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Eng 2021, 2 611 2.2.2. Sub-Critical Fluid Extraction All sub-critical fluid extraction experiments were carried out using an Applied Sep- arations laboratory model Spe-ed Supercritical Fluid Extraction (SFE) unit with carbon dioxide as the extraction fluid. The extraction vessel, manufactured by Thar Designs Inc, was made of stainless steel and could be operated at a maximum pressure of 10,000 psi. The Spe-ed SFE unit used carbon dioxide as its operating fluid, which was supplied to the unit from a carbon dioxide cylinder outfitted with a dip tube to facilitate only liquid carbon dioxide to be supplied to the SFE unit. Additionally, a chiller was used to keep the liquid carbon dioxide cool as it entered the SFE unit. However, all experiments were carried out at temperatures and pressures below the critical point (72.9 bar pressure, 31 ◦C temperature), effectively using liquid carbon dioxide. The flow rate of carbon dioxide through the bed was 5 L per minute, which is equivalent to a superficial velocity of ≈1 L per minute per cm2 through the bed. 2.3. Analysis of Oil Samples The Agilent Technologies 6890 N gas chromatograph-mass spectrometer system was again used to analyse samples and standards. The column used for all the analyses was an Agilent HP5-ms 30 m capillary column with an internal diameter of 0.25 μm and an external diameter of 250 μm. This instrument was equipped with the National Institute for Standard and Technology (NIST) peer-reviewed and fully evaluated mass spectral library to identify unknown spectra. The library search report identified each component on the spectrum by its peak number, retention time (RT), area % (area under the peak), library name or ID, reference number, CAS number (Chemical Abstracts Service number—each number represents only one substance), and the quality. The essential oils obtained sub-critically were also quantified using ar-turmerone as an internal standard. It was the only essential oil of the six most abundant essential oils collected from the extractions that was available to be purchased as a pure standard. Consequently, the masses of each of the six essential oils were quantified relative to that of ar-turmerone. 2.4. Experimental Programme 2.4.1. Hydrodistillation Four hydrodistillation experiments were carried out whereby the preparation of the raw material turmeric was varied. In each case, 100 g of material was prepared, the first two experiments being on fresh turmeric (peeled and unpeeled) and the latter two on dried turmeric (peeled and unpeeled). Each experiment was run for 180 min, after which it was deemed that extraction had been completed. The essential oil was separated from the bulked distillate by virtue of their immiscibility, and the volume collected was measured in each case. All experiments were in duplicate. 2.4.2. Sub-Critical Fluid Extraction The critical point for carbon dioxide is at 72.9 bar pressure and 31 ◦C temperature (Mukhopadhyay [32]), so all experiments were carried out over ranges of values just below these figures, specifically 65 to 71 bar pressure and 25 to 30 ◦C temperature. Approximately 20 g of dried turmeric was charged to the extraction vessel for each experiment with the extract being collected every 5 min for mass and composition determination. All experi- ments were in duplicate. Since the objective of the work was to carry out a comparison of sub-critical fluid extraction with hydrodistillation, all experiments were carried out for a fixed time at the upper end of that which could reasonably be used commercially, 300 min. 3. Results 3.1. The Initial Drying Experiments The initial drying experiments to compare oven drying for 26 h at 55 ◦C and freeze drying were carried out on sub-critical extraction at 65 bar pressure and 25 ◦C for a periodPDF Image | Sub-Critical Fluid Extraction Turmeric vs Hydrodistillation
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