36 Environmental Laboratory


A typical example showing the results of analysing a sample of biochar by GC–MS to assess its purity. In this case, the compounds highlighted would be undesirable in the fi nal product because of their known toxici- ty; work carried out at EBRI aims to understand the pyrolysis conditions that lead to these contaminants, and minimise them. The analysis used a Frontier Lab EGA/PY-3030 double-shot analytical pyrolyser, close-cou- pled with a Shimadzu GCMS-QP2010 SE system.


To study this effect, he says, the researchers use the ‘pyroprobe’ setup to assess the thermal stability of small samples of biochar-modifi ed plastic pellets, to be sure that the product is going to be safe for the purpose.


Bioliquids as fuel additives and antifungal agents


Bioliquids are also a fruitful area of study, says Dr Chris Thomas, Knowledge Exchange Associate at EBRI, and another former Ph.D. student of Dr Nowakowski. “A particular interest at the moment is what we call the ‘catalytic upgrading’ of pyrolysis liquids. This involves taking the crude, water-immiscible pyrolysis oil and treating it with hydrogen under high pressure and temperature with a catalyst. That removes oxygen from the oxygen-containing compounds, giving us an upgraded pyrolysis liquid, which can then be distilled and combined with conventional biorefi nery streams for production of biofuels.


Left: Sachin Solomon (Knowledge Exchange Associate) uses the Shimadzu GCMS-QP2010 SE system with an AOC-20i autoinjector to carry out the GC– MS analysis of pyrolysis bioliquids. Right: Dr Christopher Thomas (Knowledge Exchange Associate) working with EBRI’s ‘simulated distillation’ system, consisting of a Shimadzu Nexis GC-2030 with SimDist software.


For this application, says Dr Thomas, the boiling-point distribution is of particular interest, but distillation doesn’t work well on small scales, and optimising the pyrolysis–upgrading process on a large scale would be expensive and time- consuming. So to predict the boiling-point properties quickly from smaller-scale experiments, he used one of the GC–FID systems at EBRI to obtain a chromatogram of the crude liquid, and then applied Shimadzu’s SimDist software tool to interpret the results.


Dr Thomas is keen to emphasise the benefi ts of this approach: “Directly from what are often very complex chromatograms, we can use this ‘simulated distillation’ method to help us understand at what temperature the different components in a mixture will boil off at. The resulting distillation curve shows us the proportion of each component that evaporates at different temperatures, which is crucial for checking the quality of biofuels and other bioliquid derived chemicals”.


Another application of bioliquids that Dr Nowakowski and colleagues are working on is so-called ‘wood vinegar’. This is a light-coloured aqueous liquid dominated by carboxylic acids, including acetic acid, formic acid and propionic acid, as well as some phenolics, and many other organic compounds about which little is known.


Dr Nowakowski explains: “These liquids have received a lot of hype as ‘natural’ antifungals and antibacterials, but there’s little information about exactly what they contain, let alone studies into their environmental and health impacts. So a focus for us at EBRI over the coming year or so will be using our HPLC and GC– MS instruments to understand these liquids in more detail”.


This research is vital, he adds. “Wood vinegar defi nitely has potential for treating mould and bacterial fi lms, but there’s a big issue around process and quality control. For example, if the pyrolysis temperatures are too high, the product can contain toxic aromatics, dioxins, and chlorine-containing chemicals. If you’re applying the wood vinegar to crops, they’ll end up in the environment, which is something you certainly don’t want”.


Diverse feedstocks, multiple processes


This is just a fl avour of the work that’s going on at EBRI, says Dr Nowakowski. Other projects involve looking at other sorts of waste, including chicken manure, municipal solid waste, used cooking oil, spent barley grains from beer production, bicycle tyres, offcuts of aluminium–plastic ‘thermal covers’ and cork, as well as a scoping exercise for carbon sequestration using farmed seaweed.


And it’s not all about pyrolysis, either. When the feedstock contains a lot of water that would be too energy-intensive


RESEARCHER BIOGRAPHY


Dr Daniel Nowakowski is a Lecturer in Chemical Engineering and Applied Chemistry at Aston University (Birmingham, UK), and Laboratory Manager of Aston’s Energy and Bioproducts Research Institute (EBRI). Following undergraduate studies in Chemical Technology in Gliwice (Poland), he completed his Ph.D. degree in Environmental Catalysis at the University of Leeds (UK) in 2007. The same year, he joined Aston University as a post-doctoral research assistant, and since 2012 he has held several senior fellowship posts. He has been an active researcher since 2007, and has been involved in a wide variety of research projects and collaborations relating to the processing, analysis and application of biomass and pyrolysis products.


A typical example showing the results of analysing a sample of biochar by GC–MS to assess its purity. In this case, the compounds highlighted would be undesirable in the fi nal product because of their known toxici- ty; work carried out at EBRI aims to understand the pyrolysis conditions that lead to these contaminants, and minimise them. The analysis used a Frontier Lab EGA/PY-3030 double-shot analytical pyrolyser, close-cou- pled with a Shimadzu GCMS-QP2010 SE system.


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to remove – such as algae – they can use a process called hydrothermal liquefaction. This involves catalytic treatment of a liquid slurry, with the result being a ‘biocrude’ similar to that obtained from pyrolysis of the solid material.


Biological processes such as anaerobic digestion and fermentation are also researched at EBRI, says Dr Nowakowski. “When a feedstock has very low calorifi c value but contains some good sugars, then we can get microorganisms to convert it to methane or ethanol, which can then be used as a fuel. The advantage of this approach is that the end product is usually quite refi ned, making the analysis a lot simpler”.


In summary, it seems that EBRI has a solution for every challenge: “Whatever the feedstock type, we can select and tailor the process to extract the maximum value from it!”, he says.


Expanding biowaste research –


with support from Shimadzu Through all of his work as a researcher and laboratory manager at EBRI, Shimadzu has been there for him, explains Dr Nowakowski. “Right from 2013 when we were setting up the new laboratories for bioenergy research here at EBRI, I’ve been able to benefi t from their expertise in analytical chemistry”, he says.


“They’ve always been ready to discuss our needs, and in many cases they’ve made a major contribution to the decision-making process. For example, in one project we needed to analyse permanent gases from our hydrothermal liquefaction unit, and they helped with setting up a GC–BID system – which signifi cantly improved our research outputs compared to the GC–FID system we’d originally been planning”.


This collaboration has continued to the present day, he adds, with guidance on getting the most out of the equipment, as well as routine maintenance and timely support. “With so many people booking our equipment, business continuity is very important for us – so it’s great that we always have a quick response from Shimadzu!”, he says.


And it’s clear that there’s no let-up in the pace of work at EBRI. Dr Nowakowski says that they’re still expanding their operations: “We’re increasingly focusing on applied research and novel processing methods, including biological processes for the production of value-added chemicals. We’re also becoming very strong in materials science, with emphasis on carbon materials derived from biochar. In addition, very recently EBRI started development of an integrated laboratory-scale centre to explore production of low-carbon hydrogen from biomass”.


“There’s so much going on – and it’s good to know that Shimadzu will be there for us, ready to help with anything I need!”, he concludes.


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