Abstract
To design and optimise efficient supported catalysts, the detailed structural and electronic properties as a function of performance are required. This chapter describes characterisation methods which can be applied ex situ (before and after catalysis) as well as in situ or operando (during catalysis, under process conditions). We focus on spectroscopic techniques, i.e. IR, NMR and XAS, the combination which will shown to be specially good for supported organometallic systems, providing complementary insights in structural and electronic properties of support, ligand and reactant coordination to the metal site and the metal site itself. Selected organometallic systems are chosen to demonstrate the strengths and limitations of the individual and combined techniques.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Anderson JR (1975) Structure of metal catalysts. Academic, New York
Hacquart R, Jupille J (2009) J Cryst Growth 311:4598–4604
Testino A, Bellobono IR, Buscaglia V, Canevali C, D’Arienzo M, Polizzi S, Scotti R, Morazzoni F (2007) J Am Chem. Soc 129:3564–3575
Gao Y, Elder SA (2000) Mater Lett 44:228–232
(a) Sindorf DW, Maciel, GE (1983) J Am Chem Soc 105:1487; (b) (1983) J Phys Chem 87:5576
Carneiro JT, Savenije TJ, Moulijn JA, Mul G (2010) J Phys Chem C 114:327–332
Tüysüz H, Lehmann CW, Bongard H, Tesche B, Schmidt R, Schüth F (2008) J Am Chem Soc 130:11510–11517
Nandi M, Sarkar M, Sarkar K, Bhaumik A (2009) J Phys Chem C 113:6839–6844
Kuschel A, Sievers H, Polarz S (2008) Angew Chem Int Ed 47:9513–9517
Barrer RM Zeolite synthesis: an overview, pp 221–244 in ref 11
Basset JM, Gates BC, Candy J-P, Choplin A, Leconte M, Grignard F, Santini C (1988) Surface organometallic chemistry: molecular approaches to surface catalysis, NATO ASI Series C231. Kluwer, Dordrecht
Rabo JA, New directions in molecular sieve science and technology, pp 245–270 in ref 11
Sun JL, Bonneau C, Cantin A, Corma A, Diaz-Cabanas MJ, Moliner M, Zhang DL, Li MR, Zou XD (2009) Nature 458:1154–U90
Corma A, Diaz-Cabanas M, Martinez-Triguero J, Rey F, Ruis J (2002) Nature 418:514–517
Corma A, Fornes V, Diaz U (2001) Chem Comm 2642–2643
Castaldi P, Santona L, Enzo S, Melis P (2008) J Hazard Mater 156:428–434
Martinez-Inesta MAM, Lobo RF (2007) J Phys Chem C 111:8573–8579
Evans J (1981) Chem Soc Rev 10:159–180
Hannemann S, Grunwald JD, van Vetgen N, Baiker A, Boye P, Schroer AG (2007) Catal Today 126:54–63
Evans J, Tromp M (2008) J Phys Condens Matter 20:184020
Sellin MF, Bach I, Webster JF, Montilla F, Rosa V, Avilés T, Poliakoff M, Cole-Hamilton DJ (2002) Dalton Trans 4569–4576
Fiddy SG, Evans J, Neisius T, Sun X-Z, Jie Z, George MF (2004) Chem Comm 676–677
Abdul Rahman MBB, Bolton PR, Evans J, Dent AJ, Harvey I, Diaz-Moreno S (2002) Faraday Discuss 122:211–222
Yang AC, Garland CW (1957) J Phys Chem 61:1504–1512
Eischens RP, Francis SA, Pliskin WA (1956) J Phys Chem 60:194–201
(1985) J Am Chem Soc 107:3139–3147
Brown SC, Evans J (1978) Chem Comm:1063–1064
Brown SC, Evans J (1981) J Mol Catal 11:143–149
Besson B, Morawek B, Smith AK, Basset JM, Psaro R, Fusi, A, Ugo R (1980) Chem Comm :569–571
Dornelas L, Choplin A, Basset JM, Hsu LY, Shore S (1985) New J Chem 9:155–157
Theolier A, Choplin A, Dornelas L, Basset JM, Zanderighi G, Sourisseau C (1983) Polyhedron 2:119–121
Alexiev VD, Binsted N, Evans J, Greaves GN, Price RJ (1987) Chem Commun 6:395–397
Corker J, Lefebvre F, Lécuyer C, Dufaud V, Quignard F, Choplin A, Evans J, Basset JM (1996) Science 271:966–969
Evans J, McNulty GS (1984) Dalton Trans 587–594
Meunier FC, Goguet A, Shekhtman S, Rooney D, Daly H (2008) Appl Catal A 340:196–202
Newton MA, Jyoti B, Dent AJ, Fiddy SG, Evans J (2004) Chem Comm :2382–2382
Dent AJ, Evans J, Fiddy SG, Jyoti B, Newton MA, Tromp M (2007) Angew Chem Int Ed 46:5356–5358
Thibault-Starzyk F, Vimont A, Fernandez C, Gilson JP (2000) Chem Commun 1003–1004
Thibault-Satzyk F, Vimont A, Gilson JP (2001) Catal Today 70:22–241
Gallas JP, Goupil JM, Vimon A, Lavalley JC, Gil B, Gilson JP, Miserque O (2009) Lngmuir 25:5825–5834
Chenevarin S, Thibault-Satzyk F (2004) Angew Chem 43:1155–1158
Butler JM, George MW, Schoonover JR, Dattelbaum DM, Meyer TJ (2007) Coord Chem Rev 251:492–514
Backus EHG, Eichler A, Kleyn AW, Bonn M (2005) Science 310:1790–1793
Alexiev VD, Binsted N, Cook SL, Evans J, Price RJ, Clayden NJ, Dobson CM, Smith DJ, Greaves GN (1988) Dalton Trans 2649–2654
Alexiev VD, Clayden NJ, Cook SL, Dobson CM, Evans J, Smith DJ (1986) Chem Commun 12:938–941
Wiench JW, Michon C, Ellern A, Hazendonk P, Iuga A, Angelici RJ, Pruski M (2009) J Am Chem Soc 131:11801–11810
Rendón N, Berthoud R, Blanc F, Gajan D, Maishal T, Basset JM, Coperét C, Lesage A, Emsley L, Marinescu SC, Singh R, Schrock RR (2009) Chem Eur J 15:5083–5089
Blanc F, Basset JM, Coperét C, Sinha A, Tonzetich ZJ, Schrock RR, Solans-Monfort X, Clot E, Eisenstein O, Lesage A, Emsley L (2008) J Am Chem Soc 130:5886–5900
Blanc F, Berthoud R, Coperét C, Lesage A, Emsley L, Singh R, Kreickmann T, Schrock RR (2008) Proc Natl Acad Sci USA 105:12123–12127
Kolyagin YG, Ivanova II, Ordomsky VV, Gedeon A, Pirogov YA (2008) J Phys Chem 112:20065–20069
Keeler C, Xiong J, Lock H, Dec S, Tao T, Maciel GE (1999) Catal Today 49:377–383
Hunger M, Seiler M, Horvath T (1999) Catal Lett 57:199–204
Haw JF (1999) Topics Catal 8:81–86
Hunger M, Weitkamp J (2001) Angew Chem Int Ed 40:2954–2971
Hunger M (2008) Progr NMR Spectrosc 53:105–127
Hunger M, Wang W (2004) Chem Commun:584–585
Wang W, Xu M, Buchholz A, Arnold A, Hunger M (2003) Magn Reson Imaging 21:329–332
Mildner T, Ernst H, Freude D, Kärger WU (1999) Magn Reson Chem 37:S38–S42
Xu S, Zhang W, Liu X, Han X, Bao X (2009) J Am Chem Soc 131:13722–13727
Sederman AJ, Mantle MD, Dunckley CP, Huang Z, Gladden LF (2005) Catal Lett 103:1–8
Koptyug IV, Lysov AA, Kulikov AV, Kirillov VA, Parmon VN, Sagdeev RZ (2004) Appl Catal A 267:143–148
Koptyug IV, Lysova AA, Sagdeev RZ, Parmon VN (2007) Catal Today 126:37–43
Koningsberger DC, Prins R (eds) (1988) X-ray absorption, principles, applications, techniques of EXAFS, SEXAFS and XANES. Wiley Interscience, New York
Safonova OV, Trmp M, van Bokhoven JA, de Groot FMF, Evans J, Glatzel P (2006) J Phys Chem B 110:16162–16164
van Bokhoven JA, Louis C, Miller JT, Tromp M, Safonova OV, Glatzel P (2006) Angew Chem Int Ed 45:4651–4654
Newton MA, Dent AJ, Evans J (2002) Chem Soc Rev 31:83–95
de Groot F (2001) Chem Rev 101:1779–1808
de Groot F (2005) Coord Chem Rev 249:31–63
Glatzel P, Bergmann U (2005) Coord Chem Rev 249:65–95
Stötzel J, Lutzenkirchen-Hecht D, Fonda E, De Oliveira N, Briois V, Frahm R (2008) Rev Sci Instrum 79:083107
Matsushita T (1981) Phizackerley. Jpn J Appl Phys 20:2223–2228
Tromp M, van Bokhoven JA, Arink AM, Bitter JH, van Koten G, Koningsberger DC (2002) Chem Eur J 8:5667–5678
Tromp M, van Bokhoven JA, van Strijdonck GPF, van Leeuwen PWNM, Koningsberger DC, Ramaker DE (2005) J Am Chem Soc 127:777–789
Fiddy SG, Evans J, Newton MA, Neisius T, Tooze RP, Oldman R (2003) Chem Commun 2682–2683
Tromp M, Sietsma JRA, van Bokhoven JA, van Strijdonck GPF, van Haaren RJ, van de Eerden AMJ, van Leeuwen PWNM, Koningsberger DC (2003) Chem Comm 128–129
Tromp M, van Berkel SS, van de Hoogenband A, Feiters MC, de Bruin B, Fiddy SG, van Bokhoven JA, van Leeuwen PWNM, Koningsberger DC (2010) Organometallics, DOI:10.1021/om9010643
Newton MA, Dent AJ, Jyoti FSG, (2007) Catal Today 126:64–72
Newton MA, Dent AJ, Fiddy SG, Jyoti B, Evans J (2007) J Mater Sci 42:3288–3298
Dent AJ, Evans J, Fiddy SG, Jyoti B, Newton MA, Tromp M (2008) Faraday Discuss 138:287–300
Evans J, Puig-Molina A, Tromp M (2007) MRS Bull 32:1038–1043
Cook SL, Evans J, Greaves GN (1983) Chem Commun:1287–1289
Evans J, Pillinger M, Zhang JJ (1996) Dalton Trans 2963–2974
Bianchini C, Burnaby DG, Evans J, Frediani P, Meli A, Oberhauser W, Psaro R, Sordelli L, Vizza F (1999) J Am Chem Soc 121:5961–597
Jezequel M, Dufaud V, Ruiz-Garcia MJ, Carrillo-Hermosilla F, Neugebauer U, Niccolai GP, Lefebvre F, Bayard F, Corker J, Fiddy S, Evans J, Broyer JP, Malinge J, Basset JM (2001) J Am Chem Soc 123:3520–3540
Le Roux E, Chabanas M, Baudouin A, de Mallmann A, Coperét C, Quadrelli EA, Thivolle-Cazat J, Basset JM, Lukens W, Lesage A, Emsley L (2004) Sunley GJ 126:13391–13399
Vidal V, Théolier T-C, Basset JM, Corker J (1996) J Am Chem Soc 118:4595–4602
Rataboul F, Chabanas M, de Mallmann A, Coperét C, Thivolle-Cazat J, Basset JM (2003) Chem Eur J 9:1426–1434
Berthoud A, Baudouin A, Fenet B, Lukens W, Pelzer K, Basset JM, Candy JP (2008) Coperét C 14:3523–3526
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2010 Springer Netherlands
About this chapter
Cite this chapter
Evans, J., Tromp, M. (2010). Instrumental Techniques for the Investigation of Heterogenised Catalysts: Characterisation and In situ Studies. In: Barbaro, P., Liguori, F. (eds) Heterogenized Homogeneous Catalysts for Fine Chemicals Production. Catalysis by Metal Complexes, vol 33. Springer, Dordrecht. https://doi.org/10.1007/978-90-481-3696-4_13
Download citation
DOI: https://doi.org/10.1007/978-90-481-3696-4_13
Published:
Publisher Name: Springer, Dordrecht
Print ISBN: 978-90-481-3695-7
Online ISBN: 978-90-481-3696-4
eBook Packages: Chemistry and Materials ScienceChemistry and Material Science (R0)