Analytical Instrumental Laboratory

CHEM 314; Spring 2018

Course Name: CHEM 314, 3 credits
Prerequisites: CHEM 212
Location: Reichardt 165 (lecture); Reichardt 245 (lab)
Meeting Time: M 9:15-10:15am (lecture), MW 2:15-5:15pm (lab)
Final: Friday, May 4 1-3 pm (based on lab meeting time)
Instructor: Dr. Jingqiu Mao
Office: Reichardt 188
Phone: 907-474-7118
Email: jmao2 @alaska.edu
Office Hours: T&TH 2-4PM (other times by appointment).

Recommended Materials:
Skoog, Holler and Crouch, Principles of Instrumental Analysis
Harris, Quantitative Chemical Analysis.
** Current editions of textbooks on reserve in Rasmussen Library for 2 hr in-library use**

Course Description: A laboratory course focusing on the acquisition and interpretation of

chromatographic and spectroscopic data for quantitative chemical measurements. Students will learn
effective experimental planning and execution, critical evaluation of experimental data and written
communication in the context of the chemical sciences. Much of this course is student-directed and
project based. Students are expected to carefully prepare, plan, and execute experiments with
minimal instructor input. CHEM 314 builds on previous experience with analytical chemistry (eg
CHEM 212).

Instructional Methods: This class is based on characterizing several products given to each
student. Throughout the semester, students will use a variety of instrumentation to characterize their
products both individually and in groups. In lecture, students will learn to correctly apply, diagram,
and troubleshoot instruments. They will apply this knowledge in lab by designing experiments and
learning to use instruments to characterize their product. After each experiment is completed, written
reports will be submitted for TA and instructor review.

Course Goals: Students will learn to design an experiment, select appropriate instrumentation,
research and apply laboratory procedures, carry out experiments, troubleshoot instruments, analyze
data, and write it all up in a scientific report.

Student Learning Outcomes:

• Students will be able to diagram spectroscopic and chromatographic instrumentation and select
the appropriate instrument for a particular problem.
• Students will be able to research and apply instrumental methods for characterizing materials.
Then perform the experiment and interpret the results.
• Students will compose a scientific report in the ACS style to justify and document experiments,
interpret results, and draw conclusions.

Available Instrumentation: Flame AA, ICP-MS, FT-IR, UV-VIS, GC, GC-MS, HPLC, NMR.

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Course Policies:
Continued attendance to class indicates each student agrees to the policies set forth in this syllabus.
Behavior and Collaboration- Students are expected to conduct themselves professionally at all times.
Disrespect of the classroom learning environment, instructors, and fellow students is not tolerated!
Collaboration and working in small groups is a key component of classroom and lab time.
Attendance, Tardiness, and Late Work- Students are expected to attend class and not compromise
the experience of other students. Makeup labs are not available for this course except for school-
related travel. Work is not accepted late. This is to keep us all moving though the material efficiently.
Instructor-Initiated Withdrawals- Any time up to and including the final date to drop a course with a
“W,” the professor has the right to withdraw a student that “...has not participated substantially in the
course.”
Honor code and Academic integrity- Students are expected to conduct themselves in accordance with
the UAF Honor code. The Chemistry Department policy states: Any student caught cheating will be
assigned a course grade of F. The students academic advisor will be notified of this failing grade and
the student will not be allowed to drop the course.
Disability Services- I will work with the Office of Disabilities Services (208 Whitaker Bldg, 474-5655) to
provide reasonable accommodation to students with disabilities. It is the student’s responsibility to
make an appointment with me to discuss appropriate accommodations. A letter from disabilities
services must be provided.

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CHEM 314 Evaluation

There are 1000 total points available in this class. Grades are assigned on the typical scale 1000-
900 A, 899-800 B, 799-700 C, etc.
Assignment Points
Literature review & presentation 100
Reports (7@100 each) 550
Lab notebook 50
Exams (2@100 each) 200
Final presentation 100
Total points graded 1000
Literature review & Presentation (100 pts)- You will give a presentation based on a paper you are
provided by the instructor. The presentation is supposed to identify the major components in that
paper (see full report format below).
Final Presentation (100 pts)- You will give a final presentation at the end of the semester, based on
one of your favorite experiments you have done in this semester. You will present in a similar fashion
to your first presentation, but based on your own work!
Exams (200 pts)- Midterm and Final Exams will count for 100 points each.
Lab Notebook (50 pts, individual)- Maintaining a tidy, individual lab notebook is essential in science
and is required for this course. It is your permanent record of your progress through this course that
should be readily interpretable by anyone who picks it up- even me. Before coming to lab for
experimentation, each student must have a procedure, and data tables prepared. Lab notebooks will
be checked periodically throughout the semester without advanced notice. Students must use a
dedicated, organized bound notebook with sections for each experiment. Instrument data
may be printed out and taped into the notebook. Loose papers or disorganized work is not
acceptable.

Experiments (550 pts; individual & group)- Experiment requirements vary throughout the
semester
Experiment Report Points
Experiment 1: Standard addition Full report- individual 100 pts
Experiment 2: Flame AA Annotated Figs and Results-individual 50 pts
Experiment 3: FT/IR Full report- individual 100 pts
Experiment 4: ICP-MS Annotated Figs and Results-individual 50 pts
Experiment 5: HPLC Full report- individual 100 pts
Experiment 6: GC or GC/MS Annotated Figs and Results-individual 50 pts
Experiment 7: NMR Full report- individual 100 pts
Total 550 pts

Full reports include: Procedure, Annotated Figures, and Report

Procedure- Prior to performing an experiment, groups will write a detailed description of their plan in
their lab notebook. It will detail how you intend to prepare and analyze your samples by including: a
purpose, step by step instructions to a level of detail that another student could easily replicate your
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work, a list of all reagents and materials needed, a description of what you expect to find and/or how
you will analyze the data, and include references to any outside sources consulted.
1. Title- Exciting or boring, be descriptive
2. Purpose- what are you trying to analyze and why?
3. Background-
a. Give a brief overview of the procedure and what you are analyzing for. What are the likely
compounds you are looking for? Make a figure of their structures.
b. What are the anticipated results? Include literature spectra, chromatograms, etc have you
found as examples. If applicable, make a table of physical properties (lamda max, molar
absorptivity, etc) that will be useful or help you distinguish between the possible
compounds.
c. Suggest alternate procedures that might work if this doesn’t.
4. Safety- Print MSDS for all compounds used in your procedure.
a. List hazards associated with your procedure- either chemical or procedural
b. What engineering controls and PPE will be used to mitigate hazards?
c. What are the most likely things to go wrong? How will you react if they happen?
5. Sample prep- How will you prepare your sample? Go from the product to getting your sample
into the instrument.
6. Instrument parameters-What conditions/ parameters are you going to use to run the instrument?
7. Data tables- What information will you record during the course of the experiment? Be sure you
SPEND SOME TIME thinking though your experiment! And leave space in case things change
during the experiment.
8. Data Analysis- Plan for statistical analysis of data, estimation of error, propagation of error.
9. What do you need? If you want what you need to be available, be sure to ask for it ahead of
time! List what materials you will need: solvents, standards, glassware, etc. State the expected
results are (retention time, etc).
10. References- Where’d you get your information and inspiration?
11. Appendices- Attach MSDS and key references or methods if applicable.
Figure or Table title?
Annotated Figures- Print out copies of your figures and tables on
individual pages. In addition to figures and tables of data you have
Observations Interpretations
generated, think of other materials you will need to include in your
report. Examples: summary tables, structures of possible and identified
molecules, spectra or other reference materials from literature.

On the print-outs, add a title and descriptive caption to figures and

tables. Record observations (to go into the results section of your
report), interpretations (to go into the discussion), and a sentence
conclusion. These will be checked off in class and provide a starting
Conclusion
point for group discussion and very helpful in writing the lab report.

Full Report Format- All reports will be written in a consistent journal format in a professional
tone!
1. Descriptive title- “Report 3” won’t cut it.
2. Abstract- (250 words max)

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3. Introduction- (2-3 paragraphs) Give some background on your question. Feel free to recycle
from the project definition, but make it concise and coherent.
4. Instrument Diagram- (1-3 paragraphs) Diagram the instruments used and explain how the
measurements are made.
5. Materials and Methods- (1-3 paragraphs) This is a paired down version your procedure. Include
sample preparation procedures and instrument parameters and conditions.
6. Results- (1-3 paragraphs) Follows directly from annotated figures and include at least a
paragraph for each figure and table. Reference figures in the text.
7. Discussion- (1-3 manageable paragraphs) Follows directly from annotated figures.
8. Conclusions- (2-5 sentences) saying what you found and what that means.
9. Acknowledgments: Research projects are collaborative and substantial contributions have been
made by mentors, peers, postdocs, faculty, etc. Any person that significantly contributed to your
work and their specific contribution should be mentioned.
10. References- If you used anything other than your brains (websites, text books, another group’s
procedure, instrument instructions), cite these resources appropriately!
11. Figures and tables- Each figure and table is to be numbered and on it’s own page with a figure
title and caption. All measurements should have an error estimate and graphs should have error
bars.

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Additional Guidelines for Written Assignments
• Abbreviations are often necessary and should be introduced clearly when used the first time.
• Element names (Iron) are spelled out only if they are the first word in a sentence and when they
are part of a name (iron oxides). Otherwise, the symbol is used (Fe).
• Succinct description and clear reference in text to all figures and tables in the text.
• Do not duplicate data between the text and figures or tables
• Use SI units or the standard units in the field for all laboratory data. Appropriate formatting is used
to indicate units. For example, mg kg-1 is correct, while mg/kg or ppm is not. Pay attention to
these details in the literature you are reviewing.
• Use bold font to indicate references to figures, tables, and equations in the text. This helps during
the proofreading process. Reference to Figure 1 in the middle of a sentence and at the end of the
sentence (Fig. 1). The word is always spelled out in entirety (Table 1).
• All figures and tables must have a descriptive caption clearly explaining the figure. Explain all
abbreviations and symbols used in the figure and provide sufficient experimental and statistical
detail.
• Provide sufficient experimental detail to allow reproducibility by a person with a similar skill level
as yourself.
• Provide details on the origin of chemicals you use. Example: sodium chloride (JT Baker, lot 324)
• If instrumentation is used, report the make and model number of the instruments and location of
manufacture. Example: 7500 series High Performance Liquid Chromatography (Agilent; Ames,
IA)
• If non-standard software is used, report the version of the software and reference the developer.
Example: Sixpack (version 1.57; Webb, 2006).
• Pay attention to significant figures. All measurements should have an uncertainty associated with
them. Error only has one significant figure, and this often limits the number of significant figures in
a measurement. Example: 3.45 + 0.3 should be reported as 3.4+0.3. If you have questions about
this, see your instructor.
• Pay attention to consistent formatting for both in-text citations and in the reference list. Be sure to
manually double check that the reference list and text (including figure and tables) have the exact
same references.

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REVIEW SAFETY FEATURES IN THE LAB (REIC 245)

• Cubbies for bags and coats

• Location of personal protective equipment (PPE)
• Safety shower/eyewashes
• Fume hoods
• Exits out of room and out of building
• Waste bottles and broken glass container(s)
• Chemical/safety literature
o hazard.com/msds is a good start

LABORATORY SAFETY RULES

• USE COMMON SENSE AT ALL TIMES!!!

• No horseplay in lab
• No unauthorized experimentation
• Wear safety glasses/goggles—know when each is required
• Use of correct gloves (when appropriate)
• Knowledge of location and use of MSDS’s
• NO food, drink, or gum in lab
• Do not leave fires unattended
• Label all containers with contents, your name, your class, and date/semester
• Report any accident or spill or unsafe condition
• Observe proper storage of chemicals
• Properly disposing of laboratory waste
• Use caution around heat sources, cold sources, flame, electrical equipment
• Properly disposing of glass
• Safely handling chemicals
• No open-toed shoes, no shorts in lab
Recommend no skirts, hair tied back, no loose sleeves/clothing

OTHER IMPORTANT RULES

• This is shared lab space
o Clean up after yourself
o Follow storage rules
o “Default Dirty” Assume benches/glassware is not as clean as you would like.
• Wash your hands frequently
• LABEL EVERYTHING!!!!!
• Use caution if you must transport samples to other rooms
• Inform your instructor and/or TA if you use the last of something or break something
• You are responsible for your own safety, and the safety of everyone else in this room
GOOD SAFETY = GOOD LAB TECHNIQUE = GOOD RESULTS

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Tentative Schedule (version 1-14-2018)

Date Monday Lecture Monday Lab Wednesday Lab
1-15 1 Introduction
Lab safety
1-22 2 Introduction to Measurements (Ch 1) Noise and Error (Ch 5) Planning safe experiments
Student presentation Standard Addition
1-29 3 Interactions b/w light and matter (Ch 6) Standard Addition Standard Addition
2-5 4 Components of instruments (Ch 7) Flame AA Flame AA
Atomic spectroscopy (Ch 8-11)
2-12 5 Molecular spectroscopy (Ch 13-15) Flame AA FTIR
2-19 6 Vibrational Spectroscopy (Ch 16-18) FTIR FTIR
2-26 7 Mass spectrometry (Ch 20) ICP-MS ICP-MS
3-5 8 Midterm Exam ICP-MS HPLC
3-12 9 Spring Break
3-19 10 Chromatography & HPLC (Ch 26, 28) HPLC HPLC
3-26 11 GC-MS (Ch 27) GC/GC-MS GC/GC-MS
4-2 12 NMR (Ch 19) GC/GC-MS GC/GC-MS
4-9 13 Electron Microscopy (Ch 21-ish) NMR NMR
4-16 14 X-ray techniques (Ch 12) NMR Tour to EPA NCORE site
4-23 15 Review of Instruments Final presentation Exam Review
5-4 16 May 4, 1-3 pm Final Exam