School of Engineering and Science - Jacobs University
School of Engineering and Science - Jacobs University
School of Engineering and Science - Jacobs University
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Number <strong>of</strong> particles<br />
30 Types <strong>of</strong> sample<br />
D<br />
B<br />
25<br />
20<br />
15<br />
10<br />
5<br />
0<br />
1.0 1.5 2.0 2.5 3.0 3.5<br />
Particle size, nm<br />
Fig. 4-5. Particles size distribution for B <strong>and</strong> D types <strong>of</strong> sample.<br />
From the elemental analysis it was found, that the B-series sample contains 43.5 % C,<br />
4.3 % N or 45 % cinchonidine, based on nitrogen content. From the TGA, the Pt<br />
content was found to be 25 % thus differing from the 40 % metal content in the original<br />
work [11] for 1.5 nm sized Pt cluster, probably because <strong>of</strong> the presence <strong>of</strong><br />
moisture/CO/CO2 <strong>and</strong> possibly acetic acid (30 %).<br />
Elemental analysis <strong>of</strong> the D-catalysts before reaction (please see below) showed 16.6 %<br />
C <strong>and</strong> 1.8 % N or 20 % cinchonidine, by making average between C <strong>and</strong> N. 63 % Pt<br />
was found from TGA. The remaining content was attributed to moisture/CO/CO 2 . The<br />
content <strong>of</strong> C <strong>and</strong> N on the D catalyst after 50 min <strong>of</strong> reaction was found to be 5.3 % <strong>and</strong><br />
0.8 %, correspondingly or 7 % <strong>of</strong> cinchonidine.<br />
4.3.2 FTIR investigation <strong>of</strong> cinchonidine adsorbed on Pt<br />
FTIR investigation <strong>of</strong> cinchonidine adsorbed on Pt was performed with cinchonidine<br />
modified conventional Pt/Al 2 O 3 (Fig. 4-6) <strong>and</strong> cinchonidine modified Pt nanoclusters B<br />
(Fig. 4-7) <strong>and</strong> D (Fig. 4-8) samples. The use <strong>of</strong> different Pt sample allows comparison<br />
<strong>of</strong> adsorbed modes <strong>of</strong> the cinchonidine molecule <strong>of</strong> Pt crystals with different sizes,<br />
starting from 1.2 (B-sample), passing 2.3 nm (D-sample) with 3.8 nm (conventional<br />
alumina supported Pt) <strong>and</strong> ending with comparison <strong>of</strong> adsorption mode <strong>of</strong> cinchonidine<br />
on microscopic Pt plane from the work <strong>of</strong> Ferri [76] <strong>and</strong> Zaera [77, 178]. In the Fig. 4-6<br />
the region below 1300 cm -1 is not accessible <strong>of</strong> IR investigation, due to the contribution<br />
<strong>of</strong> alumina background, whose FTIR spectrum can be found as an inset in the Fig. 5-5<br />
from the chapter 5.<br />
35