Rings and strain in pure silica zeolites

The stability of rings in pure silica zeolite frameworks is investigated through a new method. The energetic terms influencing the stability of rings are evaluated through the short-range plus electrostatics corresponding to SiO bonds and OSiO and SiOSi angles. Several atomistic force fields have been evaluated, and a reparametrization of the Vessal-Leslie-Catlow force field has been chosen because of its physical meaning and good structural accuracy. The ring energetics are analyzed and discussed in terms of local strain in the framework and in terms of geometric variables. This methodology allows to differentiate between the strain of rings of a given size in different zeolite structures. In particular, it is found that double four rings (D4Rs) are not necessarily, as previously stated, a strained secondary building unit. The analyses of D4Rs in the topologies AST, BEC, and LTA allow the calculation of its stability in the different structures showing high energy in BEC and LTA and low energy in AST. Implications of these results on nucleation of zeolites are drawn regarding the facility with which D4Rs are inserted in different frameworks.     

In-line sample trap columns with diatomite for large-volume injection in CZE–IM–MS

The analysis of low-abundant compounds with capillary zone electrophoresis–drift-tube ion mobility spectrometry–mass spectrometry (CZE–DTIMS–MS) is compromised due to the low injectable sample volumes in CZE and low duty cycle in DTIMS. Fritless packed in-line trap columns, using solid-phase extraction sorbent particles, have been used to increase injection volumes in CZE, but these columns are difficult to prepare and exhibit rapidly increasing back pressures. To provide smooth and complete filling of trap columns as well as to ensure higher and sustained flow rates though the columns, blends of cation and anion exchange particles with diatomite were used. The application of diatomite blends ensured the use of trap columns for at least 100 injections, with maximum injection volumes over 10 µl, which corresponds to an enrichment factor of more than 1000 over conventional injections in CZE–MS, enabling the detection of low nM concentrations of N-glycans with CZE–IMS–MS.