Chemical Sciences is committed to the concept and principles of ALARA
(as low as reasonably achievable). As part of this effort, it is also the policy of The
Department of Biological and Chemical Sciences to establish procedures to minimize the
potential for adverse health effects to the unborn child of a mother who attends class in an
environment in which reproductive hazards may be present.
The following environment is an area of concern:
CHEMICAL EXPOSURES & ENVIRONMENTS: Certain chemicals and processes may
represent a risk to an unborn child. A student who works in an environment in which hazardous
chemicals or processes are used should immediately notify her instructor, Head of Department or
Dean once pregnancy is suspected. The Instructor, Head of Department or Dean (with support
from the Safety Committee) must evaluate the work environment for the presence of
reproductive hazards and then determine and communicate the risks for the unborn child. Based
on this evaluation, the Department of Biological and Chemical Sciences may recommend
changes in the environment and activities of the pregnant student or an academic course, or other
appropriate accommodation in which there is minimal exposure to the hazard.
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RESPECT.
OUT of eyes, lungs, mouth
AWAY from flames
EAT, DRINK, OR SMOKE in the laboratory
ALWAYS: WEAR goggles
USE common sense, caution, and good laboratory
practice in the manipulation and storage of chemicals.
WASH HANDS BEFORE eating.
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Column preparation
Columns using silica gel or florisil are best prepared by the slurry method.
Column chromatography
a. Rule of thumb: 1 gram of compound per 30 g of adsorbent. This can vary somewhat
depending on your system.
b. Volume of fractions: 100 mL for every gram put on the column.
c. Mass balance: Know what went on so that you can judge when everything has been
removed. Tare 50 mL Erlenmeyer flasks.
d. Solvents for column chromatography must be distilled to remove any oil or other residue
that will contaminate your fractions.
Chloroform recovery
When large amounts of this solvent are being used for, say, column chromatography, it should be
distilled and re-used, inasmuch as chloroform is very expensive. Pure commercial chloroform is
stabilized against decomposition (to the highly poisonous phosgene) by the addition of
approximately 0.75% EtOH. An appropriate amount of EtOH should thus be added to recovered
CHCl3. In recovering CHCl3 that is contaminated with benzene, simply record the boiling range
of the fraction and re-use where such a mixture of benzene-chloroform is called for.
Destroying water-sensitive organometallic intermediates
should be handled carefully by
a. cooling the reaction flask first with an ice bath and
b. adding cold water (slowly) or other decomposition agents.
Distillation
Every time you stop a distillation and then restart it, a fresh boiling chip must be added. The
same applies to recrystallization.
Filtration by gravity
“Flute” your filter paper for much more efficient filtration by folding in half, then in quarters,
then in eights, then in sixteenths, then unfolding completely.
Ice baths
Always add water (or other suitable fluid) to a crushed ice bath in order to provide proper heat
exchange between vessel and frozen phase. Cracked ice by itself does not do the job (too many
air pockets)! For ice bath temperatures a few degrees below zero, have handy a saturated solution
of NaCl (brine) and use it as the heat-exchange fluid.
Molecular sieves
Pure distilled solvents can be stored over these. Sieves of various sizes scavenge water very
efficiently when the latter is in trace amounts.
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Water sensitive reactions need to be protected especially carefully (drying tubes, glassware dried
in the oven then cooled in a large desiccator).
Nitrogen/Argon
Acceptable arrangements always start with the N2/Ar being directed through a drying tower
containing, for instance, Drierite.
a. N2/Ar can pass through your vessel and then be bubbled through a viscous fluid
(mercury, glycerol, etc.) so as to provide some “resistance” to the flow. That is to say,
never allow N2/Ar to flow “out the other side” freely.
b. Alternatively, N2/Ar can “dead end” at your reaction flask, with a branch on the N2/Ar
line leading to a suitable bubbler situated between the drying tower and the vessel.
c. Alternatively, N2/Ar can be connected by way of a three way stopcock to a manometer
and aspirator so that a vessel can be evacuated and flushed sequentially.
d. Alternatively, a balloon can be used (separate entry).
Ovens
Glassware with more than a mL of flammable organic solvent in them should not be dried in
ovens due to the obvious fire and explosion hazard.
Reactions requiring dry glassware
Dry the glassware overnight in the oven at temperatures in excess of 100 °C. Remove the
glassware, assembling it while hot, with any opening to the atmosphere being “closed” with a
drying tube. Alternatively, let the glassware cool down in a desiccator the opening to which is
also protected by a drying tube. This procedure is vital when running alkyllithium or Grignard
reactions.
Recrystallization
Beakers and Erlenmeyers work best. Test tubes are fine for very small quantities.
Refrigerators
a. Open beakers of any solvent should never be stored in refrigerators, even though these
supposedly have been modified so as to be “explosion proof”.
b. At the end of your project, check with your supervisor(s) so as to determine what can be
discarded.
Stopcock grease
Avoid putting high vacuum stopcock grease on glassware unless necessary (e.g. vacuum
distillation). Grease can contaminate samples very easily. You can remove grease with hexane
and then acetone.
Teflon stopcocks
These tend to conform to the shape of the barrel (of a separatory funnel or column). Thus, when
storing these, leave the stopcock in a loosened condition lest they freeze – and they will!
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Thin-layer chr