| Abstract: | The determination of ultra-trace levels of chromium and nickel in biological samples had previously been very difficult due to serious contamination problems in conventional laboratories. Contamination control in a conventional laboratory was studied and contamination due to various sources was minimized systematically. In addition to chromium and nickel, zinc was also determined as an indicator element prone to contamination. Measurements were carried out using electrothermal atomic absorption spectrometry (ETAAS). Contamination from the sample handling steps, digestion vessels, atmospheric fallout, and the effect of the liquid contact area were studied. In the sample handling steps, even simple procedures, such as transferring the sample solution from the volumetric flask by pouring, led to significant contamination due to the large area of liquid contact. This contamination source was eliminated by transferring the sample solution using an automatic pipette. The most suitable method for decontamination of the digestion vessels was steaming with boiling nitric acid as opposed to leaching with nitric acid at room temperature. Quartz was found to be a more suitable digestion vessel material than Teflon-PFA when Cr and Ni were determined. For Zn determination, Teflon-PFA was more suitable. Contamination from atmospheric fallout was highest in the fume hood and was reduced by simply closing the labware into Minigrip® bags before use. The surface area of the labware in contact with the handled liquid volume should be kept at a minimum because even a simple procedure, such as preparing standard solutions in volumetric flasks, can lead to significant contamination if the vessel surface area is too large. Finally, low enough contamination was achieved so that the total procedure blanks were below the instrumental detection limits for Cr and Ni. |
