The authors wish to thank the analytical laboratory of the CanmetENERGY Technology Centre for its technical support, and Suncor Energy Inc. for supplying the synthetic crude oil. Partial funding for this study was provided by Natural Resources Canada and government of Canada&#39;s interdepartmental Program of Energy Research and Development (PERD) with project ID A22.015. Yi Zhang would like to acknowledge his Natural Sciences and Engineering Research Council (NSERC) of Canada Visiting Fellowship from January 2015 to January 2016.

<ol>
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J., Schaverien, C. J., Makkee, M., Moulijn, J. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cracking+of+a+rapeseed+vegetable+oil+under+realistic+FCC+conditions.">Cracking of a rapeseed vegetable oil under realistic FCC conditions.</a> Appl. Catal. B: Environ. 72 (1-2), 44-61 (2007).</li><li>Tian, H., Li, C., Yang, C., Shan, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Alternative+processing+technology+for+converting+vegetable+oils+and+animal+fats+to+clean+fuels+and+light+olefins.">Alternative processing technology for converting vegetable oils and animal fats to clean fuels and light olefins.</a> Chin J Chem Eng. 16 (3), 394-400 (2008).</li><li>Melero, J. A., Clavero, M. M., Calleja, G., Garcia, A., Miravalles, R., Galindo, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Production+of+bio-fuels+via+the+catalytic+cracking+of+mixtures+of+crude+vegetable+oils+and+nonedible+animal+fats+with+vacuum+gas+oil.">Production of bio-fuels via the catalytic cracking of mixtures of crude vegetable oils and nonedible animal fats with vacuum gas oil.</a> Energy Fuels. 24 (1), 707-717 (2010).</li><li>Bielansky, P., Reichhold, A., Sch&#246;nberger, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Catalytic+cracking+of+rapeseed+oil+to+high+octane+gasoline+and+olefins.">Catalytic cracking of rapeseed oil to high octane gasoline and olefins.</a> Chem Eng Process. 49 (8), 873-880 (2010).</li><li>Ng, S. H., Shi, Y., Ding, L., Chen, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Catalytic+cracking+of+a+rapeseed+oil+for+production+of+transportation+fuels+and+chemicals:+Yield+structure.">Catalytic cracking of a rapeseed oil for production of transportation fuels and chemicals: Yield structure.</a> 2010 AIChE Annual Meeting. , (2010).</li><li>Bielansky, P., Weinert, A., Sch&#246;nberger, C., Reichhold, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Catalytic+conversion+of+vegetable+oils+in+a+continuous+FCC+pilot+plant.">Catalytic conversion of vegetable oils in a continuous FCC pilot plant.</a> Fuel Process Technol. 92 (12), 2305-2311 (2011).</li><li>Ng, S. H., Lay, C., Bhatt, S., Freel, B., Graham, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Upgrading+of+biomass-derived+liquid+to+clean+fuels.">Upgrading of biomass-derived liquid to clean fuels.</a> 2012 AIChE Annual Meeting. , (2012).</li><li>Ordorica-Garcia, G., Croiset, E., Douglas, P., Elkamel, A., Gupta, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+the+energy+demands+and+greenhouse+gas+emissions+of+the+Canadian+oil+sands+industry.">Modeling the energy demands and greenhouse gas emissions of the Canadian oil sands industry.</a> Energy Fuels. 21 (4), 2098-2111 (2007).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Canada's Emission Trends. , (2013).</li><li>Kayser, J. 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H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=FCC+coprocessing+oil+sands+heavy+gas+oil+and+canola+oil.+1.+Yield+structure.">FCC coprocessing oil sands heavy gas oil and canola oil. 1. Yield structure.</a> Fuel. 156, 163-176 (2015).</li><li>Cox, J. D., Wagman, D. D., Medvedev, V. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> CODATA Key values for thermodynamics. , (1984).</li><li>Ng, S. H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=FCC+study+of+Canadian+oil-sands+derived+vacuum+gas+oils.+1.+Feed+and+catalyst+effects+on+yield+structure.">FCC study of Canadian oil-sands derived vacuum gas oils. 1. Feed and catalyst effects on yield structure.</a> Energy Fuels. 16 (5), 1196-1208 (2002).</li><li>Ng, S. H., Dabros, T., Humphries, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fluid+catalytic+cracking+quality+improvement+of+bitumen+after+paraffinic+froth+treatment.">Fluid catalytic cracking quality improvement of bitumen after paraffinic froth treatment.</a> Energy Fuels. 21 (3), 1432-1441 (2007).</li><li>Scherzer, J., Magee, J. S., Mitchell, M. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chapter+5,+Correlation+between+catalyst+formulation+and+catalytic+properties.">Chapter 5, Correlation between catalyst formulation and catalytic properties.</a> Fluid Catalytic Cracking: Science and Technology. , 145-182 (1993).</li><li>Fisher, I. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+feedstock+variability+on+catalytic+cracking+yields.">Effect of feedstock variability on catalytic cracking yields.</a> Appl. Catal. 65 (2), 189-210 (1990).</li><li>Ng, S. H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Study+of+Canadian+FCC+feeds+from+various+origins+and+treatments.+1.+Ranking+of+feedstocks+based+on+feed+quality+and+product+distribution.">Study of Canadian FCC feeds from various origins and treatments. 1. Ranking of feedstocks based on feed quality and product distribution.</a> Energy Fuels. 18 (1), 160-171 (2004).</li><li>Ng, S. H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Study+of+Canadian+FCC+feeds+from+various+origins+and+treatments.+2.+Some+specific+cracking+characteristics+and+comparisons+of+product+yields+and+qualities+between+a+riser+reactor+and+a+MAT+unit.">Study of Canadian FCC feeds from various origins and treatments. 2. Some specific cracking characteristics and comparisons of product yields and qualities between a riser reactor and a MAT unit.</a> Energy Fuels. 18 (1), 172-187 (2004).</li><li>Ng, S. H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Key+observations+from+a+comprehensive+FCC+study+on+Canadian+heavy+gas+oils+from+various+origins.+1.+Yield+profiles+in+batch+reactors.">Key observations from a comprehensive FCC study on Canadian heavy gas oils from various origins. 1. Yield profiles in batch reactors.</a> Fuel Process Technol. 87 (6), 475-485 (2006).</li><li>Scherzer, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Octane-enhancing+zeolitic+FCC+catalysts:++Scientific+and+technical+aspects.">Octane-enhancing zeolitic FCC catalysts: Scientific and technical aspects.</a> Catalysis Reviews: Science and Engineering. 31 (3), 215-354 (1989).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> ASTM D7964/D7964M-14 Standard test method for determining activity of fluid catalytic cracking (FCC) catalysts in a fluidized bed. , (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> ASTM D5154-10 Standard test method for determining activity and selectivity of fluid catalytic cracking (FCC) catalysts by Microactivity test. , (2010).</li><li>Moorehead, E. 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The authors declare that they have no competing financial interests.

The protocol described here utilizes cyclic operation of a single reactor containing a batch of fluidized catalyst particles to simulate feed oil cracking and catalyst regeneration. The oil to be cracked is preheated and fed from the top through an injector tube with its tip close to the bottom of the fluid bed. The vapor generated after catalytic cracking is condensed and collected in a receiver, and the liquid product collected is subsequently analyzed for simulated distillation to determine yields of fractions in different boiling ranges. The noncondensable gaseous product is sent to an on-line gas chromatograph for analysis to determine yields of dry gas and liquefied petroleum gas. The volume of the gaseous product is measured by the water displacement method. After suitable catalyst stripping time, the deposited coke on the catalyst is determined in situ by burning the deactivated catalyst in air at high temperatures (typically over 700 &#176;C). Levels of CO2 are measured quantitatively via an IR cell and are converted to coke yield. Any water formed is recovered and determined by Karl Fischer titration. The total recovery (mass balance) of the feed should be in the range of 96 to 102% prior to normalization of each product yield.
One benefit to this procedure is the use of the automated sequence carried out by the LTU during the reaction process. After initiating the test sequence in step 3.2.2, the system begins with system priming during which the LTU uses the preset conditions programmed prior to the run. If there is spent catalyst remaining in the reactor from previous runs, it is discharged into the waste vessel, and fresh catalyst from the specified hopper is loaded into the reactor. The system then waits a sufficient length of time to allow the temperatures of the reactor, feed line, syringe, and feed bottle to stabilize within 5 &#176;C of their set points. The syringe is then filled at a feed rate of 1.2 g/min for 20 sec (corresponding to two slop times), plus injection time, and the product line is purged with N2. The system then waits again, until the reactor internal and skin temperatures are within 2 &#176;C of their set points, and the coolant temperature is within 3 &#176;C of its set point. Finally, N2 flow to the IR gas analyzer is started and the system records the initial mass on the scale used to weigh displaced water and the pressure of the initial product gas (which should be zero).
Following priming, the syringe pump is set in motion and feed is first diverted back to the feed bottle for 10 sec (first slop time) followed by feed injection into the reactor for a preset time after switching back the three-way valve ahead of the syringe pump. Upon completion of injection, feed is diverted back again to the feed bottle for another 10 sec (second slop time). At the end of feed injection, counts begin for both liquid strip time and catalyst strip time. The former is chosen as 7 (liquid strip multiplier) times the feed injection time while the latter equals liquid strip time less 10 sec with a maximum 360 sec. The product flows are sent to the gas collection vessel through liquid receivers where high-boiling products are condensed.
Catalyst regeneration starts with valve switches at the end of the catalyst stripping cycle. Air flow begins and the reactor temperature is raised to ~715 &#176;C. The CO2 concentration is continuously monitored by the IR gas analyzer until it is below 0.3%. The air is turned off and the N2 flow to the reactor is re-established at the end of regeneration. The scale reading (mass of displaced water) is recorded along with pressure and temperature of the gas in collection vessel followed by gas mixing and warming (to ~30 &#176;C). At this stage, the liquid receiver for the run can be removed manually from the system for subsequent handling if desired. The line between the collection vessel and the GC is purged with product gas, and the loop is filled for the subsequent GC analysis. Cool the reactor until the skin temperatures are 50 &#176;C below their reaction set points and save all the data for the completed run. Return the unit to the first step of the test sequence for a new run, or discharge the spent catalyst to the waste vessel if it is the last run.
The established protocol proves successful in production of transportation fuels from canola oil in a blend. Good material balances (mass recoveries) are obtained in this study with a mean of 99.35% and a standard deviation of 0.31% from 18 LTU runs (Table 2). The conversions and yields from duplicate runs at 11.25 C/O ratio for each feed at a given temperature are quite reproducible (Table 2). Several typical FCC phenomena and cracking characteristics often reported in literature were also observed in this study: (1) Catalyst poisoning by feed basic nitrogen22-24, particularly pronounced for HGO at low temperatures (490 &#176;C in this work). The effect can be reduced at higher temperatures or C/O ratios; (2) Availability or exhaustion of crackable components in the feed and liquid product. Those in the feed are usually called &#34;gasoline precursors&#34;, defined as the sum of saturates and monoaromatics20,25-28; (3) Accessibility of catalyst acid sites to molecules; for example, incomplete decomposition of bulky triglyceride molecules at 490 &#176;C while their broken linear fatty acids can easily penetrate catalyst pores and be cracked6; (4) Oligomerization of olefins29 from fatty acids to form aromatics and coke; (5) Preferential skeletal isomerization of olefins to form branched compounds23,29.
The protocol is largely based on the LTU operating manual. The procedures in the manual must be strictly followed, except as noted. Critical steps within the protocol include preparation of equilibrium catalyst (must be on-size and coke-free); reactor preparation (using a feed line that yields a constant injector height, either 1.125 or 2.125 inch); CO2 analyzer calibration; preparation of the syringe (feed rate calibration) and liquid product receiver (weighing the long liquid receiver in a draft-free environment; maintenance of coolant temperature in -12 to -15 &#176;C range); system pressure test (to ensure a leak-free environment); choices of suitable catalyst strip time and liquid strip multiplier; analyses of gases (refinery gas analysis) and liquid product (simulated distillation by ASTM D288718); assignments of molecular weight 86 (versus 89 from ASTM D7964-1430) for C5+ unresolved lump, and carbon-to-coke factor 1.0695 (versus 1.083 from ASTM D7964, which assumes that one mole of hydrogen is associated with one mole of carbon in the coke).
One modification in the protocol that deviates from the LTU operating manual and ASTM D7964-1430 is that in the final step of weighing the liquid receiver, the stopper is quickly removed from and put back in the receiver to equalize the pressure before weighing. This allows release of excess N2, which is trapped at coolant temperature. However, it may also risk the chance of losing some gaseous product. Theoretically, this step may reduce the mass balance by 2.71 mass% for a run at a C/O ratio of 10 in our study, assuming that 149 ml N2 in the liquid receiver is trapped and expanding from -15 to 25 &#176;C at 93.5 kPa (701 mmHg) atmospheric pressure. The result agrees with experimental values (versus decreases in mass balance by 3.10 and 3.22 mass% for runs at C/O ratio of 10).
This protocol has also been extended to blends containing 50 and 100 v% canola oil in HGO. The high rapeseed oil concentration appears to be harmful to the system, requiring more frequent changes of the injector than normal, especially when pure canola oil is cracked. At low concentrations such as the one presented in this study, fouling did not occur.
In addition, the LTU cannot be applied to biomass pyrolysis oil containing emulsified water, which can evaporate at high temperatures for extended periods. In this case, an alternative test unit31 with a free but attachable syringe to deliver the feed is an option12. Also, the LTU cannot determine H2S yield quantitatively due to the water displacement method used to collect gaseous products of which H2S is partially dissolved in water. The alternative test unit modified to accommodate a gasometer consisting of two gas chambers (with pistons inside) in series was found to be satisfactory for this application22,23.
The protocol has also been employed for HGOs from paraffin-rich shale oils from oil shale and light tight oils (LTO) produced by hydraulic fracturing technology. For some of the runs using the said LTU, the simulated distillation results show significant amounts of dissolved gases in the liquid products due to the waxy nature of the feeds, resulting in overestimated gasoline yields and conversions. It is therefore recommended to crack the paraffinic feeds in the alternative test unit mentioned above, which includes a degassing step after condensation of liquid product in the receiver31. The said alternative test unit is widely used to characterize performance of FCC catalysts due to its relative simplicity, flexibility, versatility, and low cost. Over the years, the test method involved has been expanded to provide additional information such as product selectivities and qualities, and the operating variable and feedstock effects32. With adequate precaution on interpretation, test results can be used to assess commercial plant performance33.
Note that the above operational deficiencies using the LTU pertain to our existing particular model. As technology evolves, new products may overcome the problems discussed above.

There is strong global interest in both the private and public sectors to find efficient and economic means to produce transportation fuels from biomass-derived feedstocks. This interest is driven by a general concern over the substantial contribution of burning petroleum fossil fuels to greenhouse gas (GHG) emissions and its associated contribution to global warming. Also, there is strong political will in North America and Europe to displace foreign-produced petroleum with renewable domestic liquid fuels. In 2008, biofuels provided 1.8% of the world&#39;s transportation fuels1. In many developed countries, it is required that biofuels replace from 6% to 10% of petroleum fuels in the near future2. In Canada, regulations require an average renewable fuel content of 5% in gasoline starting December 15, 20103. The Renewable Energy Directive (RED) in Europe has also mandated a 10% renewable energy target for the European Union transport sector by 20204.
The challenge has been to develop and demonstrate a viable economic pathway to produce fungible transportation fuels from biomass. Biological sources include triglyceride-based biomass such as vegetable oils and animal fats, as well as waste cooking oil and cellulosic biomass such as wood chips, forest wastes, and agriculture residues. Over the past two decades, research has focused on the evaluation of biomass-derived oil processing using conventional fluid catalytic cracking (FCC)5-12, a technology responsible for producing most of the gasoline in a petroleum refinery. Our novel approach in this study is to co-process canola oil mixed with oil sands bitumen-derived feedstock. Normally, bitumen must be upgraded prior to refining, producing refinery feedstocks such as synthetic crude oil (SCO)&#8212;this processing route is particularly energy intensive, accounting for 68-78% of the GHG emissions from the SCO production13 and, in 2011, constituting 2.6% of Canada&#39;s total GHG emissions14. Replacing a portion of upgraded HGO with biofeed would reduce GHG emissions, since biofuel production involves a much smaller carbon footprint. Canola oil is chosen in this work because it is abundant in Canada and the US. This feedstock possesses a density and viscosity similar to those of HGOs while the contents of sulfur, nitrogen, and metals that could affect FCC performance or product quality are negligible. Moreover, this co-processing option offers significant technological and economic advantages as it would allow utilization of the existing refinery infrastructure and, hence, would require little additional hardware or modification of the refinery. In addition, there may be potential synergy that could result in product quality improvement when co-processing a highly aromatic bitumen feed with its straight-chain biomass counterpart. However, co-processing involves important technical challenges. These include the unique physical and chemical characteristics of bio-feeds: high oxygen content, paraffinic-rich composition, compatibility with petroleum feedstocks, fouling potential, etc.
This study provides a detailed protocol for the production of biofuels at laboratory scale from canola oil through catalytic cracking. A fully automated reaction system&#160;&#8211; referred to in this work as the laboratory test unit (LTU)15 &#8211; is used for this work. Figure 1 shows schematically how this unit operates. This LTU has become the industry standard for laboratory FCC studies. The objective of this study is to test the suitability of the LTU for cracking canola oil to produce fuels and chemicals with the goal of mitigating GHG emissions.
<img alt="Figure 1" src="/files/ftp_upload/54390/54390fig1.jpg" /> 
Figure 1: Conceptual illustration of the reactor. Illustration showing flow lines of the catalyst, feed, product, and diluent. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54390/54390fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

<table border="0" cellpadding="0" cellspacing="0" width="818">
	<tbody>
		<tr height="168">
			<td height="168" style="height:168px;width:231px;">Advanced Cracking Evaluation (ACE) Unit</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;">ACE R+ 46</td>
			<td dir="LTR" style="width:309px;">Assembled by Zeton Inc. SN:505-46;&#160; consisting of (1) a reactor; (2) catalyst addition system; (3) feed delivery system;&#160; (4) liquid collection system; (5) gas collection system; (6) gas analyzing system; (7) catalyst regeneration system; (8) CO catalytic convertor; (9) coke analyzing system</td>
		</tr>
		<tr height="126">
			<td height="126" style="height:126px;width:231px;">Reactor (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;">V-105</td>
			<td style="width:309px;">A 1.6 cm ID stainless steel tube having a tapered conical bottom and with a diluent (nitrogen) flowing from the bottom to fluidize the catalyst and also serve as the stripping gas at the end of the run</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Catalyst Addition System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Six hoppers (V-120F, with respective valves) for addition of catalyst for up to 6 runs</td>
		</tr>
		<tr height="126">
			<td height="126" style="height:126px;width:231px;">Feed Delivery System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Consisting of feed bottle (V-100), syringe (FS-115), pump (P-100), and injector (with 1.125 inch injector height, i.e., the distance from the lowest point of the conical reactor bottom to the bottom end of the feed injector)</td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:231px;">Liquid Collection System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Six liquid receivers (V-110F) immersed in a common coolant bath (Ethylene glycol/water mixture in 50:50 mass ratio) at about &#8211;15 &#176;C in a large tank (V-145)</td>
		</tr>
		<tr height="127">
			<td height="127" style="height:127px;width:231px;">Gas Collection System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Based on water displacement principle; consisting of gas collection vessel (V-150) with a motor-driven stirrer (MTR-100), and a weight scale (WT-100) for weighing the displaced water collected in a beaker (V100)&#160;</td>
		</tr>
		<tr height="101">
			<td height="101" style="height:101px;width:231px;">Gas Analyzing System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Key element being Agilent micro GC (model 3000A) with four capillary columns equipped with respective thermal conductivity detectors (TCDs)&#160;</td>
		</tr>
		<tr height="101">
			<td height="101" style="height:101px;width:231px;">Catalyst Regeneration System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;">V-105</td>
			<td style="width:309px;">Spent catalyst in reactor being burned in situ in air at +700 &#176;C to ensure complete removal of carbon deposited on the catalyst</td>
		</tr>
		<tr height="109">
			<td height="109" style="height:109px;width:231px;">CO Catalytic Convertor&#160; (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">A reactor (V-140) with CuO as catalyst to oxidize any CO and hydrocarbons in exhausted flue gas to CO2 (to be analyzed by IR gas analyzer) and H2O (to be absorbed by a dryer)</td>
		</tr>
		<tr height="46">
			<td height="46" style="height:46px;width:231px;">Coke Analyzing System (ACE)</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Servomex (Model 1440C) IR analyzer for measuring CO2 in exhausted flue gas</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">R+MM Software Suite</td>
			<td style="width:168px;">Kayser Technology Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Including iFIX 3.5&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Agilent Micro GC</td>
			<td style="width:168px;">Agilent Technologies</td>
			<td style="width:111px;">3000A</td>
			<td style="width:309px;">For gas analysis after cracking</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Cerity Networked Data System</td>
			<td style="width:168px;">Agilent Technologies</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Software for Agilent Micro GC</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:231px;">CO2 Gas Analyser</td>
			<td style="width:168px;">Servomex Inc.</td>
			<td style="width:111px;">1440C</td>
			<td style="width:309px;">SN: 01440C1C02/2900</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">NESLAB Refrigerated Bath</td>
			<td style="width:168px;">Themo Electron Corporation</td>
			<td style="width:111px;">RTE 740</td>
			<td style="width:309px;">SN: 104300061</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Orion&#160; Sage Syringe Pump</td>
			<td style="width:168px;">Themo Electron Corporation</td>
			<td style="width:111px;">M362</td>
			<td style="width:309px;">For delivering feed oil to injector tube</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Synthetic Crude Oil (SCO)&#160;</td>
			<td style="width:168px;">Suncor Energy Inc.</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Identified as Suncor OSA 10-4.1</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Catalyst P</td>
			<td style="width:168px;">Petro-Canada Refinery</td>
			<td style="width:111px;"></td>
			<td style="width:309px;">Equilibrium catalyst</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Balance</td>
			<td style="width:168px;">Mettler Toledo</td>
			<td style="width:111px;">AB304-S</td>
			<td style="width:309px;">For weighing liquid product receivers</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Balance</td>
			<td style="width:168px;">Mettler Toledo</td>
			<td style="width:111px;">XS8001S</td>
			<td style="width:309px;">For weighing water displaced by gas product</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Ethylene Glycol</td>
			<td style="width:168px;">Fisher Scientifc Inc.</td>
			<td style="width:111px;">CAS 107-21-1</td>
			<td style="width:309px;">Mixed with distilled water as coolant (50 v% )</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Drierite</td>
			<td style="width:168px;">W.A. Hammond Drierite Co. Ltd.</td>
			<td style="width:111px;">24001</td>
			<td style="width:309px;">For water absorption after CO catalytic converter</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:231px;">Copper Oxide</td>
			<td style="width:168px;">LECO Corporation</td>
			<td style="width:111px;">501-170</td>
			<td style="width:309px;">Catalyst for conversion of CO to CO2</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Toluene</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">CAS 108-88-3</td>
			<td style="width:309px;">For cleaning liquid receivers</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Acetone</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">CAS 67-64-1</td>
			<td style="width:309px;">For cleaning liquid receivers</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Micro GC Calibration Gas</td>
			<td style="width:168px;">Air Liquid Canada Inc.</td>
			<td style="width:111px;">SPG-25MX0015306</td>
			<td style="width:309px;">Multicomponent standard gas</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:231px;">19.8% CO2 Standard Gas</td>
			<td style="width:168px;">BOC Canada Ltd.</td>
			<td style="width:111px;">24069890</td>
			<td style="width:309px;">For calibration of IR analyzer</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Argon Gas</td>
			<td style="width:168px;">Linde Canada ltd.</td>
			<td style="width:111px;">24001306</td>
			<td style="width:309px;">Grade 5.0 Purity</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Helium Gas</td>
			<td style="width:168px;">Linde Canada ltd.</td>
			<td style="width:111px;">24001333</td>
			<td style="width:309px;">Grade 5.0 Purity</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-15</td>
			<td style="width:309px;">Channel A</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-03</td>
			<td style="width:309px;">Channel B</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-04</td>
			<td style="width:309px;">Channel C</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Gas analyzer GC Module</td>
			<td style="width:168px;">Inficon</td>
			<td style="width:111px;">GCMOD-73</td>
			<td style="width:309px;">Channel D</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">HP 6890 GC</td>
			<td style="width:168px;">Hewlett-Packard Co.&#160;</td>
			<td style="width:111px;">G1530A</td>
			<td style="width:309px;">For simulated distillation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">ASTM 2887 Standard Sample</td>
			<td style="width:168px;">PAC L.P.</td>
			<td style="width:111px;">26650.150</td>
			<td style="width:309px;">For quality control in simulated distillation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">ASTM 2887 Standard Sample</td>
			<td style="width:168px;">PAC L.P.</td>
			<td style="width:111px;">25950.200</td>
			<td style="width:309px;">For calibration in simulated distillation</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Column for GC 6890 (simulated distillation)</td>
			<td style="width:168px;">Agilent Technologies</td>
			<td style="width:111px;">CP7562</td>
			<td style="width:309px;">10m x 0.53mm x 1.2&#181;m, HP 6890 GC column</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Liquid Nitrogen</td>
			<td style="width:168px;">Air Liquid Canada Inc.</td>
			<td style="width:111px;">SPG-NIT1AC240LC</td>
			<td style="width:309px;">For use in simulated distillation&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Nitrogen</td>
			<td style="width:168px;">Air Liquid Canada Inc.</td>
			<td style="width:111px;">Bulk (building N2)</td>
			<td style="width:309px;">For use in ACE unit operation</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Isotemp Programmable Furnace</td>
			<td style="width:168px;">Thermo Fisher Scientifc Inc.</td>
			<td style="width:111px;">10-750-126</td>
			<td style="width:309px;">For calcination of catalyst</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">GC Vials, Crimp Top</td>
			<td style="width:168px;">Chromatograghic Specialties Inc</td>
			<td style="width:111px;">C223682C</td>
			<td style="width:309px;">2ml, for liquid product</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Seals, Crimp Top</td>
			<td style="width:168px;">Chromatograghic Specialties Inc</td>
			<td style="width:111px;">C221150</td>
			<td style="width:309px;">11 mm, for use with GC vials</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">4 oz clear Boston round bottles</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">02-911-784</td>
			<td style="width:309px;">With PE cone lined caps, for use in feed system</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Sieve</td>
			<td style="width:168px;">Endecotts Ltd.</td>
			<td style="width:111px;">6140269</td>
			<td style="width:309px;">Aperture 38 micron</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Sieve</td>
			<td style="width:168px;">Endecotts Ltd.</td>
			<td style="width:111px;">6146265</td>
			<td style="width:309px;">Aperture 250 micron</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">Shaker</td>
			<td style="width:168px;">Endecotts Ltd.</td>
			<td style="width:111px;">MIN 2737-11</td>
			<td style="width:309px;">Minor-Meinzer 2 Sieve Shaker for catalyst screening</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:231px;">V20 Volumetric KF Titrator</td>
			<td style="width:168px;">Mettler Toledo</td>
			<td style="width:111px;">5131025056</td>
			<td style="width:309px;">For water content analysis of the liquid product</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Hydranal Composite 5</td>
			<td style="width:168px;">Sigma-Aldrich</td>
			<td style="width:111px;">34805-1L-R</td>
			<td style="width:309px;">Reagent for Karl Fischer titration</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:231px;">Methanol (extremely low water grade)</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">A413-4</td>
			<td style="width:309px;">Mixed with toluene (40:60 w/w) for KF titration: also used to recover water in receiver</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:231px;">Glass Wool</td>
			<td style="width:168px;">Fisher Scientific Co.&#160;</td>
			<td style="width:111px;">11-388</td>
			<td style="width:309px;">Placed inside the top of receiver outlet arm&#160;</td>
		</tr>
	</tbody>
</table>

laboratory production of biofuels and biochemicals from a rapeseed oil through catalytic cracking conversion

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil (HGO) for production of transportation fuels through a fluid catalytic cracking (FCC) route. Cracking experiments are performed with a fully automated reaction unit at a fixed weight hourly space velocity (WHSV) of 8 hr-1, 490-530 &#176;C, and catalyst/oil ratios of 4-12 g/g. When a feed is in contact with catalyst in the fluid-bed reactor, cracking takes place generating gaseous, liquid, and solid products. The vapor produced is condensed and collected in a liquid receiver at -15 &#176;C. The non-condensable effluent is first directed to a vessel and is sent, after homogenization, to an on-line gas chromatograph (GC) for refinery gas analysis. The coke deposited on the catalyst is determined in situ by burning the spent catalyst in air at high temperatures. Levels of CO2 are measured quantitatively via an infrared (IR) cell, and are converted to coke yield. Liquid samples in the receivers are analyzed by GC for simulated distillation to determine the amounts in different boiling ranges, i.e., IBP-221 &#176;C (gasoline), 221-343 &#176;C (light cycle oil), and 343 &#176;C+ (heavy cycle oil). Cracking of a feed containing canola oil generates water, which appears at the bottom of a liquid receiver and on its inner wall. Recovery of water on the wall is achieved through washing with methanol followed by Karl Fischer titration for water content. Basic results reported include conversion (the portion of the feed converted to gas and liquid product with a boiling point below 221 &#176;C, coke, and water, if present) and yields of dry gas (H2-C2's, CO, and CO2), liquefied petroleum gas (C3-C4), gasoline, light cycle oil, heavy cycle oil, coke, and water, if present.

Watch this Scientific Journal Video about Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion at JoVE.com

Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion

This paper presents an experimental method to produce biofuels and biochemicals from canola oil mixed with a fossil-based feed in the presence of a catalyst at mild temperatures. Gaseous, liquid, and solid products from a reaction unit are quantified and characterized. Conversion and individual product yields are calculated and reported.

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil ...

laboratory-production-biofuels-biochemicals-from-rapeseed-oil-through

Nanyang Technological University

Research

JoVE Journal

Chemistry

13.7K Views.  Natural Resources Canada. This paper presents an experimental method to produce biofuels and biochemicals from canola oil mixed with a fossil-based feed in the presence of a catalyst at mild temperatures. Gaseous, liquid, and solid products from a reaction unit are quantified and characterized. Conversion and individual product yields are calculated and reported.

Video: Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

Thin-layer Chromatographic (TLC) Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungi or bacteria in broth or agar), allowing time for the microbes to grow in a humid environment, and visualizing zones with no microbial growth.&#160;The effectiveness of this screening method, known as bioautography, depends on both the quality of the chromatographic separation and the care taken with microbial culture conditions.&#160;This paper describes standard protocols for TLC and contact bioautography&#160;with a novel application to amino acid-fermenting bacteria. The extract is separated on flexible (aluminum-backed) silica TLC plates, and bands are visualized under ultraviolet (UV) light.&#160;Zones are cut out and incubated face down onto agar inoculated with the test microorganism.&#160;Inhibitory bands are visualized by staining the agar plates with tetrazolium red.&#160;The method is applied to the separation of red clover (Trifolium pratense cv. Kenland) phenolic compounds and their screening for activity against Clostridium sticklandii, a hyper ammonia-producing bacterium (HAB) that is native to the bovine rumen.&#160;The TLC methods apply to many types of plant extracts&#160;and other bacterial species (aerobic or anaerobic), as well as fungi, can be used as test organisms if culture conditions are modified to fit the growth requirements of the species.

Thin-layer Chromatographic TLC Separations and Bioassays of Plant Extracts to Identify Antimicrobial Compounds

Methods are described for thin-layer chromatographic (TLC) separation of plant extracts and contact bioautography to identify antibacterial metabolites. The methods are applied to the screening of red clover phenolic compounds inhibiting hyper&#160;ammonia-producing bacteria (HAB) native to the bovine rumen.

A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the ...

A Simple and Efficient Protocol for the Catalytic Insertion Polymerization of Functional Norbornenes

Norbornene can be polymerized by a variety of mechanisms, including insertion polymerization whereby the double bond is polymerized and the bicyclic nature of the monomer is conserved. The resulting polymer, polynorbornene, has a very high glass transition temperature, Tg, and interesting optical and electrical properties. However, the polymerization of functional norbornenes by this mechanism is complicated by the fact that the endo substituted norbornene monomer has, in general, a very low reactivity. Furthermore, the separation of the endo substituted monomer from the exo monomer is a tedious task. Here, we present a simple protocol for the polymerization of substituted norbornenes (endo:exo ca. 80:20) bearing either a carboxylic acid or a pendant double bond. The process does not require that both isomers be separated, and proceeds with low catalyst loadings (0.01 to 0.02 mol%). The polymer bearing pendant double bonds can be further transformed in high yield, to afford a polymer bearing pendant epoxy groups. These simple procedures can be applied to prepare polynorbornenes with a variety of functional groups, such as esters, alcohols, imides, double bonds, carboxylic acids, bromo-alkyls, aldehydes and anhydrides.

We describe the catalytic insertion polymerization of 5-norbornene-2-carboxylic acid and 5-vinyl-2-norbornene to form functional polymers with a very high glass transition temperature.

Norbornene can be polymerized by a variety of mechanisms, including insertion polymerization whereby the double bond is polymerized and the bicyclic ...

Characterizing Electron Transport through Living Biofilms

Here we demonstrate the method of electrochemical gating used to characterize electrical conductivity of electrode-grown microbial biofilms under physiologically relevant conditions.1 These measurements are performed on living biofilms in aqueous medium using source and drain electrodes patterned on a glass surface in a specialized configuration referred to as an interdigitated electrode (IDA) array. A biofilm is grown that extends across the gap connecting the source and drain. Potentials are applied to the electrodes (ES and ED) generating a source-drain current (ISD) through the biofilm between the electrodes. The dependency of electrical conductivity on gate potential (the average of the source and drain potentials, EG = [ED + ES]/2) is determined by systematically changing the gate potential and measuring the resulting source-drain current. The dependency of conductivity on gate potential provides mechanistic information about the extracellular electron transport process underlying the electrical conductivity of the specific biofilm under investigation. The electrochemical gating measurement method described here is based directly on that used by M. S. Wrighton2,3 and colleagues and R. W. Murray4,5,6 and colleagues in the 1980&#39;s to investigate thin film conductive polymers.

A protocol for measuring electrical conductivity of living microbial biofilms under physiologically relevant conditions is presented.

Here we demonstrate the method of electrochemical gating used to characterize electrical conductivity of electrode-grown microbial biofilms under ...

Palladium N-Heterocyclic Carbene Complexes: Synthesis from Benzimidazolium Salts and Catalytic Activity in Carbon-carbon Bond-forming Reactions

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from benzimidazolium salts. Detailed and generalized protocols are also presented for testing the catalytic activity of such complexes in arylation and Suzuki-Miyaura cross-coupling reactions. Representative results are shown for the catalytic activity of the four complexes in arylation and Suzuki-Miyaura type reactions. For each of the reactions investigated, at least one of the four complexes successfully catalyzed the reaction, qualifying them as promising candidates for catalysis of many carbon-carbon bond-forming reactions. The protocols presented are general enough to be adapted for the synthesis, purification and catalytic activity testing of new palladium N-heterocyclic carbene complexes.

Palladium N-Heterocyclic Carbene Complexes: Synthesis from Benzimidazolium Salts and Catalytic Activity in Carbon-carbon Bond-forming Reactions

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from benzimidazolium salts. The complexes were tested for catalytic activity in arylation and Suzuki-Miyaura reactions. For each reaction investigated, at least one of the four complexes successfully catalyzed the reaction.

Detailed and generalized protocols are presented for the synthesis and subsequent purification of four palladium N-heterocyclic carbene complexes from ...

From Molecules to Materials: Engineering New Ionic Liquid Crystals Through Halogen Bonding

Herein, we demonstrate that a bottom-up approach, based on halogen bonding (XB), can be successfully applied for the design of a new type of ionic liquid crystals (ILCs). Taking advantages of the high specificity of XB for haloperfluorocarbons and the ability of anions to act as XB-acceptors, we obtained supramolecular complexes based on 1-alkyl-3-methylimidazolium iodides and iodoperfluorocarbons, overcoming the well-known immiscibility between hydrocarbons (HCs) and perfluorocarbons (PFCs). The high directionality of the XB combined with the fluorophobic effect, allowed us to obtain enantiotropic liquid crystals where a rigid, non-aromatic, XB supramolecular anion acts as mesogenic core.
X-ray structure analysis of the complex between 1-ethyl-3-methylimidazolium iodide and iodoperfluorooctane showed the presence of a layered structure, which is a manifestation of the well-known tendency to segregation of perfluoroalkyl chains. This is consistent with the observation of smectic mesophases. Moreover, all the reported complexes melt below 100 &#176;C, and most are mesomorphic even at room temperature, despite that the starting materials were non-mesomorphic in nature.
The supramolecular strategy reported here provides new design principles for mesogen design allowing a totally new class of functional materials.

A protocol for the synthesis of a new type of mesogens, based on the halogen-bonded supramolecular anion [CnF2n+1-I&#183;&#183;&#183;I&#183;&#183;&#183;I-CnF2n+1]&#8722;, is reported.

Herein, we demonstrate that a bottom-up approach, based on halogen bonding (XB), can be successfully applied for the design of a new type of ionic liquid ...

One-pot Microwave-assisted Conversion of Anomeric Nitrate-esters to Trichloroacetimidates

The goal of the following procedure is to provide a demonstration of the one-pot conversion of a 2-azido-1-nitrate-ester to a trichloroacetimidate glycosyl donor. Following azido-nitration of a glycal, the product 2-azido-1-nitrate ester can be hydrolyzed under microwave-assisted irradiation. This transformation is usually achieved using strongly nucleophilic reagents and extended reaction times. Microwave irradiation induces hydrolysis, in the absence of reagents, with short reaction times. Following denitration, the intermediate anomeric alcohol is converted, in the same pot, to the corresponding 2-azido-1-trichloroacetimidate.

A 2-azido-1-nitrate-ester can be converted to the corresponding 2-azido-1-trichloroacetimidate in a one-pot procedure. The goal of the manuscript is to demonstrate utility of the microwave reactor in carbohydrate synthesis.

The goal of the following procedure is to provide a demonstration of the one-pot conversion of a 2-azido-1-nitrate-ester to a trichloroacetimidate ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Fabrication and Testing of Catalytic Aerogels Prepared Via Rapid Supercritical Extraction

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three preparation methods are described: (a) the incorporation of metal salts into silica or alumina wet gels using an impregnation method; (b) the incorporation of metal salts into alumina wet gels using a co-precursor method; and (c) the addition of metal nanoparticles directly into a silica aerogel precursor mixture. The methods utilize a hydraulic hot press, which allows for rapid (&#60;6 h) supercritical extraction and results in aerogels of low density (0.10 g/mL) and high surface area (200-800 m2/g). While the work presented here focuses on the use of copper salts and copper nanoparticles, the approach can be implemented using other metal salts and nanoparticles. A protocol for testing the three-way catalytic ability of these aerogels for automotive pollution mitigation is also presented. This technique uses custom-built equipment, the Union Catalytic Testbed (UCAT), in which a simulated exhaust mixture is passed over an aerogel sample at a controlled temperature and flow rate. The system is capable of measuring the ability of the catalytic aerogels, under both oxidizing and reducing conditions, to convert CO, NO and unburned hydrocarbons (HCs) to less harmful species (CO2, H2O and N2). Example catalytic results are presented for the aerogels described.

Here we present protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms. Methods for preparing materials using copper salts and copper-containing nanoparticles are featured. Catalytic testing protocols demonstrate the effectiveness of these aerogels for three-way catalysis applications.

Protocols for preparing and testing catalytic aerogels by incorporating metal species into silica and alumina aerogel platforms are presented. Three ...

Tuning the Acidity of Pt/ CNTs Catalysts for Hydrodeoxygenation of Diphenyl Ether

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid nanosheets, a series of Pt/xHMNO6/CNTs with different solid acid compositions (x = 5, 20 wt%; M = Nb, Ta; N = Mo, W) have been prepared by carbon nanotube pretreatment, protonic exchange, solid acid exfoliation, aggregation and finally Pt particles impregnation. The Pt/xHMNO6/CNTs are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and NH3-temperature programmed desorption. The study revealed that HNbWO6 nanosheets were attached on CNTs, with some edges of the nanosheets being bent in shape. The acid strength of the supported Pt catalysts increases in the following order: Pt/CNTs &#60; Pt/5HNbWO6/CNTs &#60; Pt/20HNbMoO6/CNTs &#60; Pt/20HNbWO6/CNTs &#60; Pt/20HTaWO6/CNTs. In addition, the catalytic hydroconversion of lignin-derived model compound: diphenyl ether using the synthesized Pt/20HNbWO6 catalyst has been investigated.

A protocol for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs is presented.

We herein present a method for the synthesis of HNbWO6, HNbMoO6, HTaWO6 solid acid nanosheet modified Pt/CNTs. By varying the weight of various solid acid ...