Abstract
Crystallization of tetraethylammonium chlorochromate (C2H5)4N[CrO3Cl], TEACC, with desirable particle size as a performance characteristic was used to illustrate the design procedure. Taguchi design of experiments (DOE) method has been used for to plan a minimum number of experiments and optimization of crystallization processes. Four factors, which influence the crystal size, crystal growth and nucleation, were chosen. These factors are concentration, temperature, type of solvent and method of crystallization. After optimization the results show that concentration is most effective factor that has largest percent of contribution 53.26% and type of solvent is least effective factor that has smallest percent of contribution 4.33%. The optimum conditions are vapor diffusion as method, 0.043 g/15 mL for concentration, 0 °C for temperature and acetonitrile as solvent. These conditions must be produced suitable crystals for single crystal X-ray diffraction experiment. These results confirmed by experimental data and the crystals of the optimum conditions found to have suitable properties for single crystal X-ray diffraction. These crystals had sent for single crystal X-ray diffraction and diffraction data gathered successfully. A red block crystal was mounted on a glass fiber. The X-ray data determined monoclinic system, space group C2(#5), with a = 12.023(3), b = 7.998(2), c = 14.527(4) Å, β = 114.187(4)°, V = 1274.4(6) Å3 and Z = 4.
Index Abstract
The Taguchi design of experiments (DOE) method has been used for to plan a minimum number of experiments and optimization of crystallization processes.
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The authors would like to thank Dr. M. Hosseini and Dr. A. Asiabanha from Department of Geology, for their valuable helps and discussions.
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A number of papers about Taguchi method and its using in experimental design were found as supplementary material and by electronic search such as reference 13. MOESM1 (PDF 891 kb)
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Ghammamy, S., Baghy, M.R. Using of Taguchi Method for Experimental Design of Crystallization Processes of an Oxidant: Tetraethylammonium Chlorochromate (VI). J Chem Crystallogr 38, 907–912 (2008). https://doi.org/10.1007/s10870-008-9403-1
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DOI: https://doi.org/10.1007/s10870-008-9403-1