Conclusion (Lessons Learned + Future Works)
In conclusion, the team developed a gravity column chromatography method to purify crude LUV dye at a reduced cost. About 20 kg of silica 60 with less than 70 L of DCM is needed to purify 2 kg of LUV dye with a yield of ~70%.
From the project, the team was able to learn essential column chromatography techniques, such as basicification of silica column using ammonia hydroxide, as well as experimental design and trouble shooting methods. Although not mentioned in the experimental section, the team lost two weeks experimentation time due to the hydrophillic nature of silica gel used in the experiment. A great lesson learned by the team was to check the shelf life of any chemical compound before using it. In addition, the team also learned analytical techniques such as UV-Vis spectroscopy and analysis.
From this investigation, Kodak can expand on the results acquired by the team. One major future investigation that could be done by Kodak is to use different solvents to push the dye out of the column after all the Quat impurity adsorbs to the silica. While DCM was a good solvent for impurity separation, a large quantity of DCM is needed to achieve a 70% yield. Kodak should investigate other solvents to optimize the solvent cost as well as the yield. Another experiment that Kodak can do is to build isotherms to model the Quat concentration adsorbed in the bed. In addition, the red/orange/pink band separation is also worth study. The team believes that the red/orange band corresponds to two ions of the Quat impurity, while the pink band might be a colored amine compound that was not one of the major impurities. If that is the case, Kodak could conduct conductivity experiments of crude dye DCM solution (ideally Quat DCM solution) with varying concentrations to see if the two ions separate under natural pH with DCM only. Kodak can also do NMR on the compound of those bands.
Acknowledgments
The team would like to thank Kodak, especially, Brian Cleary, for providing the materials to perform the initial prototype tests and experiments. Furthermore, Kodak was an incredible resource for analytical testing, performing UV-Vis and GC-FID analysis on the purified samples collected from the column chromatography prototypes.
The team would also like to thank the project advisor Prof. Mark Juba, the laboratory staff, consisting of Rachel Monfredo, Clair Cunningham, and Jeffery Lefler, Prof. Melodie Lawton, and Prof. Doug Kelley, and the project teaching assistant Ryan Hayter for their support throughout the semester.
The feedback from all involved was invaluable and contributed to the success of the project. Thank you for all the help!
References
1DI-N-HEXYLAMINE | 143-16-8. Chemical Book, www.chemicalbook.com/ChemicalProductProperty_EN_CB5137002.htm.
2“[3-(Dihexylamino)Allylidene]Malononitrile SDS.” Look for Chemicals,
www.lookchem.com/sds61600-15-5.html.