A Proposal to
Combine of CHEN 5503 Instrumental Analysis of Process Products
With
CHEN 49093 Unit Operations Laboratory
Preface: ChEN 5503 is to see 36 students in two sections for the first time next Fall. This fall
one section had 14 students and the other had 6 students. Problems with the 14 student section
had most to do with equipment availability due the structure of the courses.
CHEN 5503 Instrumental Analysis
Class Structure is to have all students working on one or two pieces of equipment. Schedule is
given below.
Grading:
Scaled curve with the highest score received corresponding to 100%
Notebooks – 10%
Midterms – 30%
Memo Reports – 60%
Lab SOP’s
Material Due
Physical Properties
Lab
MEB 3215 Orientation
Measuring Wt%
Lectures
Course Overview,
Moisture
Laboratory Safety,
TH Aug
Guidelines for
Ch. 1
Density by Density
Making Physical
Questionnaire
25
Preparation of Lab
Ch. 4
Meter
Measurements,
Reports
Reading a
Error Analysis I
Hydrometer
(TR)
Refractive Index of a
Liquid
Sampling, Sample Prep., Notebooks, Sampling,
Physical Properties
pp. 2-17,
Bring dry dog or
T Aug 30 Property Characterization Measurement Techniques
Lab
38-43
cat food sample
(KR)
(practice)
Literature Review
Physical
Thermal Analysis
Ch. 6.1,
Th Sep 1
Thermal Analysis
Properties/Thermal
Physical Properties
6.2
(TR)
Analysis
Lab
Laboratory Report
Thermal Analysis
Physical
Preparation (TR),
Ch. 7.1, Physical Properties
T Sep 6
Properties/Thermal
Notebooks
Atomic Spectroscopy
11.6
Lab
Analysis
(KR)
Bring Gatoraid like
Sieve Analysis
Physical Properties /
TH Sep 8
Midterm I
Analysis for Metals juice drink of you
Atomic Absorption
choosing
Intro to Molecular
Physical Properties /
Ch. 8.1,
Metals in a Juice Physical Properties
T Sep 13
Spectrometry (TR)
Atomic Absorption
8.2
Drink
Memo Report
Prepare Standards
UV/Vis Spectrometry
UV/Vis Introduction & Ch. 8.3,
TGA
TH Sep 15
UV/Vis Spectra &
and Colorimetry (KR)
Prepare Standards
8.4
Memo Report
Analysis Lab
Infra red Spectrometry
IR/FTIR Spectra &
T Sep 20
IR/FTIR Analysis
Ch. 8.5
Notebooks
(TR)
Analysis Lab
Separations and
Ch. 9.1,
Analysis for Metals
TH Sep 22
IR Analysis Problem
Chromatography (KR)
9.2
Memo Report
LC/GC Instruments and Introduction to Gas &
Gas & Liquid
T Sep 27
Ch. 9.2
Methods (KR)
Liquid Chromatography
Chromatography
Date
Lecture Topic
Lab Topic
Reading
TH Sep 29
Quantitative GC,
Troubleshotting (KR)
T Oct 4
Midterm II
Process Analytical
Chemistry (TR)
Process (on-Line)
T Oct 11
Analysis – Components
(TAR)
Process (on-Line)
TH Oct 13
Analysis – Systems (TR)
Gas/Liquid Analysis
Problem
Gas/Liquid Analysis
Problem
TH Oct 6
Ch. 9.2
HPLC Procedure for
Testing Sugars
UV-Vis/FTIR
Memo Reports
Last Labs
GC/LC Memo
Reports
Open Lab Project
Open Lab Project
Notebooks
Open Lab Project/ Lab
Cleanup
Last Lab Memo
Report
T Oct 18
(15 meetings over 8 wks)
Memo Reports (8) are 2 to 3 pages long and a good place to get CLEAR involved with the
students’ writing.
Problems with this structure to the class:
1.) Accommodating large student numbers.
2.) Lab Techs being responsible for a new piece of equipment every week. Before they have
gotten the hang of the software on one piece of equipment they need to be proficient on
another piece of software.
3.) Equipment is not used efficiently.
4.) Reports are coming in at a pace of one per week but only after the 4th week of class.
Work overload by Students after week 4.. Grading overload by Professor after week 4.
5.) An experiment can not be started until the lecture material has been given on that
instrument and methods.
6.) Students can follow SOP’s but can not develop analytical methods.
Suggested Restructuring with 2 week assignments
Date
Lecture Topic
TH Aug Course Overview, Laboratory Safety
25
(TR)
T Aug 30
Th Sep 1
Making Physical Measurements,
Error Analysis, Spiking Method
(TR)
Laboratory Memo Report
Preparation (TR),
Lab Topic
MEB 3215 Orientation
Organize Teams
First Lab Assignment
Deadline Oral Quiz #1
Material Due
Lab work
Lab work
T Sep 6
Sampling, Sample Prep., Property
Characterization
(KR)
2nd Lab Assignment
Notebooks
TH Sep 8
Working in Teams
Deadline 2nd Oral Quiz
Memo Report 1 Due 5:00
pm Dept Office
T Sep 13
TH Sep
15
T Sep 20
Report 1 Review
Lab work
Rewriting a Report (CLEAR)
Lab work
Return Reports
Rewriting a Report (CLEAR)
3rd Lab Assignment
Notebooks
TH Sep
22
T Sep 27
TH Sep
29
T Oct 4
Memo Report 2 Due 5:00
pm Dept Office
Rewriting a Report (CLEAR)
Deadline 3nd Oral Quiz
Report 2 Review
Lab work
Rewriting a Report (CLEAR)
Lab work
Return Reports
Rewriting a Report (CLEAR)
4th Lab Assignment
TH Oct 6
Rewriting a Report (CLEAR)
Deadline 4th Oral Quiz
Notebooks
Memo Report 3 Due 5:00
pm Dept Office
T Oct 11
TH Oct
13
T Oct 18
Th Oct
20
Report 3 Review
On-Line Instrumentation Lecture
(TR)
Projects Lab Organization
Introduction to Senior Lab, Map
Safety Equipment
Lab work
Lab work
Return Reports
1st Project Lab Assignment
Notebooks
Memo Report 4 Due 5:00
pm Dept Office
1st Project Lab Oral Quiz
Laboratories are 2 weeks long (4 lab periods) for 4 reports per student.
Lecture Time for CLEAR
Teams
Writing Reviews
Oral Presentations
Other
Fixed Laboratories for 8 weeks. Do 4 Labs.
The laboratories are rotated between the groups. No lecture materials are given. The students
are required to research the equipment and methods and prepare a plan to the instructor (Oral
Quiz) before they are allowed to operate the equipment and do their experiments.
Fixed Laboratory Assignments
1) Develop analytical methods for
a. The Atomic Absorbance (AA) spectrometer, and
b. The UV-visible spectrometer
to determine the concentration of potassium in potassium permanganate solutions (or copper in
copper sulfate). Compare results by AA with results by UV-visible spectroscopy and report your
results including accuracy of the two techniques. Pre prepared unknowns are to be measured and
reported on. Method development includes calibration standard preparation and instrument
calibration. (calibration of pipettes and volumetric flasks)
2) Develop analytical methods for the comparative determination of the concentration of
impurities in natural gas using
a. The Gas Chromatograph (GC) and
b. The FTIR spectroscopy.
Compare results by GC with results by FTIR spectroscopy and report your results including
accuracy of the two techniques.
3) Develop analytical methods for the comparative determination of the density of a liquid
using
a. A hydrometer,
b. A pyncnometer and
c. A densitometer
Compare results by the various methods and report your results including the accuracy of the
techniques. (Calibration of balances)
4) Develop analytical methods for the comparative determination of the percent moisture in
dog or cat food using
a. Thermogravimetry
b. Weight loss upon drying
Compare results by the various methods and report your results including the accuracy of the two
techniques. (Calibration of balances)
5) (New) Develop analytical methods for the determination of various sugars in an apple
juice drink using
a. Liquid Chromatography
b. Diamond ATR attachment to the FTIR.
Compare results by the various methods and report your results including the accuracy of the two
techniques.
6) Develop analytical methods for the determination of the concentration of isopropanol in
water using
a. Gas Chromatography, or
b. Liquid Chromatography,
c. Refractive Index and
d. Density
Compare results by the various methods and report your results including the accuracy of the
techniques.
7) Develop analytical methods for the determination of the concentration of potassium or
sodium or other ion in water solution using
a. Atomic Absorbance Spectroscopy
b. Specific Ion Electrode (New Capability)
Compare results by the various methods and report your results including the accuracy of the
techniques.
8) Develop analytical methods for the determination of the concentration of various organic
liquids in a mixture using
a. FTIR and
b. Gas Chromatography
Compare results by the various methods and report your results including the accuracy of the
techniques.
9) Develop analytical methods for the determination of the concentration of cumene,
benzene and hydrogen in a mixture using
a. FTIR and
b. Gas Chromatography
Compare results by the various methods and report your results including the accuracy of the
techniques.
10) Develop analytical methods for the determination of the concentration of potassium or
sodium or copper or other ion in water solution using
a. The UV-visible spectrometer
b. Specific Ion Electrode (New Capability)
Compare results by the various methods and report your results including the accuracy of the
techniques.
11) Other analytical method development with two methods being compared for a single
analysis. Each case needs an unknown to analyze for.
a. BET contrasted with Surface area by PSD
i. Gibbsite before and after thermal decomposition
b. Capillary Viscometer with Brookfield Viscometer
i. Unknown Oil
Unit Operations laboratory simply follows onto the fixed (analytical) experiments.
Unit Operations Laboratory (4 week assignments) Old Grading
Day
Report
1 - Formal Report
1- Letter Report
1 - Oral Report
Date
Lecture / Laboratory Topics
T
10/18
Points
100
100
100
Lecturer(s)
Organizational Meeting, Form Groups, Schedules & Procedures, First Lab
JJM,TAR
Assignment given out, Short Assignment-Mapping,
JT
Safety Lecture
(3291 MEB)
H
10/20
Working in Teams, Oral Quiz Deadline - I
JJM, TAR, KS
T
10/25
Formal Report Writing Guidelines
JJM
H
10/27
Making Physical Measurements/Hardware, Short Mapping AssignmentTAR
due
Report Writing continued (Summary/Conclusions)
T
11/1
JJM, KS
Trouble Shooting ,
Oral Reports Presentation, Partial Reports due
H
11/3
Statistically Designed Experiments
KH, JJM
T
11/8
Review of 1st Reports, Oral Presentation Lecture
TAR
H
11/10
How to Do a Letter Report
JJM
T
11/15
First Report due in ChE Office 1 PM, Second Lab Assignment
TAR, JJM
H
11/17
Oral Quiz Deadline – 2, Oral Presentations – I
TAR, JJM
T
11/22
Oral Presentations – II
TAR, JJM
T
11/29
Oral Presentations – III, General Feedback on 1st Report, Partial Reports
KH,
dueTAR, JJM
H
12/1
Oral Presentations – IV
TAR, JJM
T
12/6
Oral Presentations - V
TAR, JJM
H
12/8
Oral Presentations – VI, 2nd Report due in CHFEN Office 1 PM
New Grading
Report
4 - Memo Reports (2week Assignments)
Laboratory Notebooks
1 - Formal Report (4 week Assignment)
1 - Letter Report (4 week Assignment)
1- Oral Report (on one of the 2 week Reports)
Points
100
100
100
100
100