CTEC 1441 – Applied Instrumental Analysis I
Course Syllabus, Summer 2010
Course: CTEC 1441 – Applied Instrumental Analysis I
Instructor: Dr. Judy Chu
Office: K-206
Phone: 230-3435
E-mail: judy.chu@brazosport.edu
Office Hours: Monday
Required Books and Supplies:
1. Kenkel, John, Analytical
Chemistry for Technicians, 3rd Edition, Published by Lewis
Publishers, 2003.
2.
3. Organic Chemistry Lab
Notebook, Published by Chemical Education Resources, 1998.
4. Scientific Calculator.
5. Safety Goggles, must meet
ANSI Z87.1-1989 certification.
Course Requirements
1. Bring textbook, class notes
and calculators to class.
2. If you miss 2 or more labs,
you will be dropped from the class.
Course Goals:
Knowledge of procedures, equipment, and techniques used in industrial laboratories will be gained by students through the performance of laboratory experiments and writing of laboratory reports. Students will perform calculations, prepare standard solutions, analyze unknown samples, and operate various analytical instruments. Topics to be covered include sampling and sample preparation, gravimetric and titrimetric analysis, introduction to instrumental analysis, analytical separations, gas chromatography, and electrochemical methods. Prerequisite: CHEM 1411 or CHEM 1405. To pass the course, the student must successfully complete the laboratory portion with a grade of D or better.
Grades
Final Grades will be determined according to the
following system:
Total points possible: 100
90-100 = A
80-89 = B
70-79 = C
60-69 = D
0-59 = F
Exams 40%
Lab 40%
Final 15%
Attendance 5%
Examinations
The
examinations will last approximately one hour during class, with the exception
of the final, which will last two hours.
The exact date of each quiz will be announced in class closer to the
actual date. Students are allowed to
bring a one-page, hand written note card containing equations, etc., to the
exams. There will be no make-up
quizzes. The final exam grade will
replace any missed quiz grade. The final
will be comprehensive.
Homework Assignments:
·
A maximum homework grade of 10 points will be awarded to homework
assignments handed in on time. All work must be shown to obtain full
credit for the homework assignments.
·
Homework assignments are due prior to the start of each exam. For example, Quiz 1 covers chapters 6, 11 and
12; therefore, homework assignments for these chapters are due immediately
before the start of Quiz 1. The 10
points will be added to the corresponding quiz grade as bonus points.
·
Homework assignments for each chapter are listed in the following page.
Class Attendance Policy
·
If you are unable to complete this course, you must withdraw by Wednesday,
August 4, 2010. Withdrawal from a course
is a formal procedure, which you must initiate; I cannot do it for you. If you stop attending class and do not
withdraw, you will receive a performance grade, usually an “F”. If you think you must withdraw from this
course, please talk with me about it first.
·
Being late for class is an extreme annoyance to the entire class. Be on time!
·
Leaving class early is also an extreme annoyance to the entire class.
Academic Code of Conduct
Anyone who cheats on an exam will get a zero on that
exam. Students are advised to read the
Standards of Student Conduct in the Student Guide and Calendar for a
complete description of college policies, rules and regulations in this and
other areas.
Study Tips
Class attendance and participation will be important
to your success. Come to class prepared.
This means that you should spend at least six hours per week outside
of class studying and doing homework assignments. Space out your studies evenly. Your retention and understanding of the
material will be enhanced if you follow these simple rules.
Student Resources:
1.
Desire2Learn: https://online.brazosport.edu/index.asp
2.
Course Name: CTEC1441-JChu-SS10
User Name: First initial of first name, last name, and
last 4 digits of your Student ID number.
Initial Password:
BC+your pin number (example: bc123456)
obtained from the registrar.
E-mail:
|
WEEK |
LECTURE MW 5:30 – |
MW 7:30-9:20 PM |
|
June
7 |
Chapter 1 – Introduction
to Analytical Science
Chapter 2 – Sampling |
Safety
and check-in. See
lab syllabus for experiments Exp.
1 – Excel |
|
June
14 |
Chapter 3 – Gravimetric
Analysis |
Exp.
3 – Gravimetric Sulfate |
|
June
21 |
Quiz 1
Chapter 6 – Introduction to Instrumental Analysis |
Exp
2a – GC of Beer |
|
June
28 |
Chapter 6 – Introduction to Instrumental AnalysisChapter 11 – Analytical Separations
|
Exp
2a – GC of Beer Exp.
2b- GC of Gasoline |
|
July
5 |
Chapter 11 – Analytical
Separations Chapter 12 – Gas
Chromatography |
Exp.
2b- GC of Gasoline |
|
July
12 |
Review for Quiz 2 Quiz 2 |
Exp.
4 – Esterification (Synthesis and Extraction) |
|
July
19 |
Chapter 4– Introduction to
Titrimetric Analysis |
Exp.
4 – Esterification (GC
Analysis) |
|
July
26 |
Chapter 5.1– Applications
of Titrimetric Analysis Chapter
5.2 – Acid –Base Titrations |
Exp.
5a – Titration (Standardization of NaOH) Exp.
5b – Standardization of HCl |
|
Aug.
2 |
Chapter
5.2 – Acid –Base Titrations |
Exp.
5c – KHP unknown Exp.
5d – Soda Ash unknown |
|
Aug.
9 |
Review for Quiz 3 Quiz 3 |
Clean
up |
|
Aug.
16 |
Review for the final exam Final Exam – Wednesday
Aug. 18, 5-7PM |
|
*This
schedule is subject to change.
CTEC 1441 –
Applied Instrumental Analysis
Summer 2010
Dr. J. Chu
Office: K-206
Phone:
230-3435
Judy.chu@brazosport.edu
Homework Assignments: A maximum homework grade of
10 points will be assigned to completed homework assignments handed in on time
(prior to the start of the exam). These
points will be added to the corresponding exam grade as bonus points.
For Quiz 1: Due before Quiz 1
1
(1, 4, 6, 8, 20, 22, 24, 27, 28, 30, 31)
2
(3, 5, 18)
3
(10, 13, 16, 19, 23, 25, 27, 29, 37, 39)
For Quiz 2: Due before Quiz 2
6
(6, 9, 23, 25, 27, 28, 29, 39, 45, 47, 51)
11
(7, 9, 11, 14, 16, 24, 27, 28, 39, 41, 49, 50)
12
(1, 6, 10, 11, 13, 17, 26, 29, 31, 43, 45)
For Quiz 3: Due before Quiz 3
4 (5,
7, 9, 11, 12, 19, 22, 32, 33, 43)
5 (7,
10, 11, 13, 18, 27)
Dr. J. Chu
Office: K-206;
Phone: 230-3435;
Experiments for Applied
Instrumental Analysis Lab
1) Graphing using Excel
spreadsheet. (Handout)
2) The Gravimetric
Determination of Sulfate in a Commercial Unknown (Kenkel, page 57)
3) GC - Gas Chromatography
a) Experiment 42: Determination
of Ethanol in Wine (or Beer) by Gas Chromatography and the Internal Standard
Method. (Kenkel, page 359, and Handout)
b) Experiment 45: The Gas
Chromatography Determination of a Gasoline Component by the Method of Standard
Additions and the Internal Standard Method. (Kenkel, page 361, and Handout)
4) Esterification Pilot Process
a) Synthesis of methyl and isopropyl benzoate (Handout)
b) Determination of the relative yields of methyl and isopropyl benzoate using the GC (Handout)
5) Titrations Using a pH Probe
a) Experiment 8: Standardization of NaOH solution against
Potassium Phthalate. (Kenkel, page 92, and Handout)
b) Experiment 8: Standardization of HCl solution against NaOH.
(Kenkel, page 92, and Handout)
c) Experiment 10: Titrimetric Analysis of a Commercial KHP
Unknown for KHP. (Kenkel, page 135, and
Handout)
d) Experiment 11: Titrimetric Analysis of a commercial Soda Ash
Unknown for Sodium Carbonate. (Kenkel, page 135, and Handout)
Dr. J. Chu
Applied Instrumental Analysis Lab
Safety:
1. Safety goggles must be worn
at all times in the laboratory.
2. Know the locations of eyewashes,
showers, fire extinguishers and exits.
3. Use common sense.
4. Bare feet are NOT allowed
into the laboratory. Open sandals and
shoes are discouraged.
Laboratory Housekeeping:
1. Arrange apparatus neatly and
compactly. Keep all books except the
laboratory manual and laboratory notebook off the laboratory workbench.
2. Do not throw paper or solid
materials into the water troughs or sinks.
3. Keep all reagent bottles
clean (especially acids and bases).
4. Keep the lab bench area
clean. Pay particular attention to
keeping the balances clean and in order.
If you spill chemicals, clean them up immediately. Put caps back on reagent containers.
5. At the end of the laboratory
period, clean off your workspace with a sponge or wet paper towel. Perform proper shutdown of the
instruments. Check to see that the gas
and water have been turned off. You are
responsible for keeping the area neat.
Repeated failure to do so may result in loss of credit.
CLEAN UP AND INSTRUMENT SHUTDOWN STARTS 10 MINUTES BEFORE THE OFFICIAL END OF THE CLASS PERIOD.
When the time is up, you are supposed to be out of
the laboratory. Failure to properly
budget your time is presumptive of poor planning and your grade may suffer.
Grading:
1. Come prepared to the lab. The introduction (objective, discussion), safety, material and apparatus, should be written in the Laboratory Notebook prior to the beginning of the experiment. The format for the lab notebook is described in detail in the handout (Report Format for CTEC 1441). This pre-lab write-up (30 points) must be checked and initialed by me prior to the start of each experiment.
2.
Experimental
data and observations must be recorded in the Laboratory Notebook. The data sheets and observations (20 points)
must be completely filled out in ink and initialed by me before you leave the
lab. When you make an error, cross it
out with a single line. Do not use
liquid paper or obliterate the error.
For example: eror error
3. After a lab is finished, write the date that you finished the lab on the lab sign-up sheet. This signifies that your lab report will be due one week from that date.
4. Analysis of the data, calculations, including any tables and graphs, and summaries and conclusions (50 points) are due one week after the conclusion of the experiment.
5. Carbon copies of the complete experimental write-up are due the week after you finish the experiment.
6. Grading will be based on completeness of the experiments and the submitted report write-up.
REPORT FORMAT for CTEC 1441
I. Introduction
A. Objective
B. Discussion
I. Theory of operation performed (what happens in the analysis to obtain results).
II. Brief write-up of procedure.
III. Reactions if any.
IV. Method used to calculate or
to obtain results.
II. Safety
precautions involved.
III. Materials and Apparatus
A. Reagents used. Equipment used (glassware etc.)
used.
B. Instrument (type - model number etc.) used.
IV. Results
A. Raw Data and Observations
This
is the data obtained in the procedure (weights, titrations, sample volumes, any
data used to obtain results). The read
out charts from the instrument determinations and graphs are attached to the
reports. The data from them is shown here too, such as peak sizes, etc. No
results here! Any deviation from the
procedure should be included here.
B. Calculations and/or Results
All calculations, if any, are
shown here.
Results are shown here.
VI. Summary and Conclusion
A. Short summary of experiment. Results are included in the summary too!
B. Comments
pertaining to: Was objective obtained? How did the experiment go? Any problems?
Your evaluation of the experiment, etc.
Grading:
Objective 10 points
Discussion 10 points
Safety 5 points
Materials & Apparatus 5 points
Raw Data 20 points
Calculations & Results 30 points
Summary & Conclusion 20 points
Reports on experiments are due one week after they are
finished. Each week that the report is turned in late, 5 points will be taken
off the grade.
An Example Report:
Experiment ##
I. Introduction
A. Objective
To determine % ppm or what is
in an unknown.
B. Discussion
1. Theory
In a chromatographic determination, the components are separated by their interaction between the mobile and the stationary phases as they move through the column. Temperature, carrier gas flow rate and the type of packing in the column affect the separations. (This is in your book as are all theories of the other methods. If it is a titration, tell what a titration is.)
2. Procedure
Short procedure. Do not put all the steps you do in order to get an instrument ready for the analysis.
3. Reactions
Reactions if any.
4. Calculation formulas
How results are arrived at, calculations etc.
II. Safety
III. Materials and Apparatus
IV. Results
A. Raw Data and Observations
Sample weights.
Area counts and calculations
as in the internal standards method.
Milliliters of titrations.
Linear regression calculations
if needed.
Anything that is used to get
the results.
Dilutions.
Any deviations from the
written procedure.
B. Calculations and Results
Calculations for results.
Titration calculations.
Results are shown here. Do not
refer to charts, graphs or readouts. They are backup data only.
V. Summary and Conclusion
A. Summary
Short write up of what was
done. Results are shown here too.
B. Conclusion
How did it go? Was objective
obtained? Problems? Anything good or bad about the experiment.
Working With
Your Lab Partner
Lab
Partner’s Name_____________________________________________________________
Best
way to contact (phone,
email...)________________________________________________
To
become a productive lab partner, develop and fine-tune the following skills and
abilities:
1. RESPONSIBILITY. Before
leaving the lab, make sure both you and your lab partner have completely filled
out both your and your partner’s data sheets.
This is your insurance policy.
2. LISTENING SKILLS. You must
be able to put your own thoughts aside and listen without interrupting or
interpreting what your partner is saying.
Try it - it’s not easy.
3. SELF-CONFIDENCE. You must
believe in yourself and in the worth of your contributions. Speak up!
4. OPEN-MINDEDNESS. Welcome
change, and listen to the ideas others bring.
5. CREATIVITY. Try stretching
yourself outside of your routines. Try a
different method. It might work better
than your current method.
6. THOUGHT. Keep your goal in
sight. Instead of following the lab
manual like a recipe, consider the instructions to be a guide. When you make an error, how can you adapt the
manual’s procedure to still reach your goal?
Which type of balance will give you enough significant digits?
7. RELIABILITY. Do what you
say you’re going to do.
8. OBJECTIVITY. Assess ideas,
thoughts, and opinions from all sides, not just yours.
9. OPTIMISM. Look at problems
as opportunities. Knocking over the
beaker containing your product can lead to learning about purification
techniques.
10. COOPERATION. You must be able
to accept team decisions and work just as hard on other people’s ideas as you
do on your own.
Adapted
from Ern, B. L. and Lawley, C. M. (1992).
The office professional as a team player. Office Hours, 229, 1.