Thursday, 10 December 2015

Particle size and shape analysis using microscope

Objective
  • To analyse the particle shape and size under the microscope.
  • To describe the distribution particle size and shape.
Date of Experiment
19 November 2015

Introduction
The dimension of the particulate solids are very important in order to achieve optimum production of efficacious medicines .The particle size of drugs is determined when the drug is synthesized and formulated .In the case ,particle size will influence the subsequent physical performance of medicines and pharmacological of the drugs There are many methods for the analysis of particle size and shape .In this case , analysis using microscope is one of the effective ways to determine the particle size and shape .It is an excellent technique because we can look at the particle directly and is relatively cheap .One of the disadvantages of using microscope for analysis the shape and size of particle is the elaborate sample preparation is slow . Moreover, it is not suitable for quality control.

Apparatus 
Microscope, weighing boat

Materials
sand with particle size of (150 mic, 355 mic, 500 mic, 850mic), lactose, sand with various sizes and MCC.

Procedure
1.     Sands with sizes of (150 mic, 355 mic, 500 mic, 850mic), sand with various sizes, lactose and MCC are placed in the different weighing boat by using spatula. The weighing boat were labeled according to the content.
2.     The microscope was set up and ready to be use.
3.     150 mic sand scattered on the glass slide and covered with the cover slip.
4.     The sand was observed under the microscope using 4x10 magnification.
5.     The particles were observed microscopically and the shape was determined.
6.     Steps 3 to 5 were repeated by using (355 mic, 500 mic, 850mic), lactose ,sand with various sizes and MCC.
Results

Question
1.Explain in brief the various statistical method that u can use to measure the diameter of a particle.
The first method is the Feret’s diameter.The Feret diameter or Feret's diameter is a measure of an object size along a specified direction.  It can be defined as the distance between the two parallel planes restricting the object perpendicular to that direction generally. Therefore ,it is also called the caliper diameter, referring to the measurement of the object size with a caliper. This measure is used in the analysis of particle sizes, for example in microscopy, where it is applied to projections of a three-dimensional (3D) object on a 2D plane. In such cases, the Feret diameter is defined as the distance between two parallel tangential lines rather than planes.

Moreover ,Martin diameter can be one of the method to determine the diameter of a particle .It is a specific method for measuring the diameter of irregular shaped particles, Martin’s diameter is the measured distance between opposite sides of a particle, and is measured transverse to the particle on a line that bisects the projected area. In essence, Martin’s diameter measures the chord of a particle and is useful for estimating the surface area of an irregular non-spherical particle.

Besides ,projected area can be one of the methods to measure the diameter of a particle .The projected area diameter is the diameter of a sphere having the same projected area as the particle. Projected area is two-dimensional area measurement of a three-dimensional object by projecting its shape on to an arbitrary plane. Besides, another useful method is the projected perimeter diameter which is based on the circle having the same perimeter as the particle. Both of these methods are independent upon particle orientation. They only take into account of 2 dimensions of the particle, thus inaccurate for unsymmetrical particle.

Lastly ,we can use Fourier analysis to determine the diameter of a particle. It provides an accurate quantification of particle morphology and texture. They describe the overall shape of soil particles which is known as morphology . A summary of higher order descriptors provides textural information which is related to local roughness features which is defined as texture.

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

Martin's diameter and Feret's diameter of a particle depend on the particle orientation under which the measurement is made. Thus, obtaining a statistically significant measurement for these diameters requires a large number of randomly sampled particles which are measured in an arbitrarily fixed orientation. Since Martin's diameter, Feret's diameter, and projected area diameter are based on the two-dimensional image of the particles, they are generally used in optical and electron microscopy. 


 Discussion

Nowadays, pharmaceutical manufacture of products quality is more dependent on the particle size control as this is becoming increasingly apparent in the pharmaceutical industry. Precise particle size control technologies have also assisted in the development of drug delivery platforms for the delivery of a medicament to various part of the body.
In order to determine the particle size, several methods can be used such as microscopy, sieving, sedimentation techniques and etc. Besides, we can further analyze the particle size by using Feret’s diameter or Martin’s diameter. Martin’s diameter refers to the length of the line which bisects the particle image, while Feret’s diameter refers to the distance between two tangents on opposite sides of the particle, parallel to some fixed direction. This is because the Feret’s and Martin’s diameter is the best statistical method in which both of them use statistical diameter which are the average over many different orientations to produce a mean value for each particle 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.These two methods consider the orientation of particles, hence this increase the accuracy of the results obtained.
Microscope is used in this experiment to examine the various particle size and shapes of sands and powder because the microscope magnification are sufficient enough to allow adequate characterization of small particles. Error can be minimised if magnification and the light is sufficient that the image of particles produced is sharp and clear. Whereby, we can examine each particle individually by observing the 2D shape, colour, etc. However, we have to know that we unable to obtain a 3-Dimensional orientation of particle size and shape through a microscope.
In this experiment, we had analyze 5 different types of sands and powders (MCC, lactose, 150 mc, 355 mc, 500 mc, 850 mc, various size ) by using a microscope. The particles which are observed microscopically were sketched and the general shape for each particle were determined. We found that the samples that we observed are varies in term of their shape and size. They can be characterized by the range of from low sphericity to high sphericity, from very angular, angular, sub-angular, sub-rounded, rounded and well-rounded. For instance, the size of 850mc sand is larger than 150mc sand as we can compare of the image of sample we got in which both are irregular shape and asymmetry.
The magnification which we used during this experiment set to be constant for all 6 sample which is 4x10 magnification. This is important so that we can compare the size and shape of the particle clearly and easily. Besides, we have to make sure that the sample particles is well-spread throughout the slide and dispersed evenly until it is a thin layer before observing it under a microscope. It is to avoid the agglomeration formed and ensure the image of specimen we obtain is accurate and clear in term of their shape and size.
There were several precaution steps taken in this experiment such as make sure that the fan is switched off and the sand granules and powder were carefully handled so that it will not spread all over the table and to ensure cleanliness of work place. Moreover, we are advised to wear goggles and mask to prevent the sand and powder gets into our eyes and to protect ourselves safety.

Conclusion

As from the observation of the image obtained from microscope by using a fix magnification, we can conclude that the shape and size of the sands and powder are different. All particles are varies in their size and have an asymmetrical and irregular shape.  

References
1. Physicochemical Principals of Pharmacy (2nd Edition) AT Florence and D.Attwood, The Macmillan Press Ltd.
2. Michael E.Aulton, 2007, Aulton's Pharmaceutics The Design And Manufacture Of    Medicines, Third Edition, Churchill Livingstone Elsevier (page 122-134)
3. Pharmaceutics, The science of dosage form design (2nd Edition) Michael E.Alton Edinburgh London New York Philadophia St Louis Sydney Toronto 2002.


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