Particle Size and Shape Analysis Using Microscope

PRACTICAL 4 : PARTICLE SIZE ANALYSIS


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 different size of particles for each sample.

1. To analyse and interpret the shape of particles with five different samples. - See more at: http://pharmatechukm.blogspot.com/2013/12/report-on-particles-size-and-shape.html#sthash.jeSbMj1O.dpuf

To analyse and interpret the shape of particles with five different samples. - See more at: http://pharmatechukm.blogspot.com/2013/12/report-on-particles-size-and-shape.html#sthash.jeSbMj1O.dpuf

To analyse and interpret the shape of particles with five different samples. - See more at: http://pharmatechukm.blogspot.com/2013/12/report-on-particles-size-and-shape.html#sthash.jeSbMj1O.dpuf

INTRODUCTION :
         
              The dimensions of the 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 size 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 methods for particle analysis is using microscope.

MATERIALS AND APPARATUS :
Electron microscope,five different samples of sand particles.( 850,500,355,150 and various sizes) and Powders (MCC and lactose).

PROCEDURE :

              A microscope was used to analyse 5 different types of sands and powders (MCC and Lactose) with particular emphasis on the size and shape of the particles. The particles observed was sketched microscopically and the general shape for the particular material was determined. The magnification used in sketching the particle was noted.

Particles are being observed by using microscope.

RESULTS :

 150 mic (4x)

355 mic (4x)

500 mic (4x)

850 mic (4x)

Various Sizes (4x)

Lactose (4x)

MCC (4x)

QUESTIONS : 

1. Describe the variety of statistical method used to measure diameter of particles.

•     The particles that consists of spheres or equivalent spheres of same diameter is to be monosized but most powder contain particles that have different diameters. The size of distribution can be broken down into different size ranges as it can be presented in the form of a histogram and cumulative frequency form. The histogram method will expose to show the distribution of size particles in three types which are normal distribution , positively skewed distribution and bimodal distribution. The cumulative frequency is usually used for undersize and oversize.
• The mode and median diameters can be obtained for incomplete particle size distribution while mean can only be determined from complete size distribution and upper and lower limit is known.    

      2. What is the best method should be used in this experiment?

• The best method should be used is histogram method. Laser diffraction is the best statistical method to determine particle size distribution of lactose and MCC.

DISCUSSION :

The particle size and shape of sand particles and powders such as MCC and lactose were analysed and we found out that each of the particles have different and irregular shape which makes it difficult to be used directly in pharmaceutical industry. Therefore , particle size reduction method is needed in order to ensure all the particle are in the same size and shape. This will ensure that granulation plays a vital role in making of drugs and for a better absorption in the human body.

There were several precaution steps taken in this experiment such as the sand granules were carefully handled so that it will not spread all over the table and to ensure cleaniness of work place.
Besides that, gloves and goggles were weared for the safety of our eyes and hands.

CONCLUSION :

The shape and size of different samples were analysed and we can conclude that all particles have different and irregular shape and sizes.

REFERENCES :

1.  Michael E. Aulton, 2007, Aulton's Pharmaceutics The Design and Manufacture of Medicines, Third Edition, Churchill Livingstone Elsevier.
2.  Patrick J Sinko ,PhD, RPh, Martin's Physical Pharmacy and Pharmaceutical Sciences, 6th Edition, Lippincott Williams and Wilkins.

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. - See more at: http://pharmatechukm.blogspot.com/2013/12/report-on-particles-size-and-shape.html#sthash.jeSbMj1O.dpuf

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. - See more at: http://pharmatechukm.blogspot.com/2013/12/report-on-particles-size-and-shape.html#sthash.jeSbMj1O.dpuf

Phase Diagram for Ethanol/Toluene/Water system theory.

PRACTICAL 1 : PHASE DIAGRAM

PART A :

Determination of Phase Diagram for Ethanol/ Toluene/ Water System Theory

Three-Component Systems



OBJECTIVE :

1. To become familiar with certain rules that relate to the use of triangular coordinates to know the mutual solubility of liquids in a two phase system.\
2. Determination of the solubility limits in a ternary system of water and two other liquids (ethanol and toluene), one of which is completely miscible (ethanol) and the other is partly miscible with water (toluene).
3. Construction of the solubility curve of the system being studied on triangular diagram.

INTRODUCTION :

Figure 1: Ternary Phase Diagram

In the diagram above, each corner of the triangular diagram represents a pure component, which is 100% A, 100%B, 100%C. Meanwhile, each side represents two-component mixtures and within the triangular diagram itself represents ternary components. Any line parallel to a side of the triangular diagram shows constant percentage value for a component, for example: DE shows 20% of A with varying amounts of B and C. So does line FG, showing all mixtures containing 50% of B. These lines intercept with each other at K, which definitely contains 20%A, 50%B as well as 30%C. 

Measurements can be made this way because in a triangular diagram, the sum of all distances from K which is drawn parallel to the three sides of the diagram is same and equals to the length of any one side of the triangular diagram.

The addition of a third component to a pair of miscible liquids can change their mutual solubility. If this third component is more soluble in one of two different components the mutual solubility of the liquid pair is decreased. However, if it is soluble in both of the liquids, the mutual solubility is increased. Thus, when ethanol is added to a mixture of benzene and water, the mutual solubility of the liquid pair increased until it reached a point whereby the mixture becomes homogenous. This approach is used in the formulation of solutions.

APPARATUS:

Burette, conical flask, retort stand, measuring cylinder, test tubes

MATERIALS:

Ethanol, toluene, distilled water

PROCEDURES:

Each determination in this experiment is done twice. Mixtures of ethanol and toluene was prepared in a sealed container measuring 100cm3 containing the following percentage of ethanol (in percent) : 10,25,35,50,65,75,90 and 95. 20ml of each mixture was prepared by filling a certain volume using a burette(accurately). Each mixture was titrated with water until cloudiness was observed due to the existence of a second phase. A little water was added and after each addition it was shaken. The room temperature was measured. The percentage based on the volume of each component was calculated when the second phase starts to appear/separate. Points were plotted onto a triangular paper to give a triple phase diagram at the recorded temperature. 

RESULTS :

                                                           The cloudiness observed.

Test tube	A	B	C	D	E	F	G	H
First titration (ml)	1.7	0.7	1.0	1.5	2.7	3.9	10.1	15.3
Second titration (ml)	1.7	0.7	1.0	1.5	2.6	3.8	10.0	14.8
Average volume(ml )	1.70	0.70	0.95	1.50	2.65	3.85	10.05	15.05

Test tube	% Ethanol (v/v)	Total volume (average v + 20.0ml)	Ethanol		Toluene		Water
			Volume(ml)	Percentage volume(%)	Volume(ml)	Percentage volume(%)	Volume(ml)	Percentage volume(%)
A	10	21.70	2.00	9.22	18.00	82.95	1.70	7.83
B	25	20.70	5.00	24.15	15.00	72.46	0.70	3.39
C	35	20.95	7.00	33.41	13.00	62.05	0.95	4.54
D	50	21.50	10.00	46.51	10.00	46.51	1.50	6.98
E	65	22.65	13.00	57.40	7.00	30.91	2.65	11.69
F	75	23.85	15.00	62.89	5.00	20.96	3.85	16.15
G	90	30.05	18.00	59.90	2.00	6.66	10.05	33.44
H	95	35.05	19.00	54.21	1.00	2.85	15.05	42.94

TRIANGULAR DIAGRAM :

QUESTIONS :

1. Does the mixture containing 70% ethanol, 20% water and 10% toluene (volume) appear clear or  does it form two layers?
It appear as a clear solution.

2.What will happen if you dilute one part of the mixture with four parts of water, toluene, and ethanol?
 (a). Water                      : Two phase is formed.
 (b). Toluene                  : Two phase is formed.
 (c). Ethanol                  : The phase remains clear.

DISCUSSION :

Toluene is soluble in ethanol while it is not soluble with water. But, as these three component were mixed until certain proportion, all three components would be completely miscible. This experiment is carried out by first making a solution of ethanol and toluene which will be completely miscible and addition of water where at first it will make up two phase. As we continue to add more water until appropriate amount, it will result to one phase system.
 
Addition of water to the mixture of ethanol and toluene increases the mutual solubility of the liquid pair until at one point the mixture become homogenous. The region under the graph shows that there are two phase system form which consist of water and toluene since the solubility of water with toluene is weaker than that with ethanol. Meanwhile the region above the graph shows homogenous mixture. 

                                                The predicted graph for this experiment.

The are some error when conducting this experiment such as the cloudiness obtained is not correctly observed and the shaking of the test tube was too vigrous for some test tube until it affects the cloudiness of the solution. Some of the precaution taken in this experiment is that parallax error was avoided by placing the eye perpendicularly to the scale of the burette. Besides that , all the glassware was rinsed with water to remove impurities except conical flask as the presence of water before addition of chemicals will affect the experiment.

CONCLUSION :
Incomplete binomial curve was obtained from our experiment due to some errors while conducting this experiment.

REFERENCES :

1. Martin's Physical Pharmacy and Pharmacautical Science, Sixth Edition, Patrick J. Sinko,     Wolters Kluwer, Lippincott Williams & Wilkins.

2. "Ternary Phase Diagram" (http://www.sv.vt.edu/classes/MSE2094_NoteBook/96ClassProj/experimental/ternary2.html)

3.Aulton's Pharmaceutics The Design and Manufacture of Medicines, Fourth Edition, Michael E.Aulton, Kevin M.G. Taylor.