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rate. The system was run as a semi-batch system, with the reactor pre-charged with approximately 100 grams of a 1-wt.% solution of butanol. The system was run for 30-60 minutes at 1500 PSI, with the supercritical carbon dioxide flow rate being 1.26mL/min 3.2 mL/min, and 9mL/min. 3.1.2 Set Up Sample Jars The samples were collected in the Pyrex sample jars (ChemGlass) containing methanol by bubbling the exit stream at atmospheric pressure. The reactor fluid was bubbled through two sample jars that were connected in series to improve the overall mass balance of the extraction. A bubble diffuser (stainless steel frit) was put at the end of the tubes to optimize the bubbling of the reactor fluid into the methanol. Before the extraction began, the sample jars were prepared by weighing the empty vials with their lids. Then methanol was added to each set of vials. 100 grams of methanol was added to the first sample jar in each series while 50 grams of methanol was added to the second jar in each series. The optimal amount of methanol to put in the sample jars was determined through a trial and error process. Too much methanol caused the gas chromatography to be less accurate, while too little methanol did not allow for the butanol to cover the diffuser in the sample jar. Every 10 to 15 minutes the sample jars were switched with two new sample jars containing fresh methanol. This allowed us to track the amount of butanol extracted at different time increments throughout the extraction. System The system was prepared for a run by completing a set of steps. The chiller, which was set from 0oC to -6oC , was turned on and allowed to cool to the set temperature. This took about 45 minutes to an hour to complete. Meanwhile, the reactor was charged with the butanol-water solution and connected to the system. Then the first two sets of sample jars were connected and placed in an ice bath. The reactor-heating jacket and the heating strips were turned on, on the lines between the back-pressure regulator and the sample jars, to reach 40oC and 60oC respectively. The next step was to open the valves on the pressurized carbon dioxide tank. With the carbon dioxide inlet stream being cooled by the 30PDF Image | Extraction of Bio-Butanol using Supercritical Carbon Dioxide
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