Thursday, 11 December 2014

PRACTICAL 1 : (E) PARTICLE SIZE AND SHAPE ANALYSIS USING MICROSCOPE

Title : Particle Size and Shape Analysis Using Microscope

Objective :
           1.      To analyse and interpret the shape of particles with five different samples
           2.   To observe and compare the size of particles for each sample.

Date of Experiment : 30 September 2014

Introduction :
The dimensions of particulate solids are important in achieving optimum production of efficacious medicines. When drug is synthesized and formulated, the particle size of drug and other powder is determined and this influences the subsequent physical performance of the medicine and the pharmacological of the drug.

Powder with different particle sizes have different flow and packaging properties, which alter the volumes of powder during each encapsulation or tablet compression event. The particles which are having small dimensions will tend to increase the rate of solution.


In order to obtain equivalent diameters with which to analyse and interpret the particle size of powder, it is necessary to carry out a size analysis using different methods. One of the method for particle analysis is using microscope. 

Material/Apparatus :
      1.      Electron Microscope

      2.      Five (5) different samples  (A=850mic, B=500mic, C=355mic, D=150mic,E=various size) 

Procedure : 

  1. 5 different types of samples were analysed by using microscope, by observing the size and shape of given particle.
  2. The samples were examined first by 4x10 magnification, followed by 10x10 magnification.
  3. The particle shape is sketched and the overall particle shape of that material is stated.

Result :


(Magnification: 10x for all observations)





Discussion : 

The ability to analyze and characterize particle size and shape can significantly improve the manufacturing efficiency and product performance. Thus, we can use of microscopy and image analysis as the most reliable technique to characterize particle shape, size and volume distribution. From this practical, it is found that the overall shape of the sand is asymmetrical. One of the methods used to measure a particle is the projected area diameter which is based on the equivalent area to that of projected image of the particle. Another method is the projected perimeter diameter which is based on the circle having the same perimeter as the particle. Both of the methods do not account the 3 dimensional shape of particle (orientation). They only consider the 2 dimensions of the particle, thus it is inaccurate for unsymmetrical particle.

            During the experiment, we put different types of sand on slide to be directly observed them using a light microscope. The sand should be spread evenly and just thin layer to avoid agglomeration that will affect the observation. We observed that the particles are irregular in shape. The size analysis is carried out on two-dimensional image of particles which are generally assumed to be randomly oriented in 3-dimensional and they are viewed in their most stable orientation.

            Feret’s and Martin’s diameter that considering the orientation of the particles is one of the methods to measure the diameter of particle. Feret’s diameter is the mean distance between two parallel tangents to the projected particle perimeter while Martin’s diameter is the mean chord length of the projected particle perimeter. The best statistical method is Feret’s and Martin’s diameter because both of them use statistical diameter which are the average over many different orientations to produce a mean value for each particle diameter. Besides, since it is accessing the three-dimensinal image of particle, we can use the electron microscope that considering the orientation and shape of the image.

Conclusion:


As a conclusion, each of the particles have different shape and they are irregular. The shape is not fix. The size of particles also various. This show that the granulation is important to ensure that flowability of drug can be achieved.

Question :


1.      Explain in brief the various statistical methods that you can use to measure the diameter of a particle.

Equivalent diameter
Symbol
Definition
Equation
Drag diameter (or frictional drag diameter)
dd
Diameter of a sphere having the same resistance to motion in a fluid as the particle in a fluid of the same density (ύf) and same viscosity (η), and moving at the same velocity (v) (ddapproximates to ds when the particle Reynolds number (Rep) is small and particle motion is streamlined. i.e. Rep < 0.2)
FD=CDAύfv22

where CD A = f(dd)
(i.e. FD = 3πddηv)
Feret’s diameter
dF
The mean value of the distance between pairs of parallel tangents to the projectedoutline of the particle. This can be considered as the boundary separating equal particle areas.
None
Free-falling diameter
df
Diameter of a sphere having the same density and same free-falling speed as the particle in a fluid of the same density and viscosity
None
Hydrodynamic diameter
dh
Diameter calculated from the diffusion coefficient according to the Stokes-Einstein equation
D=1.38×10−12T3πηdm2s−1
Martin’s diameter
dM
The mean chord length of the projected outline of the particle
None
Projected area diameter
da
Diameter of a circle having the same area (A) as the projected area of the particle resting in a stable position
A=π4da2
Perimeter diameter
dp
Diameter of a circle having the same perimeter as the projected outline of the particle
None
Sieve diameter
dA
The width of the minimum square aperture through which the particle will pass
None
Stokes diameter
dSt
The free-falling diameter (df, see above) of a particle in the laminar flow region (Rep < 0.2)
Under these conditions
dst2=dv3dd
Surface diameter
ds
Diameter of a sphere having the same external surface area (S) as the particle
S=πds2
Surface volume diameter
dsv
Diameter of a sphere having the same external surface area to volume ratio as the particle
dsv=dv3ds2
Volume diameter
dv
Diameter of a sphere having the same volume (V) as the particle
V=π6dv3




        




























































2.      State the best statistical method for each of the samples that you have analysed.

            Martin’s diameter and Feret’s diameter is the best statistical method to measure the diameter of particle.


Conclusion :
As a conclusion, each of the particles have different shape and they are irregular. The shape is not fix. The size of particles also various. This show that the granulation is important to ensure that flowability of drug can be achieved.

References :
       1.      Michael E.Aulton, 2007, Aulton's Pharmaceutics The Design And Manufacture Of    Medicines,
             Third Edition, Churchill Livingstone Elsevier (page 122-134)
       2.      http://www.horiba.com/fileadmin/uploads/Scientific/Documents/PSA/PSA_Guidebook.pdf

       3.      http://www.tcd.ie/CMA/misc/particle_size.pdf 



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