question: Using the data, discuss how the following factors affected the yield a
ID: 886312 • Letter: Q
Question
question:
Using the data, discuss how the following factors affected the yield and purity:
a. Hot filtration ( Part A vs. Part B Control)
b. Quantity of solvent ( Control vs. High Solvent Volume)
c. Rate of cooling ( Control vs. Rapid Cool)
Info:
Method Control Melting point (deg 108.6-111.2 114.5-118.1 118.0-120.5 116-118 117.9-119.5 115.8-120 116-118.6 122.9-125.0 120.0-122.4 108.4-118.1 111.7-114.7 100-102 118.3-120.1 112.3-117 114.6-116.2 120.6-122.2 96.2-102.0 112.1-117.3 118.9-125.2 112.2-115.3 119-121 115.2-117.1 113.9-119.2 118.6-123.2 116-120 116.2-118.4 117.6-119.4 121.8-124.0 115-119.4 119.2-121.9 119.8-121.9 117.9-120.5 120.6-124.6 92.0-98.9 115.4-117.8 117.2-119.6 115.8-117 116.1-118.7 % recovery (%) 82 96.5 99.5 98 90.4 64.7 83 99.97 77.84 85.6 96 127 106.9 Average mp = 115 .5degC Average % 96.5 118.4 69.48 113.5 84.86 90.00 128.1 15.1 49.5 71.81 89.89 73 56.5 89.07 98.78 65.78 68.6 36.6 97.03 98.23 118.3 124.4 78 62 73.7 Large volume Average mp = 119·0degC Average 65.0 Average 96-65.0 Quick cool Average mp 116.0 Average % = 92.7Explanation / Answer
Hot filteration:There are in soluble impurities remaining in the solution, and thereare coloured impurities may present in the solution by perfoming hot filteration we can remove insoluble, coloured impurities such that we can improve the purity of the compound.
Soluble impurities removed by suction filteration. insoluble impurities are removed by hot gravity filteration.
A minimum amount of solvent will minimize the amount of desired compound that remains dissolved in the solvent and must be thrown away.
Quntity of solvent:
solvents to extract Compounds on a large scale will tell you that the solvents are expensive. Not only is it cost-effective to recover and reuse the solvents, it is wise to use only as much solvent as is necessary, and not more. Using excess solvent lengthens the purge time and reduces the capacity of your equipment.
Of course, it is also true that the more solvent you use the higher your total yield. So, a balance must be struck between using more solvent to improve yield, and using less solvent to increase productivity. On both ends of this spectrum are diminishing returns, and the cost-benefit analysis is dependent on where priorities are placed.
What many may not realize is that the solvent-to-substrate ratio has implications not only to productivity and yield, but also to purity of final producctivity.
What these data indicate is that the more solvent you use the more material you capture, but the lower purity of final product. As solvent quantity increases, the amount of compound capture depreciates faster than does the amount of impurity capture.
By no means is this an argument in favor of using less solvent. There is certainly an argument for higher yield even if it sacrifices potency a little. It’s a balancing act.
CONTROLLED COOLING VS RAPID COOLING:I
iN CONTROLLED COOLING METHOD at initial stage very little crystals are formed the yield for the controlled coling method increased gradually.
Rapid cooling of the rate of cooling are very interesting. When a solution is cooled fast, the solids all come out of solution all at once.
A fast cooling rate during the early stage of cooling modes produced a large number of small nuclei. we noted that rapid crystallization produced much smaller crystal compared to slow crystallization. As the solvent percentage increases, for rapid crystallization moving towards the larger particle. As noted before from the slow crystallization , at higher solvent percentage, crystals become smaller. on the particle size. Generally, particles in smaller size fractions create higher agglomeration degree. The higher the usage of solvent, the smaller will be the particle size and the tendency to create CRYSTALS also increased.
Rapid crystallization creates much smaller particle size compared to slow crystallization.
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