Development of a polar-embedded stationary phase with unique properties

This paper describes a new polar-embedded stationary phase that contains an internal sulfonamide functional group coupled with an ether linkage. The synthesis involves functionalization of spherical silica particles with ligands prepared in a multi-step synthesis. The resulting material contains 16.5% carbon, corresponding to a ligand coverage of 2.4mumol/m(2). Chromatographic evaluations indicates that the new stationary phase exhibits lower polarity than any other polar-embedded packings investigated, with additional features such as low silanol activity, excellent compatibility with 100% aqueous mobile phases, higher shape selectivity for polycyclic aromatic hydrocarbons, and strong affinity to nitro-containing compounds.     

Reflection of plane waves from the boundary of a pre-stressed compressible elastic half-space

The effect of pre-stress on the propagation and reflection ofplane waves in an incompressible isotropic elastic half-spacehas been examined recently by the authors (Ogden & Sotiropoulos,1997). In the present paper the corresponding analysis for compressiblematerials is detailed. In the two-dimensional context consideredfor incompressible materials the (homogeneous) plane waves werenecessarily shear waves. By contrast, in the compressible contextpure shear waves can propagate only in specific directions inthe considered principal plane and, in a general direction,a quasi-shear wave may be accompanied by a quasi-longitudinalwave, as is the case in the anisotropic linear theory. The dependenceof the (in-plane) slowness section on the pre-stress (and finitedeformation) and on the choice of constitutive law is elucidated.This information is used to determine the reflection coefficientsfor reflection of either a (quasi-) shear wave or a (quasi-)longitudinal wave from the boundary of the half-space and tocharacterize the different cases which arise depending on thegeometry of the slowness section. The theoretical results are illustrated by numerical calculationsfor the range of possible types of behaviour with referenceforms of strain-energy function and different states of finitedeformation and to the question of stability of the half-space.     

United States environmental protection agency perchlorate method 332.0. Statistically sound recovery studies in simulated drinking water

This research is a continuation of an earlier work, which evaluated the United States Environmental Protection Agency's Perchlorate Method 332.0, in which standards were prepared in deionized water over an extended concentration range (i.e., to a maximum of 200 μg/L). This current paper investigates the performance of the same method in which standards were made in simulated drinking water. A microbore format with a 15-μL injection volume was employed to conduct a recovery study and generate recovery curves (which hold the key to a statistically sound assessment of method performance in more complex matrices). The maximum analyte concentration range was 1 to 200 μg/L. For various subset concentration ranges, recovery evaluations were made using both raw peak-area data and analyte responses scaled by the internal standard (ISTD). The results indicate that in complicated matrices such as drinking water, ISTDs may not provide simultaneously high precision and recovery.     

Removal of metallic impurities from mobile phases in reversed-phase high-performance liquid chromatography by the use of an in-line chelation column

An in-line stripper column packed with iminodiacetate chelation resin is placed between the pump and injection valve and shown to remove metallic impurities from an HPLC system. We used a test procedure based on assessing the relative peak asymmetries of 2,2'-bipyridyl, a chelating analyte and 4,4'-bipyridyl, a non-chelating analyte. Results from use of polyether ether ketone (PEEK) and stainless steel pumps are evaluated. Analytical columns with titanium/PEEK and stainless steel frits are used to assess the role of frits in metallic contamination. We demonstrated that although metal-free pumping systems contribute significantly lower metallic impurities than stainless steel systems, metal is nevertheless present in the mobile phase and the chelating stripper columns were found useful in protecting the analytical columns from contamination. The stainless steel frits were not found to be significant contributors to the contamination.