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The BIOREMA project—part 3: International interlaboratory comparison for bio-ethanol test methods

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Abstract

The main objective of the reference materials for biofuel specifications (BIOREMA) project is the development of two test materials (one bio-ethanol material and one biodiesel material) with well-established reference values. Of a series of three papers, this part describes the material preparation, homogeneity study, stability study, and characterisation of the bio-ethanol material. The test material thus obtained was used in an interlaboratory comparison (ILC) to assess current practices and comparability amongst laboratories providing bio-ethanol testing services. Only 13 participants provided data, resulting in a small dataset for evaluation. Further, it appeared that for a number of laboratories, there was not sufficient material for the determination of all requested parameters. In most cases, as far as the data permit, it can be concluded that the consensus values (based on participant’s results) are in good agreement with the reference or the BIOREMA values (obtained by NMIs participating in the project). For three parameters, namely ethanol content, water content, and density, there is good agreement between the reference and consensus values. For these parameters, the reproducibility standard deviation is close to, or even smaller than, the expanded uncertainty associated with the reference value. A number of parameters show very poor reproducibility, for example, pHe, electrolytic conductivity, and acidity. The same applies to sodium and copper content, which are very low and therefore challenging parameters to measure accurately. The results of the ILC underpin the need for certified reference materials and demonstrate the requirement for more robust quality control to improve the precision and trueness of the results from testing laboratories.

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References

  1. Baldan A, Ent H, van der Veen AMH, Held A, Ulberth-Buchgraber M, Daroda RJ, Da Cunha VS, Wise SA, Schantz M, Brewer PJ, Brown RJC, O’Connor G (2013) The BIOREMA project—part 1: Towards international comparability for biofuels analysis. Accred Qual Assur. doi:10.1007/s00769-012-0946-7 (this issue)

  2. Ulberth-Buchgraber M, Potalivo M, Held A, Baldan A, van der Veen AMH, Ent H, Cunha VS, Daroda RJ, Lang B, Schantz M, Hearn R, Brown RJC, Brewer PJ (2013) The BIOREMA project—part 2: International interlaboratory comparison for biodiesel test methods. Accred Qual Assur. doi:10.1007/s00769-012-0947-6 (this issue)

  3. European Committee for Standardization EN 15491:2007 (2007) Ethanol as a blending component for petrol. Determination of total acidity. Colour indicator titration method. Brussels

  4. Spitzer P, Fisicaro P, Seitz S, Champion R (2009) pH and electrolytic conductivity as parameters to characterise bioethanol. Accred Qual Assur 14:671–676

    Article  CAS  Google Scholar 

  5. International Organization for Standardization (2006) ISO guide 35—reference materials—general and statistical principles for certification, 3rd edn. ISO, Geneva

    Google Scholar 

  6. Lamberty A, Schimmel H, Pauwels J (1997) The study of the stability of reference materials by isochronous measurements. Fresenius J Anal Chem 360:359–361

    Article  Google Scholar 

  7. BIPM, IEC, IFCC, ISO, IUPAC, IUPAP, OIML (2008) Evaluation of measurement data—guide to the expression of uncertainty in measurement, 1st edn. GUM:1995 with minor corrections

  8. International Organization for Standardization (1994) ISO 5725-1:1994 accuracy (trueness and precision) of measurement methods and results—part 1: general principles and definition. Statistical methods for quality control, vol 2, pp 9–29

  9. International Organization for Standardization (1994) ISO 5725-2:1994 accuracy (trueness and precision) of measurement methods and results—part 2: basic method for the determination of repeatability and reproducibility of a standard measurement method. Statistical methods for quality control, vol 2, pp 30–74

  10. International Organization for Standardization (1998) ISO 15212-1—oscillation-type density meters—part 1: laboratory instruments. ISO, Geneva

    Google Scholar 

  11. International Organization for Standardization (2002) ISO 15212-2—oscillation-type density meters—part 2: process instruments for homogeneous liquids. ISO, Geneva

    Google Scholar 

  12. European Committee for Standardization (2008) EN 15837 ethanol as a blending component for petrol—determination of phosphorus, copper and sulfur content—inductively coupled plasma optical emission spectrometric direct method. Brussels

  13. European Committee for Standardization (2008) EN 15492 ethanol as a blending component for petrol—determination of inorganic chloride and sulfate content—ion chromatographic method. Brussels

  14. European Committee for Standardization (2008) EN 15692 ethanol as a blending component for petrol. Determination of water content. Karl Fischer potentiometric titration method. Brussels

  15. European Committee for Standardization (2008) EN 15721 ethanol as a blending component for petrol—determination of higher alcohols, methanol and volatile impurities—Gas chromatographic method. Brussels

  16. American Society for Testing and Materials (ASTM) (2009) ASTM D4052-09 standard test method for density, relative density, and API gravity of liquids by digital density meter. West Conshohocken, PA, USA

  17. European Committee for Standardization (2007) EN 15490 ethanol as a blending component for petrol—determination of pHe. Brussels

  18. American Society for Testing and Materials (ASTM) (2009) ASTM D5453-09 standard test method for determination of total sulfur in light hydrocarbons, spark ignition engine fuel, diesel engine fuel, and engine oil by ultraviolet fluorescence. West Conshohocken, PA, USA

  19. European Committee for Standardization (2008) EN 15486 ethanol as a blending component for petrol—determination of sulfur content—ultraviolet fluorescence method. Brussels

  20. European Committee for Standardization (2007) EN 15489 ethanol as a blending component for petrol. Determination of water content. Karl Fischer coulometric titration method. Brussels

  21. Brazilian Association For Technical Standards (ABNT) (2007) NBR 15531—Álcool etílico—Determinação do teor de água—Método volumétrico de Karl Fischer

  22. American Society for Testing and Materials (ASTM) (1992) ASTM D1744-92 standard test method for determination of water in liquid petroleum products by Karl Fischer reagent. West Conshohocken, PA, USA

  23. American Society for Testing and Materials (ASTM) (2008) ASTM E203-08 standard test method for water using volumetric Karl Fischer titration. West Conshohocken, PA, USA

  24. International Organization for Standardization (2000) ISO 12937: petroleum products—determination of water—coulometric Karl Fischer titration method. ISO, Geneva

  25. European Commission (2000) Commission Regulation (EC) No. 2870/2000 laying down community reference methods for the analysis of spirits drinks. Off J Eur Commun L333:22–45

    Google Scholar 

  26. American Society for Testing and Materials (ASTM) (2007) ASTM D6304-07 standard test method for determination of water in petroleum products, lubricating oils, and additives by coulometric Karl Fischer titration. West Conshohocken, PA, USA

  27. American Society for Testing and Materials (ASTM) (2008) ASTM E1064-08 standard test method for water in organic liquids by coulometric Karl Fischer titration. West Conshohocken, PA, USA

  28. American Society for Testing and Materials (ASTM) (2009) ASTM D1123-99 standard test methods for water in engine coolant concentrate by the Karl Fischer reagent method. West Conshohocken, PA, USA

  29. International Organisation for Legal Metrology (1975) OIML R22 international alcoholometric tables

  30. Brazilian Association for Technical Standards (ABNT) (2008) NBR 15639—Álcool etílico e suas misturas com água. Determinação da massa específica e do teor alcoólico-: Método da densimetria eletrônica

  31. American Society for Testing and Materials (ASTM) (2009) ASTM D5501-09 standard test method for determination of ethanol content of denatured fuel ethanol by gas chromatography. West Conshohocken, PA, USA

  32. Brazilian Association For Technical Standards (ABNT) (2006) NBR 9866—Álcool Etílico—Verificação da alcalinidade e determinação da acidez total

  33. Indian Bureau of Standards (2004) IS 15464 anhydrous ethanol for use in automotive fuel—specification

  34. American Society for Testing and Materials (ASTM) (2008) ASTM D6423-08 standard test method for determination of pHe of ethanol, denatured fuel ethanol, and fuel ethanol (Ed75–Ed85). West Conshohocken, PA, USA

  35. Brown RJC, Keates AC, Brewer PJ (2010) Sensitivities of a standard test method for the determination of the pHe of bioethanol and suggestions for improvement. Sensors 10:9982–9993. doi:10.3390/s101109982

    Article  CAS  Google Scholar 

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Correspondence to Adriaan M. H. van der Veen.

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Disclaimer: Certain commercial equipment, instruments, or materials are identified in this paper to specify adequately the experimental procedure. Such identification does not imply recommendation or endorsement by any of the project partners, nor does it imply that the materials or equipment identified are necessarily the best available for the purpose.

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van der Veen, A.M.H., Ent, H., Baldan, A. et al. The BIOREMA project—part 3: International interlaboratory comparison for bio-ethanol test methods. Accred Qual Assur 18, 41–50 (2013). https://doi.org/10.1007/s00769-012-0945-8

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