Instrumental Analysis Laboratory – Chemistry 341

Spring 2020
See Lecture Syllabus for additional informatino

Instructor: David Green

Office: RAC 128 Ext. 4355
E-Mail: [email protected] (attachments accepted)
URL: http://seaver-faculty.pepperdine.edu/dgreen

Location: KSC 430

Time: Thursday, 2-6 p.m
Text: Green, Laboratory Manual to Accompany Quantitative Chemistry and Instrumental Analysis
Other: Scientific calculator, laboratory notebook, safety goggles or glasses, lab coat

PHILOSOPHY The purpose of laboratory is to provide an opportunity to perform specific sample preparations
and chemical analyses of a variety of substances and mixtures using instrumental methods and
to provide reinforcement for and examples of the chemical and analytical principles discussed
in the lecture.

The overall goal of this course is to provide participants with a sufficient understanding of the
principles, laws, and theories of analytical chemistry and instrumentation for chemical analysis
to enable them to successfully analyze real samples using selected classical and instrumental
methods. The student should gain the competence to follow a standard procedure, operate the
equipment in a safe manner, collect suitable data, evaluate the reliability of the data collected,
and report the results in an appropriate form as would be required of any competent laboratory
technician. Analysis of small samples is emphasized using methods such as spectroscopy,
spectrometry, and chromatography. A working knowledge of information obtained from prior
courses (including general chemistry, quantitative chemistry, physics, and mathematics) is
essential for any level of success in this course.

STUDENT The specific Student Learning Outcomes aligned to the Chemistry Program Learning Outcomes
LEARNING is that at the successful completion of this course participants should be able to successfully
utilize analytical chemical instrumentation properly including: preparation of high accuracy
OUTCOMES standards, set the operating parameters of different instruments, and perform calibration and
analysis.

GOALS While the major foci are on the principles and capabilities of selected analytical methods and
techniques, the specific goals are that every participant will…
 learn to maintain and use precision electronic analytical equipment properly and
appropriately for the analysis at hand.
 realize the existence of a variety of analytical methods, each with its own particular
capabilities and limitations.
 develop a basic understanding of the electronic, optical, mathematical, and mechanical
subsystems in each instrument introduced or used in the laboratory.
 understand that the selection of one method as being superior to another in the solution of
a particular analytical problem, is based on such factors as sensitivity, time required,
selectivity, the economics involved, etc. Also, understand that the success of any of the
analytical methods used depends upon a working knowledge and control of the chemical
reactions, operating parameters, accuracy and precision required, and time available.
 develop or refine the chemical intuition necessary to know where physical steps in an
analysis may be modified such that accuracy and/or precision in the the analysis is not
compromised.
  recognize and appreciate the value of the analytical equipment used, as well as their
limitations, in the solution of selected problems faced by the technician.
 be instilled with quantitative analytical habits and skills that, in spite of possibly never
performing a specific chemical analysis from this course again, will be valuable regardless
of the scientific field the participant may end up in.
The laboratory course is nearly entirely a course in applied chemical analysis. Because of this
characteristic, each participant must come to the laboratory with the foundational skills expected
to have been mastered in previous chemistry courses.
Upon successful completion of this course every course participant should be able to:

 demonstrate the meticulous quantitative analytical skills necessary to perform accurate

chemical analysis as well as independently operate each instrument introduced in the
laboratory.
 properly report analytical results with appropriate statistical analysis and confidence.
 carry out calibration, preparation of a sample for analysis, safe handling of the sample
during the analysis, and proper disposal of the sample after completion of the analysis.
 use techniques for recording and evaluating analytical data.
 solve a variety of numerical problems dealing with the analysis of samples using computers
and a variety of different software packages.
 write in scientific format reports of the theory, experimental method, and results of an
analysis.

REQUIRED Investigation monographs will be distributed on a weekly basis, as in Quantitative Chemistry

MATERIALS (CHEM 340).
A permanently bound (not spiral or loose-leaf) laboratory notebook; quadruled preferred – all
procedures, data, results, calculations, and solutions to problems will be recorded in the
laboratory notebook. A lab notebook with yellow removable pages is neither required nor
preferred. If there are sufficient pages left in your Chem 340 laboratory notebook, you can simply
append experiments, investigations, and analyses to the existing notebook.
Scientific calculator
Approved laboratory safety goggles (available in bookstore or through the SAACS)
Lab coat

ATTENDANCE You are required to attend prelab discussion and laboratory at the assigned time. The lab is
scheduled for 4 hours. You will undoubtedly, at times, take longer than 4 hours. You will have
some opportunity to work on your laboratory assignments at other times as well if you are not
finished by 6 p.m (but see below, AFTER HOURS WORK). This offer of extra time does not extend
to those who leave with the intention to come back later to finish – it is only offered to those who
actually work during the assign 4 hours and cannot complete the lab on time. I will give time-
saving hints when they are available and appropriate (and don't adversely affect the analysis or
experiment). If you miss more than 3 labs, a lab grade of 'F' will be assigned. Please don't
miss lab. The laboratory grade is independent of the course grade.

You may not miss lab and make it up later. There will be lecture, discussion, and problem
solving sessions during the beginning of each lab. If you miss any part of 3 lab periods, you
will be assigned a grade of 'F' for the lab and the course.

LABORATORY A laboratory notebook must be kept for every analysis performed. The style of the book and the
NOTEBOOK format of the entries will be described in lab and is also outlined in the laboratory textbook. The
laboratory notebook will be rigorously graded.

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LABORATORY For analyses and experiments which require a formal report, a written report of the results of
REPORTS your laboratory work is due at the beginning of the second laboratory period following the
completion of the work unless otherwise informed. Reports turned in within 1 week of the date
the analysis was assigned will receive a 10% bonus. It is at the instructor’s discretion to cancel
the 10% bonus policy. Late work will be assessed a penalty of no less than 10% per day starting
the first day after the report is due. The format of the report will be described in lab and is
outlined in the laboratory textbook. The laboratory report must be typed and must be
scientifically and grammatically correct. Spelling and sentence structure counts.

You may turn in laboratory reports electronically as a email attachment, should you desire.
Laboratory reports submitted in this manner must be submitted in Microsoft™ Word® format and
the entire report must be self-contained in one file. The instructor will not open more than one
file per lab report.

Handwritten chemical formulae, chemical structures, and mathematical equations will be

accepted. However, your instructor recommends the following software for Microsoft Windows
users:

Chemical Structure Drawing:

Accelrys Draw (Dassault Systemes), ACD/ChemSketch (Advanced Chemistry
Development Laboratories), or KnowItAll (KnowItAll Informatics System, BioRad).
Knowing the rules of writing structures, you can convert
C7H6O3

into

O
C OH

OH

quickly with a very professional appearance.

The best thing about these three chemical drawing packages is that they are free. Links to
ISIS/Draw, ACD/ChemSketch, and KnowItAll are available at the Cool Links area of the
course website.

Your instructor does not know of any equivalent Mac programs which are free.

Chemical Formula Formatting:

Christopher King’s Chemistry Formatter add-in for MS Word and MS Excel is an excellent
macro add-in if you use the Microsoft Office suite. There are no versions of the add-in for
other word processor or spreadsheet programs. The intelligent chemistry formatter, when
properly installed, eliminates the need to select ‘format|font|subscript’ for the formula
stoichiometry in a chemical formula and usually gets the charge placement correct on ions.
You can also get excellent looking chemical equations quickly. For example, consider the
chemical equation

C6H12O6 + 6 O2 --> 6 CO2 + 6 H2O

Simply highlight the entire equation, apply the chemistry formatter add-in with one mouse
click, and the equation becomes

C6H12O6 + 6 O2  6 CO2 + 6 H2O

Additionally, showing a number in proper exponential notation is easy. Perhaps, because

of textual context, a result such as 0.00115 g needs to be presented in exponential notation.
Since typing the value in proper exponential notation syntax is time consuming, there is a
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 temptation to simply type 1.115E-3 since, afterall, that’s the way the value is displayed on
the calculator. However, with the Chemistry Formatter, the unconventional (and incorrect)
presentation shown previously is easy to correct. By highlighting the value and applying the
formatter, 1.115E-3 g in one mouse click becomes 1.115  10-3 g.

King’s Chemistry Formatter is free to download and use. A link to the Chemistry Formatter
can be found in the Cool Links area of the course website.

Equation Writing and Editing:

The Microsoft Office suite comes packaged with a good equation editor (aptly named
Equation Editor but it is not activated during a normal installation of the suite. Simply run
the install CD, customize the installation, and add the Equation Editor.

A better equation editor is MathType (Design Science, Inc.) for Windows and Mac. It is
actually the full version of MS Equation Editor and is extremely powerful.

Using the MathType add-in, you can easily make

k = A exp[-Ea/RT]

or the handwritten

look like a typeset equation:

k  A e
  
Ea
RT

Equation Editor is included with Microsoft Office Suite if you have the installation CD.
MathType can be purchased with an academic discount directly from Design Science, Inc.

LABORATORY There are no laboratory exams scheduled although information learned in the lab will be found
EXAMS on lecture exams. You must treat laboratory as seriously as the lecture. It is at the discretion of
the instructor to give unannounced pre-lab quizzes if situations warrant.

AFTER HOURS There will be some opportunity to work outside the normal confines of the scheduled lab time.
WORK This privilege is to provide you sufficient time to perform excellent quality work under a minimum
of time pressure. This does NOT mean that you can work on an analysis at your leisure. The
opportunity to work on laboratory analyses at unscheduled times is a privilege. This privilege
can be revoked individually or for the entire class. This level of freedom in the laboratory will
be revoked immediately for anyone who works without protective eyewear. This is a
"zero-tolerance" policy and is not negotiable. Final word... it is highly recommended that you
work with someone in case of emergency.
You may contact the professor by e-mail at any time and by phone in emergencies (be very
loose with your definition of an emergency).

COMPUTERS There is access to computers in the KSC laboratories. Computers and printers in the
laboratories are not for printing notes, handouts, reports, etc. for any class. Violation of this
policy will result a complete prohibition on using the computers.
Under no circumstances install software on any of these computers without consent of the
instructor. If you use the computers to access email, don’t forget to log off.

GRADING Your overall lab score will be calculated approximately evenly between all laboratory reports
and lab notebook entries. Laboratory attendance, efficiency and timeliness in completing
analyses also contribute significantly to your lab grade. Your lab grade will be based on the
same fixed scale as lecture.

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 Approximately 4% of the laboratory grade is based on lab cleanliness and safety. These are not
“earned” points: points will be deducted at the end of the semester for violations. The following
list will give a representative guideline of how the grade is assessed.
 Reagent bottles must be kept closed except during transfers.
 Balance areas must be kept clean at all times and spills on the balance pan and inside of
the windscreen must be remediated immediately.
 At the completion of an investigation or analysis, glassware will be cleaned and placed back
on appropriate shelves or in cabinets and drawers.
 Spills on hood decks and benchtops must be cleaned up before leaving lab.
 Hotplates and stirplates should be stored in the cabinet as neatly as possible.
Much of lab cleanliness and safety should be self-policed. Those “caught” cleaning up after
others will be rewarded. This is a shared laboratory, so courtesy is expected for the next users.

A Word On Extracurricular activities such as sororities, fraternities, athletics, drama and other artistic
Sorority, Fraternity, endeavors, etc. are important parts of your total education at Pepperdine. However, these
activities require a very significant time commitment. It is your responsibility to keep up in
Sports, SongFest, class while involved in extracurricular activities.
etc.

PLAGIARISM Fortunately, in all likelihood, no one in this class will be subject this paragraph. As a scientist
AND you have certain ethical responsibilities with respect to data collection, recording, and analysis.
Data that has been collected in the laboratory can never be changed to suit your expected
CHEATING outcomes. Plagiarism and cheating are professionally and ethically wrong. There seems to be
a strong temptation for the students in the scientific community to plagiarize material so as to
improve their course grades. There exists a fundamental difference between working
cooperatively (e.g. working together with friends or in a study group on homework problems
which this instructor not only approves of but also recommends) and simply copying someone
else's work. Plagiarizing the work of others is an offense of considerable magnitude. For
assignments in which collaboration with your peers and other faculty is considered acceptable,
you are encouraged – perhaps even expected – to do so provided you include a list of
collaborators when submitting your assignments.
You are expected to conduct yourselves per the terms of the Seaver College Code of Academic
Ethics. Any cheating (including plagiarism) will be punished as severely as allowed under
University guidelines. Please see the laboratory instructor or the Seaver College Student
Handbook for any questions about this policy. Students suspected of plagiarism will be assigned
a grade of zero for that work and may be referred to the University Academic Ethics Committee.
It's not worth it – trust me on this!

SAFETY IN Safety Goggles

THE Safety goggles or safety glasses (meeting ANSI Z87.1 standards or greater) must be worn
in the laboratory at all times when any chemical procedures are underway. Safety eyewear
LABORATORY may be purchased at the bookstore or through SAACS. Any student who is not wearing
safety eyewear will be asked to leave the laboratory, will not be allowed to make up the
laboratory, and will receive a grade of zero for that investigation. The use of safety eyewear
in the laboratory is a zero-tolerance policy and is governed by university regulations and
local, state, and federal laws.
Appropriate Dress
Students must dress appropriately for laboratory work. This means wearing a lab coat at all
times. Open-toed shoes and sandals are unacceptable in lab (this includes clogs and crocs).
You will be asked to leave and change clothes or shoes, if needed. Make sure you
come prepared, especially if you live off campus. Appropriate laboratory attire is a zero-
tolerance policy and is governed by university regulations and local, state, and federal laws.
Hair
If your hair is longer than shoulder length prudent laboratory practices suggest it should tied
behind your head in order to avoid accidental contact with open flames or chemicals that
might be on the lab bench.
Electronic Equipment

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 Audiovisual or electronic equipment (except for calculators and computers for data
collection and analysis) are not allowed in the laboratory without permission. Permission is
given freely, but restrictions apply.
Food and Beverages
You may not eat, drink, or bring food in the laboratory.

SAVING GRADED It is your responsibility to save all graded materials (exams, homework, etc.) for this class. As
MATERIALS per university policies, all grade disputes must be settled by the midpoint of the next non-
summer semester which immediately follows this course.

CELL PHONES If you bring a cellular phone to lab, please TURN IT OFF. It is very impolite and unsafe to have
incoming calls during lab. Answering calls during lab is not allowed and will adversely affect the
lab grade.

WITHDRAW Despite the independent nature and course number of the chemistry lecture and lab, except
POLICY under extreme and unusual circumstances, you may not withdraw from lab and remain in
lecture, or vice versa.

INTELLECTUAL Course materials prepared by the instructor, together with the content of all lectures and review
PROPERTY sessions presented by the instructor, are the property of the instructor. Video and audio
recording of lectures and review sessions without the consent of the instructor is prohibited.
STATEMENT Unless explicit permission is obtained from the instructor, recordings of lectures and review
sessions may not be modified and must not be transferred or transmitted to any other person.
Electronic devices other than calculators (e.g., laptops, cell phones, PDAs, calculators, and
recording devices) are not to be used during lectures or exams without prior permission of the
instructor.

COUNSELING Students who feel that they may suffer from “test anxiety” or other academic obstacles despite
exercising reasonable study and social habits may benefit by speaking to one of the staff in the
CENTER and Counseling Center.
DISABILITY
SERVICES Any student with a documented disability (physical, learning, or psychological) needing
academic accommodations should contact the Disability Services Office (TCC264, x6500) as
early in the semester as possible. All discussions will remain confidential. Visit
www.pepperdine.edu/disabilityservices/ for additional information.

COURSE At the end of every course, each student has the opportunity to evaluate the course and the
EVALUATIONS professor. This input is valuable for every faculty member so that they can discern both what is
being well-presented as well as what may need to be modified to improve the course. Course
evaluations are completed on-line near the end of the semester.

Your professor in this class appreciates your critique, both good and bad, and believes that you
do not need to be motivated to complete your evaluation by receiving “extra credit” points or
other intangible rewards.

Disclosure Statement Required by the State of California

Warning: Natural Science's laboratories contain and certain class experiments or procedures which will expose
you to chemicals known to the state of California to cause cancer, birth defects, and other reproductive harm at
levels which require a warning. For more information, contact your instructor or the Office of Regulatory Affairs
at extension 4702.

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 Instrumental Analysis Laboratory – Chemistry 341
Spring 2020
Weekly Schedule
This schedule is subject to change
Week Date Activity
1 Jan 16 Readings:
Chapter 6,13,14 (SHN)
Activity:
Introduction to Emission and Absorption Spectroscopy: Line spectra, continuous
spectra, spectroscopes, spectrophotometers
2 Jan 23 Readings:
Chapter 6,13,14 (SHN)
Analysis:
Electronic Spectroscopy I
Determination of the Formula of a Complex by the Method of Continuous Variations
Additional Investigation:
Determination of Formula and Kf of the Cu-en complex: Does Job’s method work?
3 Jan 30 Readings:
Chapter 6,13,14 (SHN)
Analysis:
Electronic Spectroscopy II
Spectrophotometric Analysis of a Complex Mixture
Additional Investigation:
Simultaneous Determination of Aspirin, Acetaminophen, & Caffeine: Is it Feasible?
4 Feb 6 Readings: TBA
A Separation Science Interlude
Analysis: Determination of Simple Sugars by HPLC-ELSD After Desalting by SPE
5 Feb 13 Readings: TBA
Analysis: TBA
6 Feb 20 Readings:
Chapter 15 (SHN)
Analysis:
Fluorescence Spectroscopy
Determination of the CMC of Sodium Dodecyl Sulfate Using a Fluorescent Probe
Additional Investigation:
Comparison of Two Instruments for Spectra, Detection limit, Signal-to-Noise, and
Results of the CMC determination
7 Feb 27 Readings: TBA
A Second Separation Science Interlude
Analysis: Gas Chromatography-Mass Spectrometry
8 Mar 5 SPRING BREAK
9 Mar 12 Readings:
Chapter 7-9 (SHN)
Analysis:
Flame Atomic Absorption Spectroscopy and Introduction to Automation
Determination of Ni by standard additions
10 Mar 19 Analysis:
Graphite Furnace Atomic Spectroscopy
Determination of Cu by direct calibration

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 11 Mar 26 Readings: TBA
Analysis: TBA
12 Apr 2 Readings:
Chapter 16,17 (SHN)
Analysis:
Vibrational Spectroscopy
Fourier Transform Infrared Spectroscopy – FT-IR
13 Apr 9 Readings:
Chapter 19 (SHN)
Analysis:
Nuclear Magnetic Resonance Spectrometry I: Proton NMR
14 Apr 16 Readings:
Chapter 19 (SHN)
Analysis:
Nuclear Magnetic Resonance Spectrometry II: Carbon NMR
15 Apr 23 Readings: TBA
Analysis: TBA
16 Apr 27 Finals Week

You are allowed to one (1) drawer for personal storage. You may store your books, lab coat, samples for analysis, or whatever,
but you may have only one (1) drawer. There will also be a shared cabinet for desiccators and other larger equipment for your
use.
You must practice good housekeeping in the laboratory since there will be many users in the laboratory besides yourselves. The
lab instructor and/or TA and/or Stockroom Staff will "clean up" unlabeled, unattended, or otherwise messy areas (you have been
warned). Proper labeling and storage techniques will be observed.
Replacement "unknowns" will cost 10% of the report score for that analysis unless otherwise notified.

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Syllabus 9