PHYSICAL AND ANALYTICAL CHEMISTRY LABORATORY, CHEMISTRY UN3085 AUTUMN, 2025
In memoriam of Professor George Kessler Fraenkel (1921-2009)
Professor Fraenkel pionered research in the field of electron spin resonance (ESR). He is credited with recording the first electron paramagnetic resonance (EPR) spectrum of quinones. His work in the early 1950s contributed significantly to the development of EPR spectroscopy and its application to organic molecules. Professor Fraenkel acted as the chairman of the Department of Chemistry from 1965 to 1968 and served as the dean of GSAS from 1968 to 1983 during the Vietnam war protests. He taught the Physical and Analytical Chemistry Laboratory course from 1984 till his retirement in 1991.
GENERAL INFORMATION, LIST OF EXPERIMENTS, AND LABORATORY RULES
GENERAL INFORMATIONLaboratory location and hours: Room 222 HavemeyerTuesday: 12:00-6:00 P.M.Instructors: Luis Avila359 Chandler Labs in Havemeyerlaa4@columbia.edu(212) 854-8587Office Hours by appointmentTeaching Assistant:Vicente Galiciavg2619@columbia.edu(212) 854-8433Office Hours by appointment
COURSE ORGANIZATION
According to the American Chemical Society ^(1){ }^{1}, many trained physical chemists pursue careers as analytical chemists. In these roles, the Physical Chemists use their expertise in thermodynamics, transport phenomena, chemical kinetics, quantum mechanics, and spectroscopy to understand and develop instrumental analytical techniques. Those who move into management positions often supervise other scientists, assess departmental needs and goals, and collaborate with business managers within their organizations.
In the physical and analytical chemistry laboratory course, you will engage in collaborative experiments to deepen your understanding of the experimental skills and topics you will need as professional chemists. The course is structured as follows:
First Semester (UN3085): You will focus on experiments related to thermodynamics, physical BB kinetics (transport phenomena), and chemical kinetics. CC
Second Semester (UN3086): The emphasis will shift to quantum mechanics and spectroscopy. To enhance your learning, the first semester is divided into three sequential four-week learning blocks:
Block A: Thermodynamics
Block B: Transport phenomena (Physical kinetics)
Block C: Chemical kinetics
During each learning block, you will learn the course topics by conducting experiments, analyzing the results, and discussing the techniques and concepts with your peers as depicted in Tables 1, 2, and 3 below.
Table 1. Experiment classification by learning block
Dynamic light Scattering DLS system, Atomic Force Microscope (AFM), Optical and FTIR microscope.
6
Polyoxometalate on Graphite
Pine Inc. WaveDriver 20 Bipotentiostat. Patterned electrodes
7
ZnO Nanoparticle growth Kinetics
UV-Vis Beckman Coulter single-beam Spectrometer.
8
Colloidal silica particles
DLS, AFM and Optical Microscopy.
9
Enzyme Kinetics
Varian Cary UV/Vis/NIR double-beam spectrometer, water circulator.
# Description Instrumentation
1 Dimerization of Formic Acid T-controlled 10 cm pathlength IR-gas cell. Water circulator, FTIR Spectrometer transmission mode, Schlenk Line.
2 Sodium Dodecyl Sulfate Micellization Conductimetry probe-coupled MicroLAB ADC, Thermocouple, Constant Temperature liquid Reactor, and T-controlled Water circulation bath.
3 Ring Strain Measurement Thermistor-coupled MicroLAB ADC, Thermocouple, Parr Bomb Calorimeter.
4 Ferrocene, and C60 Electrochemistry Eclipse BASI Potentiostat, Microelectrodes.
5 PS Latex Polymerization Dynamic light Scattering DLS system, Atomic Force Microscope (AFM), Optical and FTIR microscope.
6 Polyoxometalate on Graphite Pine Inc. WaveDriver 20 Bipotentiostat. Patterned electrodes
7 ZnO Nanoparticle growth Kinetics UV-Vis Beckman Coulter single-beam Spectrometer.
8 Colloidal silica particles DLS, AFM and Optical Microscopy.
9 Enzyme Kinetics Varian Cary UV/Vis/NIR double-beam spectrometer, water circulator.| # | Description | Instrumentation |
| :--- | :--- | :--- |
| 1 | Dimerization of Formic Acid | T-controlled 10 cm pathlength IR-gas cell. Water circulator, FTIR Spectrometer transmission mode, Schlenk Line. |
| 2 | Sodium Dodecyl Sulfate Micellization | Conductimetry probe-coupled MicroLAB ADC, Thermocouple, Constant Temperature liquid Reactor, and T-controlled Water circulation bath. |
| 3 | Ring Strain Measurement | Thermistor-coupled MicroLAB ADC, Thermocouple, Parr Bomb Calorimeter. |
| 4 | Ferrocene, and C60 Electrochemistry | Eclipse BASI Potentiostat, Microelectrodes. |
| 5 | PS Latex Polymerization | Dynamic light Scattering DLS system, Atomic Force Microscope (AFM), Optical and FTIR microscope. |
| 6 | Polyoxometalate on Graphite | Pine Inc. WaveDriver 20 Bipotentiostat. Patterned electrodes |
| 7 | ZnO Nanoparticle growth Kinetics | UV-Vis Beckman Coulter single-beam Spectrometer. |
| 8 | Colloidal silica particles | DLS, AFM and Optical Microscopy. |
| 9 | Enzyme Kinetics | Varian Cary UV/Vis/NIR double-beam spectrometer, water circulator. |
ASSESSMENT (Refer to the class schedule on page 10)
Quizzes 1 pM
On the first (9//16)(9 / 16), fifth (10//14)(10 / 14), and ninth (11//18)(11 / 18) weeks (green shading on the schedule), you will be given a 20 -minute quiz on the experiment you will be performing.
Peer-tutoring
To assure your comprehension of the material covered in each learning block, on the second (9/23), third (9//30)(9 / 30), sixth (10//21)(10 / 21), seventh (10//28)(10 / 28), tenth (11//25)(11 / 25), and eleventh (12//02)(12 / 02) weeks (yellow shading on the schedule) you will be expected to explain to each other the experiment you performed the previous week before starting the experiment. For this purpose, you must distribute the tasks among the group members, i.e., you will be either a teacher or a learner according to the group plan. However, you cannot always play the learner role and hence minimize your teaching.
For peer tutoring, plan to cover the experimental procedure, safety hazards, theoretical principles, instrumentation handling, data treatment, and error analysis for the given experiment. You will responsibly evaluate each other's ability to facilitate learning using an assessment form prepared for that purpose.
Reporting
due nextweek
You will present your experimental findings as individual written reports (W)(\mathrm{W}), oral (O)(\mathrm{O}), or poster (P)(\mathrm{P}) group presentations as indicated on the schedule on page 10 . Specifics about the reports are given below. poster board about the
WRITTEN REPORTS (W)
Hand in your written report to the TA and have it signed at the beginning of the next period. Each laboratory report is divided into sections, which are graded separately. These sections include the title, abstract, introduction, experimental method, results, discussion and references.
Title page (5 points): Course title (header), title of experiment, your name, lab partner, date performed, date submitted.
Abstract (5 points): After you have written the entire report, briefly state the purpose of the experiment, indicate the theoretical and experimental plan used, summarize the main findings, and point out major conclusions (50 to 120 words). Do not evaluate, or comment on conclusions in the main text.
Introduction (10 points): Using your own words, describe the theoretical background upon which the experiment is based. Include references to all sources used.
Experimental Method (10 points): Indicate specific details of the apparatus used (e.g., Absorbance measurements at 255 nm were made with a Varian Cary-5000 double-beam UV-Vis-NIR spectrophotometer); physical properties of chemicals used, number of runs, experimental conditions (concentration range, temperature, pressure). Mention any modification from the procedure described in the handout.
Data and Results (40 points): Tabulate all data used in the calculation of results, number the Tables and graphs, and title them properly. Perform error analysis of your data. Provide a typical sample calculation both for the results obtained and the associated uncertainty. Use a different numbering pattern for Tables, figures, graphs and equations.
Discussion and Conclusions (20 points): The purpose of the discussion is to expand on your observations or to comment on possible reasons of poor results. Make a quantitative comparison of your results with literature values. Evaluate the experiment's accuracy and precision. Answer the questions given in the handout. Summarize the main conclusions and results.
References (10 points): Bibliographic styles vary depending on the journal, which specifies the format to be used for citations. The following citation guidelines are specific to the Journal of Physical Chemistry. In this format, you should number the citations sequentially as they appear in the text and provide a list of these references at the end of your report, as demonstrated in the example below.
a. Citing an article:
(1) Giancarlo L, Fang H., Avila L., Fine, L., Flynn G. Journal of Chemical Education 2000, 77, 66.
b. Citing a book:
(2) Szafran, Z.; Pike, R.; Singh, M. Microscale Inorganic Chemistry, John Wiley & Sons, Inc Publishers: New York, 1991.
c. Citing a chapter in a book of several authors:
(3) Avila, L.; Fine, L. Infrared spectroscopy and education. In Handbook of vibrational spectroscopy; Chalmers, J. M., Griffiths, P. R., Eds.; John Wiley & Sons, Ltd.: Chichester, UK, 2002; Vol. 4; pp 3207.
To better handle bibliographic files, download the citation management software of your choice, available free of charge to all current students, faculty and staff from the Columbia University Libraries Research Support services: http://www.columbia.edu/cu/lweb/help/howto/endnote/index.html
GROUP ORAL PRESENTATIONS (O)
On weeks 4^("th "),8^("th ")4^{\text {th }}, 8^{\text {th }}, and 12^("th ")12^{\text {th }} (orange shading on the class schedule, page 10 ) you will present your experimental findings on the experiments assigned to you as group oral presentations (page 10 reporting schedule) in room (TBA) starting at 12:00 pm. Prepare a 20 -minute slide presentation about the experiment performed and the results you obtained. Use the basic format followed for the written lab reports, i.e., explain what you measured, how you measured it, what you found, and how you interpreted your results.
The documentation for the oral presentations consists of the copy pages from your laboratory notebook, showing all the data work-up and calculations, and it is due a week after the experiment is performed.
GROUP POSTER PRESENTATION (P)
You will display your poster on weeks 4^("th "),8^("th ")4^{\text {th }}, 8^{\text {th }}, and 12^("th ")12^{\text {th }} (orange shading on the schedule, page 10) starting at 12:00 p.m. in room (TBA). The stages for preparing a poster are described below.
The documentation for the poster presentations consists of the copy pages from your laboratory notebook, showing all the data work-up and calculations, and it is due a week after the experiment is performed.
I. Getting ideas:
The Chemistry Research Complex consists of three buildings: Havemeyer Hall (Central building), the Chandler labs (West wing), and Havemeyer extension (East wing). Each research group has some of its work displayed in the form of posters in the hallways of the chemistry research complex; visiting the different groups will help you configure a good poster.
II. Constructing:
We will provide you with a poster board at the beginning of the course. You must reuse the board along the semester so avoid using glue to post the information presented.
Divide the poster into sections such as title, introduction, methods, results and conclusions. Indicate by numbering or lettering the order in which these sections should be read; arrows can be used for this same purpose.
Improve the graphic impact of the poster by mounting the sheets on colored construction paper. However, keep in mind that simplicity and ease of reading are more important than artistic flamboyance.
Choose a simple font such as Times New Roman, Palatino or Helvetica.
Use a larger font size, bold or underline to make something stand out. Do not overuse outlining and shadowing.
The title should be in very large type, 84 pt. or larger. Your name should also be written in large type such as 72 pt .
Do not enlarge photocopies.
Text on panels should be between 18 and 24 pt. to be legible. Use double or 1.5 spacing. Focus selectively on major findings (present the details in a handout). Framing the text by putting a box around it will also help readers to focus.
Use ChemDraw to represent chemical reactions.
Use graphs, charts, figures, pictures, or lists to convey your message effectively. Avoid using tables unless they clearly enhance the presentation of the poster. Include references in a smaller font due to space limitations.
Presenting:
Explain what you did, how you did it, and your findings using your poster as guidance. Avoid sounding as if you have memorized a script; be excited about your work.
Address questions as appropriate.
NUTS AND BOLTS
(a) PLANNING THE EXPERIMENTS
In consultation with your group peers, instructor, and TA, thoroughly prepare for each experiment before the laboratory session. Develop a plan of action to safely perform the procedures. Some experiments will involve theoretical and/or experimental principles and techniques that may be unfamiliar to you and will require considerable study. We encourage full collaboration within your peer group to work through challenging aspects and seek advice from the laboratory instructors as needed. Complete any calculations that can be done in advance before arriving at the laboratory. Some experiments will take the entire period, while others may take less time, assuming no mishaps occur.
GENERAL LABORATORY POLICIES
Visit the EH&S Environmental Health and Safety at Columbia site and open the Lab Safety, Chemical Hygiene and Hazardous Management Rascal course.
Take the TC4951 course, which link I pasted below.
Keep all equipment and working areas in the laboratory clean. At the end of the laboratory period, you are required to clean up your work area and common work areas as required by the instructor.
Wash the glassware and properly discard chemical waste.
CONSULT AN INSTRUCTOR FIRST when in doubt about how to use a piece of equipment or apparatus.
(b) LABORATORY NOTEBOOKS
All data and other primary information on an experiment must be recorded directly in your laboratory notebook. Be sure that the original (white) copy of all data is clear and legible. At the end of the period, you must submit the copy of your data. Spectra should be submitted with your laboratory report as appendices. Reports without these data will not be accepted. DO NOT USE LOOSE SHEETS OF PAPER FOR ANY DATA TAKEN IN THE LABORATORY.
Be certain that your name, the name of your partners, the date the data were taken, and the (short) title of each experiment is written on each page before you start taking data. Write subtitles for each part of the experiment. Clearly indicate with titles, headings, and comments what the data refer to, what the units are, and enter data in chronological order. If for some reason the data is not entered
in chronological order, note this fact in your lab notebook.
Indicate any changes from the prescribed procedure that may have occurred. Fully record any difficulties encountered as well as any identifying numbers and/or calibrations on special equipment.
(c) LATE REPORT PENALTIES
I. FIVE PERCENTAGE POINTS WILL BE IMPOSED FOR EACH DAY (EXCLUDING WEEKENDS AND HOLIDAYS) THAT A SPECIFIC ASSIGNMENT IS LATE. UP TO TWO WEEKS (PENALTY OF 30 POINTS) UNLESS AN EXTENSION HAS BEEN GRANTED FOR UNUSUAL AND EXTENUATING CIRCUMSTANCES.
II. A student with more than three ASSIGNMENTS WITH THE MAXIMUM PENALTY AUTOMATICALLY RECEIVES A FAILING GRADE (F) IN THE COURSE UNLESS SPECIAL DISPENSATION IS MADE FOR UNUSUAL AND EXTENUATING CIRCUMSTANCES.
(d) ACADEMIC HONESTY
Columbia University takes academic honesty very seriously. Any student caught plagiarizing from any source will receive a grade of ZERO ( 0 ) on the assignment and will be reported to the Office of Judicial Affairs and Community Standards (OJA). http://www.college.columbia.edu/facultyadmin/academicintegrity/responding)
It is your responsibility to understand what constitutes plagiarism and to consult any of the instructors if you have questions.
(f) ATTENDANCE
Attendance is mandatory both in the laboratory and at all lectures and student presentations. Please notify the instructors at least one week in advance if you have a conflict or provide a doctor's note in case of illness.
(g) GRADES
Your final grade will be determined by the following weighting scheme:
Laboratory reports 50%50 \%
Peer Tutoring 10%10 \%
Peer Feedback 15%
Attendance 15%
Quizzes 10%
100% Points will be deducted for failure to observe laboratory safety guidelines and for poor laboratory skills
observe not on lap
(h) DIRECTORY
Group
Name
UNI
Flynn Group Josh scaning microsang
Anyah
aff2127
Litian
lz2964
Camilo
rn2635
Bent Group #209. piprical chemist
Jordan
xw2970
Min Jae
mk4435
distribution
Eisenthal Group
Savannah
sb4900
Edward
es4113
Gabrielle
gmc2192
Group Name UNI
Flynn Group Josh scaning microsang Anyah aff2127
Litian lz2964
Camilo rn2635
Bent Group #209. piprical chemist Jordan xw2970
Min Jae mk4435
distribution Eisenthal Group Savannah sb4900
Edward es4113
Gabrielle gmc2192| | Group | Name | UNI |
| :--- | :--- | :--- | :--- |
| | Flynn Group Josh scaning microsang | Anyah | aff2127 |
| | | Litian | lz2964 |
| | | Camilo | rn2635 |
| | Bent Group #209. piprical chemist | Jordan | xw2970 |
| | | Min Jae | mk4435 |
| | | | |
| distribution | Eisenthal Group | Savannah | sb4900 |
| | | Edward | es4113 |
| | | Gabrielle | gmc2192 |
EXPERIMENT
GROUP E1 E2 E3 E4 E5 E6 E7 E8 E9
Group I W O P P W O O P W
Group II P W O W O P P W O
Group III O P W O P W W O P| | EXPERIMENT | | | | | | | | |
| :--- | :--- | :--- | :--- | :--- | :--- | :--- | :--- | :--- | :--- |
| GROUP | E1 | E2 | E3 | E4 | E5 | E6 | E7 | E8 | E9 |
| Group I | W | O | P | P | W | O | O | P | W |
| Group II | P | W | O | W | O | P | P | W | O |
| Group III | O | P | W | O | P | W | W | O | P |