Further round-robin tests to improve the comparability between laboratories of the measurement of carbon in diesel soot and in environmental samples

Abstract

Objectives: An informal European coordination group organized two round-robin tests on filters collected from environmental, workplace and diluted diesel emissions. Previous inter-laboratory comparisons have shown that experimental samples give reasonably good results in terms of the dispersion around the mean, from all the participating laboratories. However, there were significant differences between the laboratories owing to a narrow distribution of the results within a single laboratory. In order to gain a better understanding of the differences obtained between the laboratories, it was decided to carry out more round-robin tests and to investigate further the possible factors which may influence the results. Methods: The first round-robin (RRT3) was performed on six different samples (eight replicates) analyzed by ten laboratories. The range of loading was 40 to 138 μg cm⁻² of total carbon (TC). Laboratories used their own thermal procedure parameters. The second round-robin test (RRT4) was performed on three different diluted diesel emissions (two replicates) samples analyzed by 13 laboratories. The range of loading was 21 to 37 μg cm⁻² TC. Laboratories analyzed samples using imposed temperatures (500, 650 and 800 °C) and imposed duration (12 min). Results: Inter-laboratory coefficients of variation for diluted diesel emission samples were 10% for RRT3 and ranged from 6 to 19% for RRT4. The influence of the desorption temperature was clearly demonstrated and the results tended to show that a desorption temperature of 650 °C could be an acceptable compromise. The influence of the organic carbon/elemental carbon (OC/EC) ratio was shown to be insignificant with pure diesel soot samples. Conclusions: It was expected that a significant improvement would be seen in the inter-laboratory dispersion by the use of a common standardized thermal desorption program, but the objectives of these RRTs were only partly reached. This paper provides new information that will be useful in the elaboration of a standardized procedure for the European Normalisation Centre (CEN TC 137 WG2 – General requirements for measuring procedures).