Two of the most commonly used solid biomass sources for fuel are wood chips and wood pellets. The calorific value and the moisture content of those biofuels determine the efficiency of the CHP and the biorefinery plants. Therefore, with the increased shift towards a biobased economy, the biomass cost and its physical properties must be precisely determined. Most of the current standards are lacking and provide neither enough details about the issues caused by the biomass heterogeneity nor with the variation in experimental practice. Phenomena such as data scattering, poor repeatability and wide uncertainty, are mostly observed during the measurements of the calorific value and the moisture content. To overcome such issues, an interlaboratory comparison between three national metrology institutes using bomb calorimetry has taken place. The comparison helped to identify the root causes behind the poor reproducibility of the wood samples. Factors such as the equilibrium moisture content of the biomass, the pellet mass, the applied pressure to form the pellet, the handling techniques and the determination errors are highlighted and analyzed. The final results paved the way to provide an enhanced detailed experimental practice where the repeatability and reproducibility have been strongly improved. Moreover, the detailed uncertainty sources and calculations are presented. It has been found that by fulfilling the recommended approach the measurement repeatability improved by up to 50–80%, while the final uncertainty improved by 10–30%. This enhancement leads to a maximum relative expanded uncertainty of around ±1% (coverage factor of k = 2 and a confidence level of 95%).
In this study, five laboratories, namely, BRML (Romania), TUBITAK UME (Turkey), IMBIH (Bosnia and Herzegovina), BAM (Germany), and DTI (Denmark), developed and validated analytical procedures by ICP-MS, ICP-OES, MWP-AES, WD-XRF, and ID-MS for the determination of inorganic impurities in solid and liquid biofuels, established the budget of uncertainties, and developed the method for determining the amount of ash in the measurement range 0–1.2% with absolute repeatability less than 0.1% and absolute reproducibility of 0.2% (according to EN ISO 18122). In order to create homogeneous certified reference materials, improved methodologies for the measurement and characterization of solid and liquid biofuels were developed. Thus, information regarding the precision, accuracy, and bias of the method, and identifying the factors that intervened in the measurement of uncertainty were experimentally determined, supplementing the information from the existing standards in the field.
Main text The COOMET project 744/RU-a/18 was organized for the purpose of determination of the degree of equivalence of the national standards for combustion energy measurement. Three coal samples with different values of sulfur content (AH - 1,192 %, AL - 0,193 %, LC - 0,412 %) were used in the comparison. Six laboratories participated between July 2019 and November 2020: VNIIM, Russia; NIM, China; BelGIM, Belarus; BRML-NIM, Romania; UME, Turkey; PTB, Germany. All the participants sent their measurement reports to the coordinator. The measurement results were provided with the detailed uncertainty budgets of the participants. The reference value was determined in accordance with CIPM MRA "Guidelines for organizing, participating and reporting" and COOMET R/GM/19:2016 "COOMET Recommendation Guideline on COOMET supplementary comparison evaluation". The degree of equivalence with the reference value was calculated for each sample and laboratory. The reported results were inconsistent, thus it was found necessary to process the data using the DerSimonian-Laird method. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCT, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
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