• Analytical Science and Technology
• /
• v.26 no.1
• /
• pp.34-41
• /
• 2013

Split-flow thin cell (SPLITT) fractionation (SF) is a rapid separation technique capable of separating colloidal particles or macromolecules into two or more fractions. SF allows fractionations in a preparative scale as sample is fed continuously. Generally SF uses a thin ribbon-like channel equipped with two flow stream splitters at the inlet and outlet of the channel. Thus there exist two flow inlets and two flow outlets at the top and bottom of the inlet and outlet of the channel, respectively. There are two operating modes in SF, conventional mode and full-feed mode (FFD). Although the resolution in the FFD mode is lower than that in the conventional mode, FFD mode has some merits. The design of the channel and operation are simpler in the FFD mode, as it does not require the feeding of the solvent. Thus there is no flow stream splitter at the channel inlet, and only one pump is needed, unlike the conventional mode, where two pumps are required for the feedings of the sample and the solvent separately. Also the sample is not diluted in the FFD mode as there is no solvent feeding, which is important for fractionation samples with low colloidal concentrations such as environmental samples. For some of environmental samples, pre-concentration is often required. In this study, a new large-scale splitter-less FFD-SF channel was implemented, where there is no splitter at the outlet as well as at the inlet of the channel. It was possible to build the channel in a much larger dimension than conventional ones, allowing much higher sample throughput (TP). The new channel was tested and optimized with polyurethane (PU) latex beads, and then applied to large-scale separation of Polyacrylate (PA).

• Analytical Science and Technology
• /
• v.28 no.6
• /
• pp.453-459
• /
• 2015

Split-flow thin cell fractionation (SPLITT fractionation, SF) is a particle separation technique that allows continuous (and thus a preparative scale) separation into two subpopulations based on the particle size or the density. In SF, there are two basic performance parameters. One is the throughput (TP), which was defined as the amount of sample that can be processed in a unit time period. Another is the fractionation efficiency (FE), which was defined as the number % of particles that have the size predicted by theory. Full-feed depletion mode (FFD-SF) have only one inlet for the sample feed, and the channel is equipped with a flow stream splitter only at the outlet in SF mode. In conventional FFD-mode, it was difficult to extend channel due to splitter in channel. So, we use large scale splitter-less FFD-SF to increase TP from increase channel scale. In this study, a FFD-SF channel was developed for a large-scale fractionation, which has no flow stream splitters (‘splitter less’), and then was tested for optimum TP and FE by varying the sample concentration and the flow rates at the inlet and outlet of the channel. Polyurethane (PU) latex beads having two different size distribution (about 3~7 µm, and about 2~30 µm) were used for the test. The sample concentration was varied from 0.2 to 0.8% (wt/vol). The channel flow rate was varied from 70, 100, 120 and 160 mL/min. The fractionated particles were monitored by optical microscopy (OM). The sample recovery was determined by collecting the particles on a 0.1 µm membrane filter. Accumulation of relatively large micron sized particles in channel could be prevented by feeding carrier liquid. It was found that, in order to achieve effective TP, the concentration of sample should be at higher than 0.4%.

• Analytical Science and Technology
• /
• v.27 no.1
• /
• pp.34-40
• /
• 2014

SPLITT fractionation (SF) allows continuous (and thus a preparative scale) separation of micronsized particles into two size fractions ('fraction-a' and 'fraction-b'). SF is usually carried out in a thin rectangular channel with two inlets and two outlets, which is equipped with flow stream splitters at the inlet and the outlet of the channel, respectively. A new large scale splitter-less gravitational SF (GSF) system had been assembled, which was designed to eliminate the flow stream splitters and thus is operated by the full feed depletion (FFD) mode (FFD-GSF). In the FFD mode, there is only one inlet through which the sample is fed. There is no carrier liquid fed into the channel, and thus prevents the sample dilution. The effects of the sample-feeding flow rate, the channel thickness on the fractionation efficiency (FE, number % of particles that have the size predicted by theory) of FFD-GSF was investigated using industrial polyurethane (PU) latex beads. The carrier liquid was water containing 0.1% FL-70 (particle dispersing agent) and 0.02% sodium azide (used as bactericide). The sample loading rate was varied from about 4 to 7 L/hr with the sample concentration fixed at 0.01%. The GSF channel thickness was varied from 900 to $1300{\mu}m$. Particles exiting the GSF channel were collected and monitored by optical microscopy (OM). Sample recovery was monitored by collecting the fractionated particles on a $0.45{\mu}m$ membrane filter. It was found that FE of fraction-a was increased as the channel thickness increases, and FE of fraction-b was increased as the flow rate was increased. In all cases, the sample recovery has higher than 95%. It seems the new splitter-less FFD GSF system could become a useful tool for large scale separations of various types of micron-sized particles.

• Bulletin of the Korean Chemical Society
• /
• v.32 no.2
• /
• pp.681-686
• /
• 2011

SPLITT Fractionation (SF) provides separation of sample into two subpopulations. Separation into more than two subpopulations requires repeated SF operations. In this study, two Gravitation SF (GSF) channels were connected in a series (Tandem GSF) to obtain a separation into three subpopulations and to improve the fractionation efficiency (FE) of the fraction-b in the full-feed depletion (FFD) mode. In a single channel FFD-GSF operation, the fraction-a contained mostly the beads smaller than the cutoff diameter ($d_c$), while the fraction-b contained beads smaller than $d_c$ as well as those larger than dc, as expected. The measured FE's of the fraction-b are much lower than those of the fraction-a in all cases. The FE's of the fraction-a are higher than 84% with the average of about 91%, while those of the fraction-b are lower than 60% with the average of about 43%. No particular trends were found between FE and $d_c$, indicating the performance of FFD-GSF does not change with $d_c$ in the range where tested. Also no clear trends were observed between the FE and the sample-feeding flow rate, indicating higher sample-feeding rate can be used to increase the sample throughput without losing resolution. When two GSF channels were connected so that the flow stream emerging from the outlet-b of the channel-1 is fed directly into the channel-2, all three FE's measured for the fraction-1a were high with the average value of 99%, indicating it contains almost purely the beads smaller than $d_c$. The FE's measured for the fraction-2a are still good with the average value of 92%. The FE's measured for the fraction-2b are 64% in average, which is about 20% improvement from those obtained in a single channel FFD-GSF at the same conditions.