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In-class announcements:
    For practice how to calculate error of a voltmeter related to tis internal resistance, study the problems and examples on p. 31.

 

Class syllabus (download the PDF version here but note that Test III was rescheduled)

CHEMISTRY 425, Analytical chemistry II.  Spring 2012
8:00-9:15 Tuesday and Thursday
La Tourette Hall 201

TENTATIVE  LECTURE  SCHEDULE

 

INSTRUCTOR: Dr. Petr Vanýsek; Office, La Tourette Hall 418

 

 

OFFICE HOURS: 9:30 – 10:30 Tuesdays and Thursdays. Other times by appointment only. I will help you with your problems, but when you come to see me, have your questions and problems already at least partially prepared. Bring your class notes along; I will want to see what you write down. Do not expect the instructor to give you your own private make-up class. When coming to the office hours, be prepared to share the office or the time with other students.

Laboratory sections (all meet in La Tourette Hall 304)

          1          Tuesday       17:30-21:20            TAs: Julie Meyer, Andrii
          2          Thursday     13:00-16:50                 Piatkivskyi, Daniel Renfus
          3          Thursday     17:30-21:20                 Tsehaye Eyassu
          4           Wednesday  17:30-21:20        

1 Tuesday 17:30-21:20 TAs: Julie Meyer, Andrii Piatkivskyi, 2 Thursday 13:00-16:50 Daniel Renfus, 3 Thursday 17:30-21:20 Tsehaye Eyassu 4 Wednesday 17:30-21:20

 

TEXTBOOK: D. A. Skoog, F. J. Holler and S. R. Crouch: Principles of Instrumental Analysis, 6th Ed. Thompson Brooks/Cole, Belmont, CA 2007. ISBN: 0-495-01201-7.

 

Recommended material: H. M. Kanare: Writing the laboratory notebook. American Chemical Society, Washington, D.C. 1985.

Recommended material: 1. H. F. Ebel, C. Bliefert and W. E. Russey, "The Art of Scientific Writing", VCH Publishers, New York 1987. 2. J. S. Dodd, Editor: The ACS Style Guide, ACS, Washington, 1986.

 

DATE

dd.mm.yy

TOPIC  

CHAPTER

17.01.12  

Introduction

 

19.01.12

Electronics, signals and noise

2-5

24.01.12

Electronics, signals and noise

2-5

26.01.12

Electronics, signals and noise
Download a text on operational amplifiers here.

2-5

31.01.12

Electronics instrumentation,

handling of data

class

notes

2.02.12 

Radiation,

spectrometer components

6-7

7.02.12

Radiation,

spectrometer components

6-7

9.02.12

Test I (Study guide)

 

14.02.12 

Schemes to detect radiation

6-7, handouts

16.02.12

Atomic spectrometry

8-10

21.02.12

Atomic spectrometry

8-10

23.02.12

Atomic spectrometry

13-18

28.02.12

Molecular spectrometry

13-18

1.03.12

Test II (Study guide)

 

6.03.12

Molecular spectrometry

13-18

8.03.12

Molecular spectrometry

13-18

13.03.12

Spring break

 

15.03.12

Spring break

 

20.03.12

Mass spectrometry
Note on proper way how to calculate isotope excess, correctiong what the book shows.

11 & 20

22.03.12

Mass spectrometry

11 & 20

27.03.12

X-ray spectrometry

and surface characterization

12 & 21

29.03.12

X-ray spectrometry

and surface characterization

12 & 21

3.04.12

X-ray spectrometry

and surface characterization

12 & 21

5.04.12

Electrochemistry (the test, originaly scheduled for this day was rescheduled for April 12)

 22-25

10.04.12

Electrochemistry

22-25

12.04.12

Test III (rescheduled, originally was on the fifth) (Study guide)

 

17.04.12

Electrochemistry

22-25

19.04.12

Electrochemistry

22-25

24.04.12

Electrochemistry 

(possibly rescheduled)

22-25

26.04.12

Electrochemistry

22-25

1.05.12

Electrochemistry

22-25

3.05.12

 

 

 

 

Tests

9 February   Test I   (Study guide) 100 points
1 March   Test II  (Study guide) 100 points
12 April   new date Test III   100 points
8 May  (Tuesday) Final 8:00 – 9:15
(Study guide)
200 points

 

Laboratory: 280 points as described in the laboratory handout

Grading: Total of 780 points is possible. Percent average (earned points divided by 7.8) will be used for determining the final grade. The following is a tentative scale: 85% A, 75% B, 65% C, 55% D, less than 55% F. Note however, that you have to complete all the laboratory assignments to get a passing grade.

Laboratory syllabus

LABORATORY  EXPERIMENTS            

 

EXPERIMENT

Note: The linked documents were current, to be used in the Spring 2011 lab. The handouts for the titles without links still need to be updated. You can find similar handouts from past years. Read them for your education, but do not print them to be used as your handouts. The new procedure might be different.

WEEK OF

(Instructor initials)

1.

Introduction to the uses of an oscilloscope and amplification function of an operational amplifier (new for 2012)
Guide for reading resistor values

23 Jan. 2012 (JM)

2.

Operational amplifiers II (updated for 2012)

30 Jan. (TE)

3.

Flame atomic absorption of cadmium

6 Feb. (TE)

4.

UV-VIS spectrophotometry (updated for 2012) 13 Feb. (AP)

5.

Spectrophotometric determination of manganeese in steel

20 Feb. (AP)

6.

Fluorescence spectrometry (updated for 2012) 27 Feb. (AP)

7.

Potentiometric simultaneous titration of chloride and iodide 

5 March   (DR)

8.

Ion selective electrodes - Chloride and fluoride

19 March (DR)

9.

Amperometric titration

26 March (JM)

10.

Cyclic voltammetry

2 April (JM)

11.

Rotated disk electrode 

9 April   (DR)

12.

Bipotentiometric end-point indication. Redox titration 16 April (TE)
     
     
 
[Note on Fourier transformation]
 

 

Material needed: Your textbook, handouts, bound a page-numbered laboratory notebook. The TA will specify protective gear and any other safety related matters. Necessary handouts  will be available on the web: http://www.vanysek.com/electrochem/ Some may be available also in class before the laboratory.

For writing the laboratory reports consult the specific handout.

The experiment is completed by submitting a laboratory report to the teaching assistant. Laboratory reports are due on Thursday at 5:00 P.M. the week following the week during which the laboratory work is supposed to be finished. The experiment, which would be due during the spring break, is due one week later. No exceptions! Note though, that groups may be assigned to two separate experiments on a particular day another experiment, different from the scheduled experiment may be performed on a particular day. This will of course change the lab numbers which will be due, but not the due date. There is a late penalty of two points for each day the report is late. (Each day counts, including weekends and there is no limit -- negative scores are possible.)

Each laboratory report is worth 20 points. You have to finish all the 12 laboratories to pass. The quality of your laboratory notebook and timely note taking is worth 40 points. From these points the teaching assistants may subtract demerit points for safety violations, tardiness, sloppiness and other breach of common sense and good manners. There is 280 points total in the labs. (If, for serious reason, e.g., failed instrument, a lab has to be cancelled, the grading will have to be adjusted accordingly, i.e., fewer points for the labs.)

 

FORMAT  FOR  LABORATORY  REPORTS

 (Note that additional requirements and due-dates will be specified by the teaching assistants).

Additional material can be downloaded here.

Word processed reports are required. The format should be a maximum of 4 pages, according to the following section. Standard font (10 or 12 pitch, 12 and Ariel is preferred) and single spacing should be used. The page format limit cannot be achieved by judicious adjustment of font sizes and margins. You should prepare Sections I - IV before the laboratory begins and bring it with you to the lab.

 

Section I NAME. (Do not write the word "Name" at the beginning of this section.) Give your name (on top right corner), date(s) the experiment was performed and the date submitted, course number (CHEM425), section (day of the week, time), full name of the TA in charge, names of the partners, if you were split into groups (which you will be). Do not generate a separate page only as a cover page.

Section II TITLE. (Do not write the word "Title" at the beginning of this section.) Experiment title and number (from the syllabus), identification number of the unknown and what concentration was determined for the unknown (with units and standard deviation).

Section III OBJECTIVE. Give a brief statement of the problem or experiment. State the parameter(s) to be determined. Do not use the text from the handouts, use your own words.

Section IV METHOD. Describe the method to be used and the basic principle of the method. Write in your words a brief synopsis of the experiment, following the handout, but omit procedural details unless there is a difference from those given. List equipment used. If you are using one of several identical instruments (e.g., a pH meter, an oscilloscope) note the inventory or serial number on your list.

Section V CALCULATIONS. Write all the calculations in a neat way here. Write first a general formula, using formal variables. Define the variables. Only then show a numerical calculation. (If a particular tricky equation is used, you may insert it by hand. However, learning how to do it on a word processor is a skill that will take you long way. Consider using an equation editor.)

Section VI DATA. Set the table conveniently to record all significant obtained data. If a large set of data is obtained as on a computer you should decide on some convenient way to reduce the number of printed points. Data output should be always supplemented (if not bypassed) by a graph.

Section VII RESULTS & ERROR. Write the results from section (V)  here. Remember to identify the unknown sample by its number or letter.

Section VIII GRAPHS, DISCUSSIONS, QUESTIONS, PROBLEMS. Report what you have learned, provide interpretation of the results. Compare with literature values of expected values. Point out accuracy and precision, possible sources of error, unusual aspects encountered and their possible effects on results, advantages and disadvantages (or limitations) of the technique, ideas for further work. Include here also answers to specific questions and exercises posed in the instructions that accompanied the assignment. This is where a graph imported into the word processor should fit.

From the report itself, the significance as well as the eventual use of the data should be clear to a knowledgeable reader who has not read the experimental procedure. A good two-step test is: 1) Do the plots and tables stand alone? Are all the units and their symbols included (use SI units) and do the titles clearly state the data contained? As an example, peruse an issue of Analytical Chemistry. 2) Does the text adequately explain the data and point out important values? Is the language correct?

Adherence to the above requirements as well as neatness and legibility of the work will be graded in addition to the correct value of the unknown and a sound discussion of results. Some of common errors include omission of units, reporting in wrong units (Do not forget any dilution you may have done. Typically, if an unknown is issued in a volumetric flask, report concentration when diluted to the mark.), omission of the standard deviation (Make enough experiments to be able to calculate it!), too few or too many (usually) significant figures and careless graphs.

Note on academic integrity

    In general, any graded work is to be performed by the student who is being graded, with the help of only such tools that are specifically allowed. For tests, your personal knowledge, pen and a calculator are specifically allowed tools. Books, notes, or other data storage devices are not allowed. Simple scientific calculators are preferred, although more advanced calculators are permissible as long as you honestly refrain from storing and retrieving substantial information such as equations or course material. Notebooks, laptops etc., with sizable storage space and a keyboard should not be used. No devices allowing communication with other people or storage media will be used. Cell phones, pagers, etc. must be turned off.

    Laboratory work is done in groups and discussion on solving the problems with others in the group is encouraged. However, the laboratory reports must be written individually. Substantial similarity of reports is cheating; in general, both involved parties are guilty. (Note for industrious students: Do not loan your finished reports to anyone.) Resist temptation to reuse old reports, reports found on the web and be careful not to copy the text from the lab handouts. I consider cheating to be the gravest academic offense and usually seek academic dismissal.  

 

Other issues:

 

-  Calculators: For tests only calculators without data storage/retrieval capability can be used. The calculator function on cell phones cannot be used during tests.
-  No smoking in the building, no food or drink in the class or the laboratory.
-  TAPING/RECORDING OF THE LECTURE:  You are encouraged to take good notes, reflecting your interpretation and understanding of the lecture. However, you are not permitted to make verbatim recording or transcription of the lecture.
-  ATTENDANCE: The material in the lectures is essential for understanding the subject. Although there is no formal enforcement of attendance, due to the size of the class your absence will be clearly apparent to me. Be prepared to explain and justify your absence to me.
-   CELL PHONES AND THE LIKE: Cell phones are great technology and it is great to have one with you for emergency. (Campus police: 815-753-1212). However, please, turn off your phones and other noise-making devices as a courtesy to others, and do not distract yourself by reading and sending text messages.

 

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Inception: 12 December 2006 (modeled after the syllabus from 1999) 
Last revised: 16 May 2014 14:23

© Petr Vanýsek 2012
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