An electrochemical robotic system using standard microtiter plates as reaction wells for potentiostatic and galvanostatic electrosynthesis and high-throughput electroanalysis was conceived and realized using stepmotor driven positioning stages in combination with a flexible software. Electrode bundles specifically adapted to the experimental needs are accurately positioned in the wells of a microtiter plate followed by the automatic performance of sequences of electrosynthetic or electroanalytical techniques. The system allows us to work under inert-gas atmosphere, in aqueous and organic solvents, and to add or remove solutions by means of integrated syringe pumps. A specifically developed script language permits the user to perform very complex experimental sequences in the different wells of the microtiter plate. The hardware and software features of the developed electrochemical robotic system, the design of suitable electrode arrangements for electrosynthesis and electroanalytical techniques, as well as the reproducibility in aqueous and organic electrolytes are described. The performance of the system is demonstrated by redox screening of a Ru-complex library and by electrosynthesis with in situ analysis of a compound library.

1.
G.
Jung
(Ed.),
Combinatorial Chemistry
(
Wiley-VCH
, Weinheim,
1999
).
2.
R.
Hoffmann
,
Angew. Chem., Int. Ed. Engl.
40
,
3337
(
2001
).
3.
F.
Stieber
,
U.
Grether
,
H.
Waldmann
,
Angew. Chem.
111
,
1142
(
1999
);
F.
Stieber
,
U.
Grether
,
H.
Waldmann
,
Angew. Chem., Int. Ed. Engl.
38
,
1073
(
1999
).
[PubMed]
4.
J. J.
Hanak
,
J. Mater. Sci.
5
,
964
(
1970
).
5.
S. A.
Sundberg
,
Curr. Opin. Biotechnol.
11
,
47
(
2000
).
6.
C. D.
Bevan
and
R. S.
Lloyd
,
Anal. Chem.
72
,
1781
(
2000
).
7.
H.
Lund
and
O.
Hammerich
(Eds.),
Organic Electrochemistry
, 4th ed. (
Marcel Dekker
, New York,
2001
).
8.
B.
Speiser
,
Curr. Org. Chem.
3
,
171
(
1999
).
9.
E.
Steckhan
, in
Laboratory Techniques in Electroanalytical Chemistry
, 2nd ed., edited by
P. T.
Kissinger
and
W. R.
Heineman
(
Marcel Dekker
, New York,
1996
), pp.
641
681
.
10.
J. W.
Schultze
and
A.
Bressel
,
Electrochim. Acta
47
,
3
(
2001
).
11.
U.
Evans
,
P. E.
Colavita
,
M. S.
Doescher
,
M.
Schiza
, and
M. L.
Myrick
,
Nano Lett.
2
,
641
(
2002
).
12.
E.
Reddington
,
A.
Sapienza
,
B.
Gurau
,
R.
Viswanathan
,
S.
Sarangapani
,
E. S.
Smotkin
, and
T. E.
Mallouk
,
Science
280
,
1735
(
1998
).
13.
M. G.
Sullivan
,
H.
Utomo
,
P. J.
Fagan
, and
M. D.
Ward
,
Anal. Chem.
71
,
4369
(
1999
).
14.
R.
Feeney
and
S. P.
Kounaves
,
Electroanalysis
12
,
677
(
2000
).
15.
R.
Jiang
and
D.
Chu
,
J. Electroanal. Chem.
527
,
137
(
2002
).
16.
Y.
Sun
,
H.
Buck
, and
T. E.
Mallouk
,
Anal. Chem.
73
,
1599
(
2001
).
17.
A. K.
Yudin
and
T.
Siu
,
Curr. Opin. Chem. Biol.
5
,
269
(
2001
).
18.
T.
Siu
,
W.
Li
, and
A. K.
Yudin
,
J. Comb. Chem.
2
,
545
(
2000
).
19.
T.
Siu
,
S.
Yekta
, and
A. K.
Yudin
,
J. Am. Chem. Soc.
122
,
11787
(
2000
).
20.
S.
Suga
,
M.
Okajima
,
K.
Fujiwara
, and
J.-I.
Yoshida
,
J. Am. Chem. Soc.
123
,
7941
(
2001
).
21.
V.
Kulikov
and
V. M.
Mirsky
,
Meas. Sci. Technol.
15
,
49
(
2004
).
22.
S.
Nad
and
R.
Breinbauer
,
Angew. Chem.
116
,
2347
(
2004
);
S.
Nad
and
R.
Breinbauer
,
Angew. Chem., Int. Ed. Engl.
43
,
2297
(
2004
).
[PubMed]
23.
E.
Tesfu
,
K.
Maurer
,
S. R.
Ragsdale
, and
K. D.
Moeller
,
J. Am. Chem. Soc.
126
,
6212
(
2004
).
24.
S.
Reiter
,
K.
Eckhard
,
A.
Blöchl
, and
W.
Schuhmann
,
The Analyst
126
,
1912
(
2001
).
25.
T.-C.
Tang
,
A. P.
Deng
, and
H.-J.
Huang
,
Anal. Chem.
74
,
2617
(
2002
).
26.
This paper constitutes Part 2 of this series. For Part 1 see Ref 27.
27.
W.
Märkle
,
B.
Speiser
,
C.
Tittel
, and
M.
Vollmer
,
Electrochim. Acta
50
,
2753
(
2005
).
28.
S.
Dümmling
,
E.
Eichhorn
,
S.
Schneider
,
B.
Speiser
, and
M.
Würde
,
Curr. Sep.
15
,
53
(
1996
).
29.
E.
Lindner
,
I.
Warad
,
K.
Eichele
, and
H. A.
Mayer
,
Inorg. Chim. Acta
350
,
49
(
2003
).
30.
E.
Lindner
,
H. A.
Mayer
,
I.
Warad
, and
K.
Eichele
,
J. Organomet. Chem.
665
,
176
(
2003
).
31.
SBS Recommended Microplate Specifications, Society for Biomolecular Screening (SBS) standards committee
1999
.
32.
A. J.
Bard
,
Scanning Electrochemical Microscopy
(
Marcel Dekker
, New York,
2001
).
33.
G.
Gritzner
and
J.
Kuta
,
Pure Appl. Chem.
56
,
461
(
1984
).
34.
R.
Noyori
and
T.
Ohkuma
,
Angew. Chem.
113
,
40
(
2001
);
R.
Noyori
and
T.
Ohkuma
,
Angew. Chem., Int. Ed. Engl.
40
,
40
(
2001
).
[PubMed]
35.
S. L.
Queiroz
,
A. A.
Batista
,
G.
Oliva
,
M. T.
do P. Gambaredella
,
R. H. A.
Santos
,
K. S.
MacFarlane
,
S. J.
Rettig
, and
B. R.
James
,
Inorg. Chim. Acta
267
,
209
(
1998
).
36.
V. D.
Parker
,
Acta Chem. Scand.
24
,
2768
(
1970
).
37.
H.
Fernández
and
M. A.
Zón
,
J. Electroanal. Chem.
283
,
251
(
1990
).
38.
W.
Jugelt
and
L.
Grubert
,
Z. Chem.
25
,
408
(
1985
).
39.
S.
Crljenak
,
I.
Tabaković
,
D.
Jeremić
, and
I.
Gaon
,
Acta Chem. Scand., Ser. B
37
,
527
(
1983
).
40.
B.
Speiser
,
W.
Märkle
, and
S.
Heiß
, in
Elektronentransfer in Chemie und Biochemie
, edited by
J.
Russow
and
H. J.
Schäfer
,
GDCh-Monographien
, Frankfurt,
2001
, Vol.
23
, pp.
285
.
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