Determination of ammonium, calcium, magnesium, potassium and sodium in drinking waters by capillary zone electrophoresis on a column-coupling chip.

This work deals with simultaneous determination of ammonium, calcium, magnesium, sodium and potassium in drinking waters by capillary zone electrophoresis (CZE) on a column-coupling (CC) chip with suppressed hydrodynamic and electroosmotic transports. CZE separations were carried out in a propionate background electrolyte at a low pH (3.2) containing 18-crown-6-ether (18-crown-6) to reach a complete resolution of the cations. In addition, triethylenetetramine (TETA) coated the inner wall surface of the chip channels. The concentration limits of detection (cLOD) for the studied cations ranged from 4.9 to 11.5 microg/l concentrations using a 900 nl volume of the sample injection channel. 93-106% recoveries of the cations in drinking waters indicate a good predisposition of the present method to provide accurate analytical results.

Analysis of antibiotics in urine and wipe samples from environmental and biological monitoring--comparison of HPLC with UV-, single MS- and tandem MS-detection.

Results of the simultaneous determination of the structurally different antibiotics cefazoline, cefotiame, cefuroxime, chloramphenicol, ciprofloxacin, ofloxacin, sulfamethoxazole and trimethoprim from environmental and biological monitoring using high-performance liquid chromatography with UV, single mass and tandem mass spectrometry were compared. For sample enrichment and clean-up a SPE method using bakerbond C18 cartridges was developed. Mean recovery rates were above 70%. Because of the complex urine matrix, only the wipe samples could be analyzed by UV-detection. However, UV-detection and single MS-detection are useful for control measurements after spillage, e.g. (LOD=1-2 ng/cm(2)). Samples from biological monitoring of occupational uptake should be analyzed by LC-MS/MS. The limits of detection (LOD) in urine ranged from 0.4 to 70 microg/L for LC-MS and 0.01 to 0.9 microg/L for LC-MS/MS detection. The limits of detection in wipe samples ranged from 0.003 to 0.13 ng/cm(2).

Comparison of spark OES methods for analysis of inclusions in iron base matters.

A statistical model for the evaluation of the emission intensities of single spark discharge spectra on three different spark OES instruments (ARL 4460, OBLF-QSN 750, SpectroLab) was developed for the analysis of non-metallic inclusions in steel. In total, the raw measurement data consists of several thousand data points (intensities), about 2000 per element channel. A histogram (frequency distribution of pulse height intensities) of inclusion-forming elements like Al, Ti and Mn performed in intensity classes and the related frequencies contain the information of the measurement. Measurement of a pure iron sample with slag powder rubbed into the surface by single spark emission spectrometry changes the originally (nearly) symmetrical histogram for inclusion related element signals to higher intensities. Thus, the known asymmetry of the histograms for steel samples is explained by the presence of inclusions.A sum of Gaussian fits representing the histogram was expected to express the different elemental species and inclusion sizes by using the variables mean, standard deviation and area of the peak containing the information of the measurement. Even a less complex approximation using a sum of two Gaussian fits is not practicable for the Al, Ti and Mn channel and the three spectrometers due to too many variables in the fitting function resulting in a large scattering. Coincidences of high signals in different element channels could be seen only in terms of MnS.A further attempt was to form the second differential of the logarithmic normal distribution and to compare the resulting partial areas below the functional graph to get information about the asymmetry of the fitting function of the original histogram. Two different procedures to evaluate the effect of the inclusion concentration on the size of the partial areas were applied to measurements on a set of synthetic samples with different concentrations of aluminium oxide in micro alloy steel. The results of both evaluation procedures correlate significantly with the inclusion concentrations. Electronic Supplementary Material is available if you access this article at http://dx.doi.org/10.1007/s00216-002-1595-1. On that page (frame on the left side), a link takes you directly to the supplementary material.