IIn order to develop the design of experiments we first developed fish bone diagram and based on that we developed a matrix of possible experiments using Taguchi design explained elsewhere [11].
The fish bone analysis turned out to be as follows:-
Following aspects have already been covered in research work done by earlier scientists:-
It had already been investigated activity followed the order; Co2(CO)8 > Co(NO3)2> Co(CH3COO)2 while chain growth probability followed the sequence Co(NO3)2 > Co2( CO)8 > Co(CH3COO)2 [6]. Based on these findings Co(NO3)2 was a preferred precursor salt. Salt concentration was based on the solubility in water (134 g/100ml) and ethanol (9g/100ml). Usually a base is used as the precipitation agent (by adjusting the pH of the system). Urea has been used earlier in different experiments because its hydrolysis is slow but rapidly precipitates [12].
Prior work has identified that surface properties of silica support, its interaction with the precursor solvent, and system pH have strong influence on the dispersion of catalyst. Ho et al [13] observed that when ethanol is used as the solvent instead of water for cobalt nitrate there is an increase of dispersion while retaining the high extent of reduction. They proposed that ethoxy (-OCH2CH3) group on the silica gel during the impregnation might hinder the aggregation of CO3O4 by physical interference during the thermal decomposition of cobalt nitrate as well as affects sintering process during reduction. It has also been reported that water as a solvent formed a glassy immobilized layer as a result of hydrogen bonding with silanol groups on the silica surface [14].
Drying rate was adjusted in order to ensure the stability ...
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...t even been added).
Experiment PrSl PrEv DrRt CalEv RdRt
1 -1 -1 -1 -1 -1
2 -1 -1 +1 -1 -1
3 -1 -1 -1 +1 -1
4 -1 -1 +1 -1 +1
5 -1 -1 +1 +1 -1
6 -1 +1 -1 -1 -1
7 -1 +1 -1 +1 -1
8 -1 +1 +1 -1 +1
9 -1 +1 +1 +1 +1
10 +1 +1 +1 -1 -1
11 +1 -1 -1 -1 +1
12 +1 -1 -1 +1 +1
13 +1 -1 +1 -1 -1
14 +1 -1 +1 +1 -1
15 +1 +1 -1 -1 +1
16 +1 +1 -1 +1 +1
17 +1 +1 +1 +1 -1
While selecting the final set of experiments we limited the scope of work to the effect of change in solvent and the change in precipitation/calcination environment (sample 2, 5, 10, 17). Our set of experiment reduced to four as shown in table 3. Such an arranged will step wise identify the impact of these factors on the final metal distribution.
Neidig, H. A., and J. N. Spencer. "Precipitating Lead Chromate on a Small Scale." General Chemistry For Engineering And Science. Mason: Cengage Learning, 2012. 83-90. Print. Signature Lab Ser.
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Michael P. Broadribb, C. (2006). Institution of Chemical Engineers . Retrieved July 26, 2010, from IChemE: http://cms.icheme.org/mainwebsite/resources/document/lpb192pg003.pdf
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The procedure for this experiment can be found in Inorganic Chemistry Lab Manual prepared by Dr. Virgil Payne.
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