Instrumental Analysis II:
Chemistry 4243
Text: Principles
of Instrumental Analysis by Skoog, Holler, and Nieman, fifth edition
Lecture
M.
Bushey, Spring 2001
Dates
Topic
Chapter
Electrochemical
Methods
Jan.
9, T
Introduction to Course and Electrochemistry
22
lab lecture
Jan.
16
MB out of town, no class
Jan.
23
Voltammetry
25
Jan.
30
Voltammetry
Feb.
6
Potentiometry
23
Feb.
20
Introduction to Chromatography
26
Mar.
6
Electrochemistry Exam
Mar.
13
Spring Break, no class
Mar.
20
HPLC, instrumentation
28
Mar.
27
HPLC, methods
Apr.
3
HPLC, cont
Apr.
17
Mass Spectrometry, methods and analysis
Apr.
24
Mass Spectrometry, new methods
May
1
last day. Review, evaluations
May
8, Tuesday, 2:00 PM
Final Exam – Separations
This course explores how chemists use instruments to obtain chemical
information. We will examine how these instruments work, how they are best used
and what type of performance we can expect. This course focuses on
electrochemical and separation methods, including mass spectrometry.
This is a 2 credit course, with 1 hour for lecture for a total of 14
lectures and the remainder assigned to lab time. There are 5 experiments, 2 of
which are designed to be performed in course of 3 afternoons (provided students
are properly prepared). The remaining two can be completed in one long
afternoon. While many of these experiments do require a substantial amount of
work in order to be completed, the laboratory portion of this course is designed
around a team concept. Part of the purpose of the team approach is to divide the
work load so that experiments which are slightly more interesting than the usual
can be performed.
Since it is necessary to rotate groups through the various experiments,
you will find that sometimes you perform an experiment prior to the class
discussion, and vice verse. Sometimes a lecture topic will not be explored in
the lab and a lab topic will not be discussed in the lecture. You should expect
this to be the case as it is through the combination of lecture and lab that you
will gain in experience and understanding of instrumental analysis.
Although attendance at course lectures is not explicitly required, I
generally expect you to attend the lectures. I realize that situations may arise
which cause you to miss an occasional lecture. I do not expect this to occur on
a regular basis. If you miss a lecture, it is your responsibility to obtain
class notes, or to make arrangements to complete any missed course requirement.
Also, although I would prefer that everyone arrive at class on time, I prefer
that you come to class late rather than not at all.
Laboratory Schedule
Team I
Team II
A
JC Bunch
Erika Garcia
B
Mary
Falgout
Alexis Thompson
C
Amber Rakowitz
Linnzi Wright
High
Performance Liquid Chromatography, Capillary Electrophoresis,
Cyclic
Voltammetry, GC-MS, Anodic Stripping Voltammetry
Date
I
II
Due:
Jan.
9
no lab----------lab lecture------
Jan.
16
MB OOT no lab
Jan.
23
CV
GC-MS
2/2 (I)
Jan.
30
ASV
GC-MS
2/9 (II)
Feb.
6
ASV
--
2/16 (I)
Feb.
20
GC/MS
ASV
3/2(I)
Feb.
27
--
ASV
3/3 (II)
Mar.
6
no lab Electrochemistry exam
Mar.
13
no lab------------Spring Break---------------------------------
Mar.
20
HPLC
CE
Mar.
27
HPLC
CE
Apr.
3
HPLC
CE
4/12 (Thursday)
Apr.
10
CE
HPLC
Apr.
17
CE
HPLC
Apr.
24
CE
HPLC
5/1 at5PM(Tues)
Due
Dates for Analytical Chemistry (Journal of Chromatography) article summaries:
Issue
Date
Due Date
1/1
1/16
1/15
1/23
Five may be turned in for 10 points of extra credit each.
2/1
2/13
I strongly recommend that you take advantage of this
2/15
2/20
opportunity of extra credit. It can dramatically change
3/1
3/13
your final grade.
3/15
3/27
4/1
4/17
Grading
five experiments @ 100 pts each
500
(30% yellow sheets, 70% group
report)
electrochemistry exam
50
final exam for lecture section (no echem)
100
final exam for lab section
50
Analytical Chemistry summaries
(50)
(optional, 10 pts. each)
total
700 (750)
Assignments:
duties
A
B
C
HPLC
solutions
technical
manager
GC-MS
solutions
manager
technical
CE
manager
technical
solutions
ASV
manager
solutions
technical
CV
technical
manager
solutions
Grading
Late
reports will be penalized 5% per day late. Due dates for late reports with no
penalty must be negotiated with the instructor prior to the original due date.
All notebook information is due at the same time as the formal reports. Report
formats are discussed below. Notebooks will also form a substantial portion of
the lab grade. Notebook formats are also listed below.
While
not every analysis is perfect, the following are a few errors which can
substantially lower laboratory grades: failure to properly specify the time and
date of critical records; loss or corruption of electronic data or irreplaceable
hard copy data; statistically bad results; poor graphical presentation of data;
“blunders”; use of scrap paper in place of notebooks, inappropriate use of
balances, weighing paper, glassware, etc., failure to clean up the work area or
glassware at the conclusion of the experiment.
Analytical
Chemistry extra credit article reports: Analytical Chemistry which is published on the 1st and 15th of each
month is the journal for this field.
The journal is available at the library and through the ACS web page. The
journal is divided into two sections, “A” page articles and research
articles. You may to turn in 5 summaries, each from a different issue date, 1 to
2 pages in length, for 10 points of extra credit each. Note: late reports will
not be accepted unless special circumstances have been discussed in advance. The articles you choose must be full length papers, not
correspondence or technical notes. You should make efforts to choose articles
from a wide range of topics. Each report you choose to turn in must be from a
different journal issue. The library also has a subscription to The
Journal of Chromatography. This is another extremely important journal in
the field of analytical chemistry. You have the option to substitute up to two
reports on an article in this journal in place of Analytical Chemistry articles. A full literature citation is
required on all submitted article summaries. If your article is from The
Journal of Chromatography, please submit a copy of the original article with
your report. Do not submit a copy if your article is from Analytical
Chemistry. In addition to the formal reports, you are encouraged to browse
through these journals, and at the very least, read several of the abstracts.
Lab Organization
This laboratory is designed around a team concept. You will be working in
teams of three. Each of you will have a specific and assigned role to play for
each of these experiments. The reasons for organizing the class this way are
many. One of the more important reasons is that this type of organization mimics
what is often found in industry. While it may be several years, if ever, before
you enter chemical industry, working in a team setting forces you to work and
interact with other people, a valuable skill. Although during much of your time
here at Trinity you have worked individually on your chemistry, rarely do
chemists work alone.
The labs you will be performing this semester can be completed in one or
two three hour afternoons, but only if
you come to lab prepared and ready to begin work. If you come to lab not knowing
how to manipulate the software of a particular piece of equipment, or without
having mixed crucial solutions, or without knowing how to mix particular
solutions, you will not finish these
labs in time. It is vital for the success of these labs that you are prepared on
Tuesday afternoon. By dividing the work for these labs into three components,
the overall workload of this class is lessened. Some of you will be required to
work on aspects of these labs prior to Tuesday, some will be required to work on
aspects after Tuesday, every group member is
required to be in lab on days your group is actually performing an experiment.
Typically you will have access to equipment for two weeks in order to complete
the experiments. Lab reports are typically due one and one half weeks
after completion at the experiment by noon on Friday.
The three roles for each team are: Reporter (Manager), System Software
and Operation, and Solution Preparation. The general duties of these roles are
described below. Reporter/Manager. The Manager is in charge and responsible for
the design, organization, and implementation of the experiment. The Manager is
responsible for the outcome and reporting of the experiment and for inter- and
intra-team communications and division of labor within the team. The Manager
does pre-experiment library research and
prepares the final report on an experiment, based upon the individual and
intra-team reports. All other team members are answerable to the Manager. The
Manager must submit an evaluation of the performance of each group member with
each experimental report. The Manager may delegate authority within the team but
cannot delegate responsibility.
Solution Preparation. The
person is responsible for the acquisition, preparation, blending, and delivery
of all reagents, standards, and samples based upon the Manager’s instructions
and the experimental needs. Most of this work must
be done before the scheduled laboratory period if the team hopes to finish
an experiment in a single afternoon.
System
Software and Operation. The person is responsible for the preparation and
operation of the instrumentation. The person actually performs the analysis and
whatever pre-experiment research is necessary to ensure safe and reliable
instrumental operation. Much of this work, familiarization of the instrumental
operation and software, must be done
before the scheduled laboratory if the team hopes to finish an experiment in
a single afternoon.
Note that the work load of these positions will vary from experiment to
experiment, and the managers should feel free to redistribute duties as deemed
necessary. The only duty that cannot be redistributed is the writing of the
final report. However, while the manager is the report writer, all team members
are expected to be thoroughly familiar with the report contents and may be
expected by their managers to contribute to data interpretation.
Because of staggered experiment scheduling, no graded reports will be
handed back. Groups may schedule office time with me to discuss and review
graded reports throughout the semester. You are strongly encouraged to do this.
I reserve the right to change any report grade after all groups have completed
all experiments. You will be informed of any grade changes.
Reports
As stated, the Manager prepares the final report. The grade on this
report will be 70% of the teams’ grade on the experiment. The other 30% comes
from the individual notebooks. There are a few other general rules. Although the
System Operator actually performs the experiment, all
team members must be present when
the experiment is actually run in order to provide all components of information
input into the experiment. Intra-team communication is extremely important. At
the conclusion of the experiment, all team members should be thoroughly familiar
with all aspects of the experiment. All team members are responsible for
informing all other team members about their individual roles. It is also
necessary for all team members to
keep proper laboratory notebooks. A key factor in my grading the notebooks will
be whether or not I think the entire experiment could be repeated from any of
your notebooks. All notebooks should have two copies of any instrument output
(one taped into white pages, one taped into yellow pages), all calculations and
conclusions. Each team member should sign the report and keep a personal copy. A
copy of raw data and final data work up is part of the report. The report is a
stand-alone document, separate from any lab notebook. Although only the Reporter
will be preparing the final report, each team member is expected to be
knowledgeable about the report contents.
Reports will not be returned. Questions based on the specific reports will
appear on the lab final for 50 points of credit.
In addition to the report itself, for each experiment, the Manager must
submit an evaluation of each team members’ contribution to the final analysis.
This evaluation must be initialed by the team member in question signifying that
they have had the opportunity to read the evaluation. In addition, each team
member, including the Manager, is assigned a contribution percentage, typically
100%. If a team member does not live up to the group expectations then their
percentage should be reported as less than 100%. However, this means that
someone took up the slack and someone else’s percentage should then be
reported as more than 100%. The total for each group must be 100 x # of group
members. This percentage will be multiplied by the assigned grade to determine
individual grades. If you feel that the effort on any experiment was not equally
shared, and that a common group grade is unwarranted, then you are encouraged to
use variable percentages to account for these discrepancies.
Should a team member prove to be repeatedly unreliable and repeatedly
fail to live up to group expectations and norms, the Manager has the right to
“fire” the group member. The remaining group members will then be expected
to carry out the duties of this person. The dismissed group member must then
negotiate with Upper Management for the opportunity to complete the course
requirements. In order to avoid this situation, Managers and groups are
encouraged to respond and rectify potential problems at their earliest
appearance.
Reports and notebooks: As stated, the reporter/Manager prepares the
report on each experiment for the entire group. Each report should begin with
>a
title, experiment date(s), the Manager’s evaluations of each group member and
the percentage contributions for each group member.
Each group member must sign this page.
>a
brief statement of purpose
>an
abstract. Do not make this section too long! The most appropriate style is that
of the abstracts found in Analytical
Chemistry. I suggest that you read up to ten abstracts in that journal to
get a feel for the style. It is appropriate to summarize the results in the
abstract.
>an
experimental section with provides details on solution preparation and
experimental design sufficient in detail so as to allow duplication of the
experiment by someone of similar experience. Any
deviation from the handout should be clearly noted. Any
blunder, etc. should be clearly noted. Mention should be made of which team
member performed which duties. This section is ideally fashioned after the
experimental section of Analytical
Chemistry articles.
>data
presentation, including any calculations, tables, graphs, or printouts comes
next. Make sure all data items are properly labeled. Graphs should be presented
in a manner suitable to support the conclusions with the appropriate labels and
units. Raw data should be included. Label all raw data, and present it in an
easily readable form! I need to be able to check any and all calculations based
on the presentation of this section.
>data
analysis and concluding comments, reference
to literature data should follow. Include a bibliography section for
literature references. A brief mention of any possible sources of error and how
this affects results should be included. Be sure to answer any questions from
experimental handouts.
The
entire report, excluding figures, tables, and raw data, should not exceed six
pages!
Notebooks
Your laboratory notebook is the only medium through which you can legally
communicate the experiments and their results that you have accomplished. Your
ability to keep an accurate and complete record is the measure of your research
capabilities. All members of the research team are required to maintain their
research notebook up-to-date according to the general guidelines outlined in
this instruction form.
All work is dated with the date of the work evident on each page of the
notebook, usually on the top of the page or in the left hand margin. A separate
page should be reserved for each experiment that you perform, even when you are
performing a series of experiments. each experiment should be given a brief
title which may be as simple as “MEKC of Tea Components”
or “GC-MS of Fluorene”. The same title should be listed in the index.
Reserve the first two pages of your notebook for the index. You are required to
keep the index up-to-date. Upper Management reserves the right to spot check
anyone’s work at any time. You can continue in the notebook used for 4241.
The format for each experiment is as follows:
>After
listing the title, a brief experimental purpose should be given. If appropriate,
a chemical equation should be provided. Besides each major reactant, product, or
compound of interest, list its physical characteristics and constants.
>A
table of reagents should be provided, clearly listing the chemical name,
structure, source, amount actually used (g, mL), number of moles actually used,
an accurate description of the measuring device used.
>An
exact description of the lab activities, in sufficient detail so as to allow
another person to exactly follow your procedures. Observations, detailed
methods, etc. should be included in this section. Think of this section, in
particular, as a diary of your laboratory experience. -- Since you will be
divided into teams in this course it is extremely important, that any team
member’s notebook be sufficient to duplicate the experiment. You will need to
be explicitly clear as to which information is simply obtained from another
group member’s notebook and which information is original to your notebook. It
is important that no data be missing from anyone’s notebook. Equipment
settings, model numbers, etc. should be included.
>Analysis
of the data follows as well as interpretation of the results including clearly
outlined calculations. Everyone’s notebook should contain this section. No
notebook will be considered complete without an analysis of the data.
>Comments
regarding suggestions for future changes in the lab are always welcome.
Each notebook page should have
the legible name and the signature of the notebook owner. No more than one line
should be skipped in a notebook at any time unless a single line is drawn
through the extra lines clearly indicating the intention to keep those lines
blank. The notebook must be legible to another person. The notebook can be used
for scratch work, etc. as long as these sections are clearly identified.
Mistakes, etc. can only be indicated by a single line through the offending
material - no erasures, white-outs, etc.
Managers in particular may have additional information in their
notebooks. This information may be important in planning the experiment or in
commenting on the quality of other group members work and data. As always, think
of the notebook as a diary of the total experiment.