Identification of human calculi with time-of-flight secondary ion mass spectrometry.

Time-of-flight secondary ion mass spectrometry was used to study four human calculi and to compare the results with those from twelve commercially available urinary calculi minerals including three organic compounds (L-cystine, uric acid and sodium urate). Phase identification of calcium phosphate compounds was carried out by considering the relative ion abundances of [Ca(2)O](+) and [CaPO(2)](+). Deprotonated [M-H](-) and protonated [M+H](+) uric acid were detected and used for component recognition in pure uric acid and in the mixed samples of struvite, calcium oxalate and uric acid. Iodine related to the medical history of a patient was also detected.

High performance temperature controlled UHV sample holder.

A requirement of many surface science studies is the capability to alter a sample temperature in a controlled mode. Sample preparation procedures such as heating or cooling ramps, high temperature spikes, fast annealing, or simply maintaining a sample at a very high, or very low, temperature are common. To address these issues, we describe the design and the construction of a multipurpose sample holder. Key points of this design are operation in an extended temperature range from liquid nitrogen (LN(2)) temperature to approximately 1300 K, temperature control during heating and cooling, low thermal inertia with rates up to 50 K s(-1) (heating) and -20 K s(-1) (cooling), and small heated volume to minimize background problems in thermal desorption spectroscopy (TDS) spectra. With this design the sample can be flash heated from LN(2) temperature to 1300 K and cooled down again in less than 100 s. This sample holder was mounted and tested in a multitechnique apparatus and adds a large number of sample preparation procedures as well as TDS to the list of already available surface analysis techniques.

Counterions in poly(allylamine hydrochloride) and poly(styrene sulfonate) layer-by-layer films.

The amount of counterions in layer-by-layer (LBL) films of poly(allylamine hydrochloride) (PAH) and poly(styrene sulfonate) (PSS) has been determined with X-ray photoelectron spectroscopy (XPS) for films prepared from solutions with various NaCl concentrations. Sodium and chloride counterions are present in LBL films produced from salt solutions, which are located at the surface and in the bulk of the films. The percentage of bulk counterions increases with the ionic strength of the polyelectrolyte before reaching a constant value. The bulk sodium/sulfur percentage ratios tend to 0.8 for samples washed with pure water and for samples washed with NaCl aqueous solutions, while the bulk chlorine/nitrogen percentage ratios tend to 0.5 for the same samples. The ratio between the percentages of polyelectrolyte ionic groups lies close to unity for all samples, indicating that counterions do not contribute to charge compensation in the polyelectrolyte during the adsorption process. The presence of counterions in LBL films is explained by Manning condensation near the polyelectrolyte ionic groups, leading to inter-polyelectrolyte ionic bondings via ionic networks. It is believed that condensation leads to the formation of NaCl crystallites in these LBL films, which was confirmed by X-ray diffraction measurements.