The construction of a high-temperature reaction cell for operando X-ray absorption spectroscopy characterization is reported. A dedicated cell was designed to operate as a plug-flow reactor using powder samples requiring gas flow and thermal treatment at high temperatures. The cell was successfully used in the reaction of dry reforming of methane (DRM). We present X-ray absorption results in the fluorescence detection mode on a 0.4 wt. % Ni/ZrO2 catalyst under realistic conditions at 750 °C, reproducing the conditions used for a conventional dynamic microreactor for the DRM reaction. The setup includes a gas distribution system that can be fully remotely operated. The reaction cell offers the possibility of transmission and fluorescence detection modes. The complete setup dedicated to the study of catalysts is permanently installed on the Collaborating Research Groups French Absorption spectroscopy beamline in Material and Environmental sciences (CRG-FAME) and French Absorption spectroscopy beamline in Material and Environmental sciences at Ultra-High Dilution (FAME-UHD) beamlines (BM30B and BM16) at the European Synchrotron Radiation Facility in Grenoble, France.

1.
S. R.
Bare
and
T.
Ressler
, “
Characterization of catalysts in reactive atmospheres by X-ray absorption spectroscopy
,” in
Advances in Catalysis
, 1st ed. (
Elsevier, Inc.
,
2009
), Chap. 6.
2.
B. R.
Fingland
,
F. H.
Ribeiro
, and
J. T.
Miller
,
Catal. Lett.
131
,
1
(
2009
).
3.
Y.
Iwasawa
,
K.
Asakura
, and
M.
Tada
,
XAFS Techniques for Catalysts, Nanomaterials, and Surfaces
(
Springer International Publishing AG
,
Switzerland
,
2017
).
4.
J.-D.
Grunwaldt
,
M.
Caravati
,
S.
Hannemann
, and
A.
Baiker
,
Phys. Chem. Chem. Phys.
6
,
3037
(
2004
).
5.
F. W.
Lytle
,
P. S. P.
Wei
,
R. B.
Greegor
,
G. H.
Via
, and
J. H.
Sinfelt
,
J. Chem. Phys.
70
,
4849
(
1979
).
6.
See www.exafsco.com for details about commercial XAS cells.
7.
S.
Hannemann
,
M.
Casapu
,
J. D.
Grunwaldt
,
P.
Haider
,
P.
Trüssel
,
A.
Baiker
, and
E.
Welter
,
J. Synchrotron Radiat.
14
,
345
(
2007
).
8.
D.
Bazin
,
A.
Triconnet
, and
P.
Moureaux
,
Nucl. Instrum. Methods Phys. Res., Sect. B
97
,
41
(
1995
).
9.
B. S.
Clausen
and
H.
Topsøe
,
Catal. Today
9
,
189
(
1991
).
10.
G.
Sankar
,
P. A.
Wright
,
S.
Natarajan
,
J. M.
Thomas
,
G. N.
Greaves
,
A. J.
Dent
,
B. R.
Dobson
,
C. A.
Ramsdale
, and
R. H.
Jones
,
J. Phys. Chem.
97
,
9550
(
1993
).
11.
N. E.
Tsakoumis
,
A.
Voronov
,
M.
Ronning
,
W.
Van Beek
,
O.
Borg
,
E.
Rytter
, and
A.
Holmen
,
J. Catal.
291
,
138
(
2012
).
12.
See http://fmb-Oxford.com for details about the FMB-Oxford heating gas blower.
13.
J.-D.
Grunwaldt
,
N.
van Vegten
,
A.
Baiker
, and
W.
van Beek
,
J. Phys.: Conf. Ser.
190
,
12160
(
2009
).
14.
W.
van Beek
,
O. V.
Safonova
,
G.
Wiker
, and
H.
Emerich
,
Phase Transitions
84
,
726
(
2011
).
15.
S. J.
Tinnemans
,
J. G.
Mesu
,
K.
Kervinen
,
T.
Visser
,
T. A.
Nijhuis
,
A. M.
Beale
,
D. E.
Keller
,
A. M. J.
Van Der Eerden
, and
B. M.
Weckhuysen
,
Catal. Today
113
,
3
(
2006
).
16.
G. L.
Chiarello
,
M. V.
Dozzi
,
M.
Scavini
,
J. D.
Grunwaldt
, and
E.
Selli
,
Appl. Catal., B
160-161
,
144
(
2014
).
17.
J. D.
Grunwaldt
,
S.
Hannemann
,
C. G.
Schroer
, and
A.
Baiker
,
J. Phys. Chem. B
110
,
8674
(
2006
).
18.
S. R.
Bare
,
N.
Yang
,
S. D.
Kelly
,
G. E.
Mickelson
, and
F. S.
Modica
,
Catal. Today
126
,
18
(
2007
).
20.
A.
Bansode
,
G.
Guilera
,
V.
Cuartero
,
L.
Simonelli
,
M.
Avila
, and
A.
Urakawa
,
Rev. Sci. Instrum.
85
,
84105
(
2014
).
21.
D.
Testemale
,
R.
Argoud
,
O.
Geaymond
, and
J. L.
Hazemann
,
Rev. Sci. Instrum.
76
,
043905
(
2005
).
22.
V. F.
Kispersky
,
A. J.
Kropf
,
F. H.
Ribeiro
, and
J. T.
Miller
,
Phys. Chem. Chem. Phys.
14
,
2229
(
2012
).
23.
S.
Wang
,
G. Q.
Lu
, and
G. J.
Millar
,
Energy Fuels
10
,
896
(
1996
).
24.
A. J.
Brungs
,
A. P. E.
York
,
J. B.
Claridge
,
M.
Carlos
, and
M. L. H.
Green
,
Catal. Lett.
70
,
117
(
2000
).
25.
See http://www.htw-gmbh.de/index.php5?lang=en&nav0=0 for Hochtemperatur-Werkstoffe (GmbH).
26.
K.
Tamura
,
M.
Inui
, and
S.
Hosokawa
,
Rev. Sci. Instrum.
66
,
1382
(
1995
).
27.
B.
Fang
,
N. K.
Chaudhari
,
M.-S.
Kim
,
J. H.
Kim
, and
J.-S.
Yu
,
J. Am. Chem. Soc.
131
,
15330
(
2009
).
28.
F.
de Groot
,
G.
Vankó
, and
P.
Glatzel
,
J. Phys.: Condens. Matter
21
,
104207
(
2009
).
29.
D.
Cabaret
,
A.
Bordage
,
A.
Juhin
,
M.
Arfaoui
, and
E.
Gaudry
,
Phys. Chem. Chem. Phys.
12
,
5619
(
2010
).
30.
B.
AlSabban
,
L.
Falivene
,
S. M.
Kozlov
,
A.
Aguilar-Tapia
,
S.
Ould-Chikh
,
J.-L.
Hazemann
,
L.
Cavallo
,
J.-M.
Basset
, and
K.
Takanabe
,
Appl. Catal., B
213
,
177
(
2017
).

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