product was verified through comparison of its mass spectrum
with the instrument’s library and the molar percentage of each
product was calculated based on peak areas, previously calibrated
by using a series of standard solutions containing known amounts
of each component. Each experiment was repeated at least twice
in order to verify reproducibility; the variations in the calculated
TOF values for repeat experiments were typically within 10%.
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4
.8. Selective thiophene poisoning tests
The procedure for selective poisoning experiments was analogous
to the one described in section 4.6, except that the substrate
(
toluene or quinoline) was mixed with thiophene (~1 mol%) before
1
1
1
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6 A. Denicourt-Nowicki, A. Ponchel, E. Monflier and A. Roucoux,
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At the end of the reaction, the reactor was allowed to cool to
room temperature, vented, opened and the mixture was completely
transferred into a Schlenk flask under a nitrogen atmosphere. The
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2
3
1
0 cm of deoxygenated solvent was added and the mixture was
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was dried under vacuum for 2 h. A second hydrogenation run was
then performed with this catalyst; further recycling steps were
carried out by repeating this procedure.
2
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¨
We thank Dr Nim Lal Nakarmi and Cai Bo (Physics Department)
for assistance in preparing samples for TEM and Dr Zhongqi
Cheng (Geology Department) for assistance with XRD mea-
surements, both through the Environmental Sciences Analytical
Center (ESAC) of Brooklyn College, and Drs. Alan Lyons and
Qianfeng Xu (Chemistry Department, College of Staten Island,
CUNY) for assistance and use of their XPS instrument. Acknowl-
edgement is made to the Donors of the American Chemical Society
Petroleum Research Fund and to the US Department of Energy
for support of this research through Grants 47472-AC3 and DE-
EE0003129, respectively.
6
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Dalton Trans., 2011, 40, 10621–10632 | 10631