Results of the IEA round Robin on viscosity and aging of fast pyrolysis bio-oils:long-term tests and repeatability

An international round robin study of the viscosity measurements and aging of fast pyrolysis bio-oil has been undertaken recently, and this work is an outgrowth from that effort. Two bio-oil samples were distributed to two laboratories for accelerated aging tests and to three laboratories of long-term aging studies. The accelerated aging test was defined as the change in viscosity of a sealed sample of bio-oil held for 24 h at 80 °C. The test was repeated 10 times over consecutive days to determine the intra-laboratory repeatability of the method. Other bio-oil samples were placed in storage at three temperatures, 21, 5, and -17 °C, for a period of up to 1 year to evaluate the change in viscosity. The variation in the results of the accelerated aging test was shown to be low within a given laboratory. The long-term aging studies showed that storage of a filtered bio-oil under refrigeration can minimize the amount of change in viscosity. The accelerated aging test gave a measure of change similar to that of 6-12 months of storage at room temperature for a filtered bio-oil. Filtration of solids was identified as a key contributor to improving the stability of the bio-oil as expressed by the viscosity based on results of the accelerated aging tests as well as long-term aging studies. Only the filtered bio-oil consistently gave useful results in the accelerated aging and long-term aging studies. The inconsistency suggests that better protocols need to be developed for sampling bio-oils. These results can be helpful in setting standards for use of bio-oil, which is just coming into the marketplace. © 2012 American Chemical Society.

Results of the IEA round robin on viscosity and stability of fast pyrolysis bio-oils

An international round robin study of the stability of fast pyrolysis bio-oil was undertaken. Fifteen laboratories in five different countries contributed. Two bio-oil samples were distributed to the laboratories for stability testing and further analysis. The stability test was defined in a method provided with the bio-oil samples. Viscosity measurement was a key input. The change in viscosity of a sealed sample of bio-oil held for 24 h at 80 °C was the defining element of stability. Subsequent analyses included ultimate analysis, density, moisture, ash, filterable solids, and TAN/pH determination, and gel permeation chromatography. The results showed that kinematic viscosity measurement was more generally conducted and more reproducibly performed versus dynamic viscosity measurement. The variation in the results of the stability test was great and a number of reasons for the variation were identified. The subsequent analyses proved to be at the level of reproducibility, as found in earlier round robins on bio-oil analysis. Clearly, the analyses were more straightforward and reproducible with a bio-oil sample low in filterable solids (0.2%), compared to one with a higher (2%) solids loading. These results can be helpful in setting standards for use of bio-oil, which is just coming into the marketplace. © 2012 American Chemical Society.

Editorial

Readers may have noted that a short but very important announcement was made in the last issue of CLAE, at the top of the contents page. CLAE has been accepted by Thomson Reuters for abstracting and indexing in its SciSearch, Journal Citation Reports, and Current Contents services. This will ensure a greater visibility to the international research community. In addition, in June 2012 CLAE will receive its very first official Impact Factor – a measure of journal influence of importance to authors and readers alike. The impact factor value has not yet been decided but internal estimates by Elsevier estimate it will be around 1, and it will be applied to all CLAE issue back to January 2009 (volume 32). I would guess readers at this stage would have one of two responses – either ‘that's good news’ or perhaps ‘what's an impact factor?’ If you are in the latter camp then allow me to try and explain. Basically the impact factor or citation index of a journal is based on how many times in the previous year papers published in that journal in the previous two years were cited by authors publishing in other journals. So the 2012 impact factor for CLAE is calculated on how many times in 2011 papers that were published in CLAE in 2010 and 2009 were cited in other journals in 2011, divided by the number of papers published in CLAE 2010 and 2009. Essentially authors will try and get their work published in journals with a higher impact factor as it is thought that the paper will be cited more by other authors or the paper will have higher visibility in the arena. For universities having its published output in higher journals is one of the markers used to judge esteem. For individual authors publishing in journals with a higher impact factor or the number of times one of their papers is published is something that they are likely to add to their CVs or demonstrate the importance of their work. Journals with higher impact factors tend to be more review journals or journals with a wider spectrum so for a relatively small journal with a specialised field like CLAE it is great to be listed with a citation index. The awarding of a citation index crowns many changes that CLAE has undergone since the current Editor took the reins in 2005. CLAE has increased from four issues (in 2004) to six issues per year with at least one review article per issue and one article with continuing education per issue. The rejection rate has gone up significantly meaning that only best papers are published (currently it stands at 37%). CLAE has been Medline/Pubmed indexed for a few years now which is also a very important factor in improving visibility of the journal. The submission and reviewing process for CLAE in now entirely online and finally the editorial board has changed from being merely a list of keynote people to being an active group of keynote people who are enthusiastically involved with the journal. From the editorial board one person is appointed as a Reviews Editor plus we have two additional editors who work as Regional Editors. As ever, on behalf of CLAE I would like to thank the BCLA Council for their continued support (especially Vivien Freeman) and Elsevier for their continuing guidance (in particular Andrew Miller and Rosie Davey) and the excellent Editorial Board (Christopher Snyder, Pauline Cho, Eric Papas, Jan Bergmanson, Roger Buckley, Patrick Caroline, Dwight Cavanagh, Robin Chalmers, Michael Doughty, Nathan Efron, Michel Guillon, Nizar Hirji, Meng Lin, Florence Malet, Philip Morgan, Deborah Sweeney, Brian Tighe, Eef van Der Worp, Barry Weissman, Mark Willcox, James Wolffsohn and Craig Woods). And finally, a big thanks to the authors and reviewers who work tirelessly putting manuscripts together for publication in CLAE. Copyright © 2012 Published by Elsevier Ltd.

An international round-robin calibration protocol for nanoindentation measurements

Nanoindentation has become a common technique for measuring the hardness and elastic-plastic properties of materials, including coatings and thin films. In recent years, different nanoindenter instruments have been commercialised and used for this purpose. Each instrument is equipped with its own analysis software for the derivation of the hardness and reduced Young's modulus from the raw data. These data are mostly analysed through the Oliver and Pharr method. In all cases, the calibration of compliance and area function is mandatory. The present work illustrates and describes a calibration procedure and an approach to raw data analysis carried out for six different nanoindentation instruments through several round-robin experiments. Three different indenters were used, Berkovich, cube corner, spherical, and three standardised reference samples were chosen, hard fused quartz, soft polycarbonate, and sapphire. It was clearly shown that the use of these common procedures consistently limited the hardness and reduced the Young's modulus data spread compared to the same measurements performed using instrument-specific procedures. The following recommendations for nanoindentation calibration must be followed: (a) use only sharp indenters, (b) set an upper cut-off value for the penetration depth below which measurements must be considered unreliable, (c) perform nanoindentation measurements with limited thermal drift, (d) ensure that the load-displacement curves are as smooth as possible, (e) perform stiffness measurements specific to each instrument/indenter couple, (f) use Fq and Sa as calibration reference samples for stiffness and area function determination, (g) use a function, rather than a single value, for the stiffness and (h) adopt a unique protocol and software for raw data analysis in order to limit the data spread related to the instruments (i.e. the level of drift or noise, defects of a given probe) and to make the H and E r data intercomparable. © 2011 Elsevier Ltd.