Pressurized sample infusion: An easily calibrated, low volume pumping system for ESI-MS analysis of reactions

Simplified Real-Time Mass Spectrometric Analysis of Reactions

“…To demonstrate the efficacy of this approach, we studied the catalytic oxidation of triphenylphosphine by dioxygen mediated by Pd(PPh 3 ) 4 [1]) without the rigorous exclusion of oxygen, the palladium catalyst rapidly added dioxygen to form [Pd(PPh 3 )-(1)(O 2 )] − and catalyzed the formation of the phosphine oxide of 1 (1O, Figure 3). The appearance of the phosphine oxide is a good indicator of a less-than-perfect air-free technique, though of course such conditions are typical of many catalytic reactions.…”

Alkylation of [Pt2(μ-S)2(PPh3)4] with boronic acid derivatives

“…29,30 The reaction mixture is prepared in a Schlenk flask into which a length of PEEK tubing attached to the source of the mass spectrometer is inserted. An overpressure of 2 -4 psi is applied displacing the reacting solution into the MS.…”

Mechanistic insights from mass spectrometry: examination of the elementary steps of catalytic reactions in the gas phase

“…In terms of how to conduct these experiments successfully, we have covered the practical aspects -especially as practiced in our own laboratory -in a recent review [1]. The review covers issues such as cross-contamination, avoiding aggregation [2], protection from oxygen and water [3], ensuring the softest possible ionization [4], analysis in non-polar solvents such as toluene and hexane [5], selection of counter-ions and the design of charged tags [6,7], and the pressurized sample introduction method for continuous reaction monitoring [8]. Readers interested in these issues should sample the appropriate papers or go straight to the review for an overview of the problems and solutions.…”

“…We introduced pressurized sample infusion (PSI) [8,14] as a means of enabling real-time analysis of catalytic reactions, and have applied it to a variety of different systems. It has the beneficial properties of being able to be applied to entirely ordinary reaction flasks at any temperature up to reflux, and exhibits excellent point-to-point reproducibility.…”