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Crystallisation is a common method of separating solids from liquids in a solution.

The main method is to heat the solution and allow for the liquid to evaporate out,
then to filter out the remaining liquid from the solid crystals.
In the experiment a different route was taken. 2.5g Calcium Carbonate and 100ml of
water should be scaled out and added into a beaker with a magnetic stirrer, used to
create an ideal vortex to ensure mixing, and a hot plate used to get the solution to a
near boiling temperature, in order to help with the speed at which the solid would
dissolve into the liquid without or with as few solid particles floating around
undissolved. Some solid will remain on the outer edge of the beaker above the
water level so add water along the sides via the pipette until all the solid is in the
solution, this will bring the water level up to about 150ml.
Unlike other examples which mainly aim to separate the solid from the liquid in the
solution, this experiments priority is the formation and analysis of crystals and so
the top of the beaker will be covered to reduce (not prevent) liquid escaping as
vapour. After the solid had completely (mostly) dissolved the solution will be cooled,
while cooling the formation of crystals can be observed and once at a suitable
temperature the solution is dried via vacuum filtration to reduce the amount of
liquid in the crystallised solution. After the maximum amount of liquid, that could be
safely filtered so as not to damage the crystals with excessive force, is filtered the
crystallised solution will need to be further dried in an oven.
As crystallisation is the main focus the two experiments are done. The one
experiment is left to slowly cool down and the other is rapidly cooled in an ice bath.
After both experiments crystals are dried the results can be seen under a
microscope. A small spatula scoop from each experiment should be placed on a
microscope slide on a small amount of silicone oil so hold the crystals in place and
prevent crushing while the covering slide is placed on top.
Crystallisation is a process used often in industry especially in the pharmaceutical
industry since it is a useful as a purification and separation process for the isolation
and synthesis of pure active pharmaceutical ingredients (API) according to S.
Rohani (2010), meaning crystallisation is used to gain purer forms of medical
ingredients. Crystallisation can also be used to control the drug delivery to a site of
action and the drug release. In order to get the drug to react at the correct part of
the bodys directional tract the form that the drug takes and retakes is different
since the conditions of the environment that the drug takes changes vastly in
temperature, presence of fluid and pH. The drug needs to remain inactive and
unreactive until the site of activation. (Huddersfield University, Chemical
Engineering, Year 1: Pharmaceutics 2015-16)
The purpose of this paper is to describe some applications of particle size
analysis in the pharmaceutical industry.
Crystallisation is the process in which crystal like structures are obtained from
malts, vapours or solutions. These crystals can also be formed from molecules, ions
or even atoms by a collision between the particles leading to the formation of
clusters (). It is mainly used for determining the size and shape of particles,
parameters such as temperatures and cooling rate are some of the important
factors for this process.
Crystallisation (2014). (1st Ed.) Oxford University press.
The process of crystallisation or powders at present years have become more
important in order to analyse the shape and size of the particles to classify
themselves in terms of their physical and chemical properties. It has a wide range of
advantages when this process is carried out in industries especially in powder
industries, pharmaceutical industries for the production of medicinal drugs and so
on. A study was carried out using the process of crystallisation for the powder
calcium carbonate; it mainly focuses on analysing the particle behaviour from its
crystals formed and its applications in cement industries and for biomineralisation.
It states that crystals formed are stabilized by specific interactions between the
particles from its complex structures (Falini, G., et al, 2007).

Falini, G., Manara, S., Fermani, S., Roveri, N., Goisis, M., Manganelli, G., & Cassar, L. (2007).
Polymeric admixtures effects on calcium carbonate crystallization: Relevance to cement
industries and biomineralization. Crystengcomm, 9(12), 1162-1170. doi:10.1039/b707492a

Particle size analysis plays a major role in industries now days. Mainly in
pharmaceutical industries. It provides primary information for dosage properties of
drugs and its quality control treatment. Particle size analysis apparently has a lack
of interest in its applications probably because of its significantly high cost and
involvement of time for characterizing the size distribution for a particular fine
powder (Orr, N. A., & Spence,(1977).

Orr, N. A., & Spence, J. (1977). Applications of particle size analysis in the pharmaceutical
industry. The Analyst, 102(1215), 466-472. doi:10.1039/an9770200466

According to Kassel (2011),the characterisation of particle size is an analytical tool


in the pharmaceutical industry as it provides key information regarding the quality
specifications, safety and so on. The author states that at present years, the particle
size analysis is carried out using modern equipments which has made the
characterisation of particle size more quick and convenient. Such equipment involve
the Coulter counter, IS2 , Malvern mastersizer 2000 etc.

Kassel, J. (2011). Particle dispersion for size analysis. Journal of GXP Compliance, 15(3), 17.

This experiment was carried out using a calcium carbonate powder in which the
particle size was observed microscopically from the crystals obtained. Intermediate
process involved in this process was filtration to form crystals and normal
microscopy determine the length and width of individual crystals.
Errors observed in the generation of particle size data occur due to the selection of
a technique inappropriate to the material type or through the use of poor sampling
and dispersion techniques (i.e., sample preparation). In many cases, the end
application in which the particle size will be used is not properly considered, thus
the amount of dispersion needed is inadequate or overcompensated.

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