Robotics in the Instrumental Analysis Lab

The 378 lab is designed to teach how individual skills, once mastered, can be combined into progressively larger group efforts, working with progressively larger instrumental systems, eventually culminating in a public presentation and discussion of a fully computer-based, custom liquid chromatography instrument. The way that the experiments are organized is first shown in the block diagram below, and then in the individual laboratory experiments that are tagged as links to typical results from past lab students. The actual calendar for the Fall, 2001 offering can be viewed for specific dates on which the experiments will be performed.

I have been fortunate to have support from The Dow Chemical Co. Foundation and the Zymark Co., collectively, to use a Zymark Zymate II Laboratoy robot in my teaching of instrumetal analysis. I used it between 1991 and 2003, in the manner shown here and for the experiments shown below. I am indebted to these companies and to Dr. Mel Koch and Mr. Frank Zenie for their endorsements and encoiragement in this exciting stages of my career.


Lab Course Pedagogy

The Fall, 2002 offering is a special one. It is the last time teach this (or any) analytical chemistry course. After that, I retire and move on to other challenges. For most of my adult career I have wanted to teach an instrumental course that emphasized primarily pure instrumentation and modern interfacing electronics. This last offering has been that. The calendar for Fall 2002 shows how this was done. It may not meet the ACS CPT requirements, but it is what I truly believe should be offered in this last analytical course that most undergraduates will take. It took me from 1964 until fall, 2002 (and two academic institutions) to teach this one course the way I believe it should be taught, but it was worth the wait and all of the political struggles. Most of the experiments use LabVIEW® as the primary software environment for data acquisition, processing, display, and storage. The LabVIEW® "virtual instruments" (VI's) we use for the experiments are available for downloading as "stuffed .sit" binary Mac files by clicking here. If you wish to download a "portable data format" (x.pdf) version of a complete experiment writeup, without the LabVIEW® VI's, then click here.


The way in which the experiments expand from individual execution to whole group collaboration is shown in the diagram below.

lab structure


ACS CPT Approved Lab in Instrumental Analysis
Click on any linked item in the calendar below to see example data or instructional illustrations.
(Calendar Dates are for Fall, 2000)

Su

Monday

Tuesday

Wednesday

Thursday

Friday

S

3

4 Week 1 Activities

5

6

7

LabVIEW Tutorials:

3 people at 1:30 and 3 at 3:30 in SC 321/328

8 Class 1

LabVIEW Tutorials:

3 people at 1:30 and 3 at 3:30 in SC 321/328

9

10

11 Class 2

Staff Meeting
to explain BCD number/port representation

12 Lab 1 Week - DIO

Making a Digital pH Meter - Wiring BCD Connector -
Hardware

13 Class 3

Making a Digital pH Meter - Building the Front Panel -
Software

14

Using the Digital pH Meter - FET Electrode Response -
Chemist

15 Class 4

Story Board on Measuring Responses with Digital pH Meter

16

17

18 Class 5

Staff Meeting to explain A/D conversion in LabVIEW

19 Lab 2 Week - A/D

Measuring High Level Signal - Lissajous Plots

Software

20 Class 6

Measuring Low Level Signals with AD620 amp

Hardware

21

Measuring Physiological Signal with AD620 amp-

Chemist

22 Class 7

Story Board on A/D Conversion w/ AD620 Instr. Amp

23

24

25 Class 8

Staff Meeting to select personal waveform to send to chart recorder.

26 Lab 3 Week - D/A

Designing D/A Experiment Setup -

Chemist

27 Class 9

Plotting Special Chemical Waveforms-

Software

28

Recording Special Chemical Waveforms -

Hardware

29 Class 10

Story Board on Computer Generated Chemical Waveforms

30

1-Oct

2 Class 11

Staff Meeting to explain PID temp. control & select goals for same.

3 Lab 4 Week - all 3

Mock GC Oven - Learn Oven Temp. Control Apparatus

4 Class 12

Mock GC Oven - Build Temp. control VI

5

Mock GC Oven - Control Mock Oven Temp.

6 Class 13

SC Story Board. on Mock GC Oven Temp. LabVIEW Controllers

7

8

9 Class 14

Staff Meeting on Polarography and Heyrovsky

10 Lab 5 Week - Staircase Polaro
Dropping Mercury Electrode Study

Manager & Hardware

11 Class 15

Polarography - Effect of Gelatin Study

Manager & Software

12

Polarography - Concentration Study

Manager & Chemist

13 Class 16

Story Board on Quantitative Uses of Staircase Polarography

14

15

16 Class 17

Staff Meeting on how to set potential scan range for smooth CV display.

17 Lab 6 Week - CV

Cyclic Voltammetry - Gold Electrode Oxidation Study
Manager & Hardware

18 Class 18

Cyclic Voltammetry - Air Oxidation Fe+2-- Fe+3 Study
Manager & Software

19

Cyclic Voltammetry - Reversibility Study

Manager & Chemist

20 Class 19

Story Board on Precision in the Use of Cyclic Voltammetry

21

22

23 Class 20

Staff meeting to learn standard additions and select water sample source.

24 Lab 7 Week

Atomic Absorption.- Instrument Operation

Manager & Hardware

25Class 21

Atomic Absorption - Robot Solution Prep Design
Manager & Software

26

Atomic Absorption - Std Addition Detn Limits

Manager & Chemist

27 Class 22 -

Story Board on How to doAtomic Absorption Std Addition for Water Analysis

28

29

30

Fall Break

Get Mike ready for tutorials

31

Fall Break

Get Mike the Zymark lab robot ready for individual tutorials

1 Nov Class 23

Robot Tutorials:

2 people at 1:30 and 2 at 3:30 - room 328.

2

Robot Tutorials:

2 people at 1:30 and 2 at 3:30 - room 328.

3 Class 24

Robot Tutorials:

2 people at 1:30 and 2 at 3:30 - room 328.

4

5

6 Class 25

Staff Meeting to learn 3M IR cards and to select food flavoring component .

7 Lab 8 Week

FT/IR Spectral Subtraction -Using the 3M IR Card Technique

Manager & Hardware

8 Class 26

FT/IR Spectral Subtraction Project - Taking the Spectra on 3M IR Cards
Manager & Software

9

FT/IR Spectral Subtraction Project - Identifying the Peaks for Subtraction
Manager & Chemist

10 Class 27

Story Board on Utility of Using FT/IR Difference Spectra for Mixture Analysis

11

12

13 Class 28

Staff Meeting to coordinate lab group responsibilities for hydrolysis experiment.

14 Lab 9 Week
Robot Aspirin Hydrolysis Spectral Setup -

Full Company A

15 Class 29

Robot Aspirin Hydrolysis Reagents -

Full Company B

16

Robot Aspirin Hydrolysis Program -

Full Company C

17 Class 30

Story Board Showing of Robot Methods Development

18

19

20 Class 31

Staff Meeting to assign corrective measures before starting robot run.

21 Lab 10 Week

Start Robot on Aspirin Hydrolysis Run

Companies A, B, & C

22

Thanksgiving Break

Mike analyzes aspirin

23

Thanksgiving Break

Mike analyzes aspirin

24

Thanksgiving Break

Mike analyzes aspirin

25

26

27 Class 32

Post Aspirin Hydrolysis Rate Data on 3rd Floor Bulletin Board
28 Lab 11 Week

HPLC AutomationVirtual Instrumentation

29 Class 33

HPLC Automation Physical Instrumentation

30

HPLC Automation Laboratory Results

1-Dec Class 34

SC Public Demo of HPLC Proficiency Exam Instruments

2

3

4Class 35

Staff Meeting to decide if GC/MS run or public HPLC session be done.

5 Lab 12 Week

GC/MS Analysis -
Learning Instrument Operation

Full Company A

6 Class 36

GC/MS Analysis -
Recording and Processing LC Peaks and MS Spectra

Full Company B

7

GC/MS Analysis -
Figuring and Plotting Cracking Patterns

Full Company C

8 Class 37

Story Board Showing of GC/MS Methods Development

9

10

11 Class 38
Help Clean up the robot & the lab!

12

13

14Final exam week

starts - ends 20 Dec.

15

16

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