NMR studies of the molecular dynamics of tert-butyl chloride confined in the mesoporous molecular sieve MCM-41

Wasyluk, Lidia; Peplińska, Barbara; Klinowski, Jacek; Jurga, Stefan

doi:10.1039/b200634k

Cited by 12 publications

(19 citation statements)

References 40 publications

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“…The reduction is larger for 7.4 nm pore size, showing increasing restriction of the translational motion and tumbling with the reduced pore size. These results are in agreement with previous observations [1,2] and those given in literature [5,6,8]. Below the temperature of the solid I -solid II phase transition of TBC confined to 15.6 nm CPG, two spin-lattice relaxation components are revealed by proton and deuteron data.…”

Section: Spin-lattice Relaxationsupporting

confidence: 93%

“…The linewidths of the broad components are nearly constant up to 138 K and than grow continuously, reflecting the decreasing in the rate of the molecular reorientations C 3 and C 3 . We have made similar observations in previous investigations of TBC confined to other sizes CPG and other types of pores [1,2].…”

Section: 3supporting

confidence: 88%

“…The amount of the liquid TBC was chosen so that to fill the pores completely and keep a few percent of excess liquid outside the pores to detect the bulk and determine precisely the temperature depression. 1 …”

Section: Dsc Measurementsmentioning

confidence: 99%

“…The specific surface area measured by nitrogen adsorption equals 153 m 2 /g for 7.5 nm and 91 m 2 /g for 15.6 nm CPG. The sample preparation has been described in the previous papers [1,2].…”

Section: H Andmentioning

confidence: 99%

“…where all parameters have their usual meaning [1,2]. It is sufficient to assume the existence of only two kinds of tert-butyl groups in bulk-like phase of TBC in both 15.6 and 7.4 nm CPG.…”

Section: Spin-lattice Relaxationmentioning

confidence: 99%

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Molecular Dynamics of Tert-butyl Chloride Confined to CPG (7.4, 15.6 nm)

2005

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The paper complements our earlier NMR investigation of molecular dynamics of tert-butyl chloride restricted by geometries of the type MCM-41 and CPG by the new sizes of CPG and by differential scanning calorimetry method. We report proton and deuteron NMR lineshapes and the spin--lattice relaxation results of tert-butyl chloride in CPG of the 15.6 nm and 7.4 nm pore diameter in the temperature range 70 K ≤ T ≤ 292 K. The bulk-like component of the confined tert-butyl chloride, in temperatures corresponding to phase III, is interpreted as a composition of two dynamically different subphases. The parameters of motions of both subphases are derived. The tert-butyl group motion in both subphases is more restricted than in the bulk tert-butyl chloride, although the activation energies are lower. Differential scanning calorimetry was used to determine temperatures of the phase transitions (140 K ≤ T ≤ 292 K). The results show that the depression of the phase transition temperature is pore size dependent and that the confinement has less influence on transition to the plastic phase than on the freezing and on the solid II -solid III transition.

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Section: Spin-lattice Relaxationsupporting

confidence: 93%

Section: 3supporting

confidence: 88%

Section: Dsc Measurementsmentioning

confidence: 99%

Section: H Andmentioning

confidence: 99%

“…where all parameters have their usual meaning [1,2]. It is sufficient to assume the existence of only two kinds of tert-butyl groups in bulk-like phase of TBC in both 15.6 and 7.4 nm CPG.…”

Section: Spin-lattice Relaxationmentioning

confidence: 99%

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