In respect of complete digestion of organic waste materials, a relevant potent digestion technique was developed, and a prototype of a high pressure ashing device with infrared heating (IR-HP-asher) was built. The apparatus consists of six quartz digestion vessels inside a steel autoclave. The performance of the IR-HP-asher was tested for pure organic substances, for representative wastes from the recycling industry, and for several biological samples. In all cases, complete digestion could be attained within 90 min as well as complete recovery of metal(loid)s present in the sample. Concerning the completeness of digestion and absence of analyte loss, the IR-HP-asher was found to be superior to two conventional microwave digesters also tested.
Human urine samples after fish consumption have been investigated by low-temperature gas chromatography with inductively coupled plasma mass spectrometric detection after sample derivatization by hydride generation (HG/LT-GC/ICP-MS). This analytical technique enabled the identification of organometal(loid) compounds in human urine; species of the six elements germanium, arsenic, selenium, tin, antimony, and mercury were determined. Three different organic selenium species, two germanium species, seven arsenic species, four tin species, five antimony species, and one species of mercury were found; 18 of the 22 species detected could be identified. The relative detection limits ranged between 2 and 12 pg x L(-1) (x=element). These organometal(loid) compounds probably build up in the human body under the influence of micro-organisms, in the presence of hydrogen sulfide and methane, in the human intestine.
An inductively coupled plasma mass spectrometer (ICP-MS) was coupled on-line with an electrothermal vaporisation (ETV). The influence of aerosol gas flow as well as the variation of the coupling distance on the signal intensity was investigated and compared with the results of hydraulic high-pressure nebulizer (HHPN) measurements. Furthermore, temperature programs known from graphite furnace atomic absorption spectroscopy (GFAAS) were applied to ETV-ICP-MS. After optimisation of temperature programs, calibration series based on mono-element and multi-element solutions were carried out. The dynamic range and the detection limits of the method were determined. By use of internal standardisation it was tried to improve linearity and reproducibility. According to the results, internal standardisation does not have a great impact on linearity, but may be a useful tool to improve reproducibility. However, the latter is still low.