1. Laboratory exercise Puu-0.3130
Instrumental analysis in surface, polymer and nanoscience
Lokanathan Arcot
2nd March 2015

2. Outline Chronology of the laboratory works Each step in detail
General issues
Writing the report

3. Chronology Students are divided in groups consisting of two persons
Each group receives one sample
List of samples
Chitosan
Xylan (from birch wood)
Cellulose triacetate (DS 3)
Cellulose acetate (DS 2.5)
Carboxymethyl cellulose (DS 0.9)
Carboxymethyl cellulose (DS 1.2)
Pectin
Guar gum
Methyl cellulose
Hydroxyethyl cellulose ethoxyate (quaternized)
Cationic starch (DS 0.75)
Hydroxypropyl cellulose

4. (morphology/thickness)
Sample Analysis
NMR
(30 min)
Sample
identification
(meeting)
(2h)
Sample
identification
(~4h)
IR (45 min)
Raman
(30 min)
Find out
a solvent
for your sample
(~1 h)
AFM
(morphology/thickness)
(4h)
XPS
(chemical analysis)
(2 h)
Make a solution
and spin coat
ultrathin films
(1.5 h)

5. Chronology IR (3rd and 5th March)
Experimental Exercise ( Total 8 groups)
6 groups with 3 students each; 2 groups of 2 students each )
IR (3rd and 5th March)
Raman (4th March)
Sample Identification (6th March)
Sample dissolution (10,11th of March)
Spin Coating (12,13 of March)
AFM (16,17,18,19,20,24,25,26 March)
XPS
NMR (2,8,9 April)
* QCM-D, SPR (Demo only) (23 and 27 March)

6. Infrared (IR) spectroscopy
Sample form – Powder (KBr pellet preparation)
Samples will be analyzed with photoacoustic IR
Location: PUU 1
Samples must be dry before the measurement (should be placed in the oven in the IR room)
Contact person (Depending on date)
Meeting place room 234 PUU 1
3rd March
and
5th March

7. Raman spectroscopy Sample form – Powder (Direct measurement)
Samples will be analyzed with confocal and UV raman
Time allocated for each group: 15 min
Location: room 303 in PUU2
Contact person: Leonardo Galvis Rojas

8. Meeting on sample identification
IR data should be utilized to identify which sample your group has
Search for literature on IR spectra on polysaccharides to compare with your spectra
A meeting is scheduled where each group presents their spectra and proposes the identity of their sample (with argumentation)
Location: PUU1, room 311
Contact person: Lokanathan Arcot

9. Dissolution and spin coating
After the identifying the sample, each group must find out what is a suitable solvent for their sample
Each group must come up with a proposition for a suitable solvent before entering the exercise dealing with dissolution and spin coating
The sample will be dissolved in a suitable solvent for spin coating
Furthermore, the sample will be dissolved in a deuterated suitable solvent for NMR analysis
Total 2 solutions – 50 mL 10g/ml normal solvent
200 mg in 1 ml deutrated solvent
Films of four different thicknesses will be cast by spin coating from solutions of four different concentrations (10, 5, 2.5 and 1 g/l)
Duration: 1h 30 min
Location: room 339 in PUU1
Contact person:
(For Sample dissolution)
(For Spin coating)

10. Atomic Force Microscopy (AFM)
The morphology of spin coated ultrathin films will be characterized with AFM
The thickness of the ultrathin films will be determined by scratching the sample and measuring the height difference in the scratch with AFM
Time allocated for each group: 4 hours
Location: PUU1, room 336 (wait outside until escorted inside)
Contact person:

11. X-ray Photoelectron Spectroscopy (XPS)
The chemical nature of the spin coated ultrathin films will be probed with XPS (Used the spin coated sample with 10g/l sample concentration, the same sample used for AFM)
This is a demonstration: the measurements are so long that you cannot follow them in real time
The results will be ed to you shortly after the demonstrations
Contact person: Leena-Sisko Johansson phone: )
Meeting point – Room 318, PUU 1

12. Nuclear Magnetic Resonance (NMR)
The sample dissolved in a suitable deuterated solvent will be analyzed by NMR spectroscopy
Time allocated for each group: 45 min
Place: Chemistry Department, room D238b
Contact person: Reeta Salminen phone: )

13. General issues
Please carry a memory stick throughout the exercises; it is handy for data collection
If you cannot find a suitable time for your group, please contact the contact person of the relevant exercise

14. Laboratory report Each group hands in a laboratory report
Detailed instructions on how to construct the report will appear shortly in Noppa
Deadline for the report: 25th May 2015
Submission through to Lokanathan Arcot
All reports will be automatically checked for plagiarism

15. What happens now? Form the groups (three persons each)
Take your samples
Book the times for each exercise
Let’s move to the IR lab to get your samples dehydrated overnight