Friday, December 12, 2014

Practical 3 : Sieving

PART A

Title : Sieving

Objectives

   1. To determine the size and size distribution of a particular powder.

   2. To classify and differentiate the powders based on their diameter.

Date of Experiment : 20 November 2014

Introduction

Sieving  are most frequently used to break down agglomerates and determine the size and size distribution of a particular powder. In this experiment, sieve nest was used to determine the particle size and the size distribution of both powders. 

                       sieve nest

Procedure



1. 100g of lactose was weighed.



2. The sieve nest was prepared in descending order, from the largest to the smallest diameter, from 
     top to bottom.

3. The lactose powder was placed at the uppermost sieve and allow the sieving process to proceed
     for 10minutes.

4. When the sieving process already completed, the powder in each sieve was collected and weighed.   A particle size distribution histogram was plotted.

5. The process was repeated by using MCC. 

                                 MCC powder

Result
   



Discussion

                Sieving is a method used to assess the particle size distribution of a granular  material or powders. Sieving can be performed on any  type of organic or non-organic granular materials and for this experiment, we were using lactose and MCC powders. At the beginning of this experiment,  100g of lactose and MCC was poured into the sieve nest and undergo sieving process for 10 minutes.
After the process finished, the weight of lactose and MCC are 99.88g and 98.90g respectively.  The weight for both powders after the sieving process finished is slightly less than the initial weight. From this result, it shows that there is a loss of powders during the sieving process. This loss is due to some of the powders particles are still stuck in the woven sieve cloth.       

Based on the histogram, the highest amount of lactose powders collected at the sieve with the range of 200≤x<300mm, which is 53.56% of the lactose. Followed by 24.08% of lactose at sieve within the range of 150≤x<200mm and lastly at the range of 50≤x<150mm with 22.01% of lactose powders. However  for MCC powders, the highest amount of these powders were remained at the sieve range less than 50mm which consist of 58.63% of the MCC powders and followed by 34.00% of MCC powders at sieve with range 50≤x<150mm. There is a different between the result due to differences in physical properties of both powders.


Questions


1.What are the average particle size for both lactose and MCC?

   The average particle size for both lactose and MCC are 45µm and then followed by <50µm, between 50 – 150 µm, between 150 – 300 µm, between 300 – 425 µm and lastly >500µm.

2.What other methods can you use to determine the size of particle?

  Other methods that can be used to determine the size of particle are laser light scattering or LD technique, microscope method, sediment method and electron zone sensing method (coulter counter).

3.What are the importance of particle size in a pharmaceutical formulation?


   The important physical characteristic of material used in order to create pharmaceutical products is  particle size distribution of active ingredients and excipients. Bulk properties, product performance,  processability, stability and appearance of the end product is affected by the size, distribution and  shape of the particles. Particle size and product influence are closely linked to dissolution,  absorption rates and content uniformity so it can achieve optimum production of 

   efficacious medicines especially in pharmaceutic phase.

Conclusion

   Sieveing is one the process to determine the size of a particle. The particle size is quite important in pharmaceutical industry. Hence,  the distribution size of a particle can be analysed after conducting this experiment. 

Wednesday, December 10, 2014

Practical 3 : Phase Diagram


PART A


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

Objectives                  
1.      To understand the concept of phase diagram.
2.      To determine the phase diagram for ethanol, toluene and water system theory.

Date of experiment        :  4 November 2014

Introduction   
                       
Phase diagrams are graphical representations of the liquid, vapour, and solid phases that co-exist at various ranges of temperature and pressure within a reservoir. Ternary phase diagrams represent the phase behaviour of mixtures containing three components in a triangular diagram, hence it is also known as three component systems. For three component systems at constant temperature and pressure, the compositions may be stated in the form of coordinates for a triangular diagram.



In the diagram, each corner of the triangular diagram represents a pure component A, B and C respectively which all are 100 per cent pure. Meanwhile, each side of the triangle 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 instance, line DE shows 20% of A with varying amounts of B and C, line FG, showing all mixtures containing 50% of B. The interception point, K 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 mutual solubility of two miscible liquids can be altered when a third component is added into them. If this third component is more soluble in one of the two different components the mutual solubility of the liquid pair is decreased. On the other hand, if it is soluble in both of the liquids, the mutual solubility is increased. 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. Examples of three-component systems that have been studied include castor oil, alcohol, water; peppermint oil, propylene glycol, water; peppermint oil, polyethylene glycol, water.
 In this system, there are 3 components but only 1 phase exists. Thus, by using the phase rule, it is determine that this system have 4 degrees of freedom which are temperature, pressure, and any two from the three component concentration.
Calculation for degree of freedom:
F = C – P + 2
F = 3 – 1 + 2
F = 4

Material and Apparatus
                
Burette and Retort Stand

Toluene

Sulphuric Acid

Distilled Water
Measuring Cylinder

 100 cm3 Conical Flask



Experimental Procedures                 

      1.      Mixtures of ethanol and toluene are prepared in sealed containers measuring 100cm3 containing the following percentages as well as volume of ethanol and toluene.

Container
Ethanol
Toluene
Percentage (%)
Volume (ml)
Percentage (%)
Volume (ml)
A
10
2
90
18
B
25
5
75
15
C
35
7
65
13
D
50
10
50
10
E
65
13
35
7
F
75
15
25
5
G
90
18
10
2
H
95
19
5
1
         




      2.      Each mixture is titrated with water until cloudiness is observed due to the existence of a second phase by using a burette.    
  
         

      3.      A little water is added and shaken well after each addition.
      4.      The room temperature is measured.
      5.      The percentage is calculated based on the volume of each component when the second phase starts to appear.
    6.      The points are plot onto a triangular paper to give a triple phase diagram at the recorded temperature.


Result         
                     
Containers
Volume of water added (ml)
A
0.0
B
0.2
C
1.2
D
1.6
E
2.7
F
4.2
G
10.4
H
16.1
   
Containers
Percentages (%)
Ethanol
Toluene
Water
A
10.00
90.00
0.00
B
24.75
74.26
0.99
C
33.02
61.32
5.66
D
46.30
46.30
7.40
E
57.27
30.84
11.89
F
61.98
20.66
17.36
G
59.21
6.58
34.21
H
52.63
2.77
44.60



Discussion 
    
In ternary phase diagrams, the solubility of two liquid can be changed when a third component is added. There are two possible outcomes. First, if the third component is soluble in both the liquid, it may increase the solubility of the system. Hence, it can be used to mix two immiscible or slightly immiscible components such as water and benzene. Initially, water and benzene appear in two phase but once alcohol is added into the system, the final solution contains only one phase. Secondly, the other possible outcome is if the third component added is only soluble in one of the two different components, the solubility of the system will be decreased.

In this experiment, we used ethanol, toluene, and water. Water is used as the third component. As we know, toluene is soluble in alcohol; hence toluene is miscible in ethanol. On the other hand, toluene is insoluble in water while ethanol is soluble in water. As a result, the solubility of the system will decrease as water added into the mixture of toluene and ethanol. Cloudiness which indicates the existence of two phases is observed in the end of the experiment.

In the triangular paper, the top corner of the triangle is labelled as toluene, the left corner is ethanol while the right corner is water. Each corner represents 100% pure of the three components respectively. Any points on the sides of the triangle show that there are only two components while the points within the triangle show that there are three components in the mixtures.

Based on the triangular paper, a curve can be drawn when all the points on the paper are joined together. The curve separated the triangular paper into two sides, left and right. On the left side of the curve, the mixtures appear to have only one phase. Meanwhile, on the right side of the curve, the mixtures appear to have two phases and cloudiness can be observed.

There are several errors that were formed when conducting this experiment which leads to this inaccuracy .They includes:
  • Exact point when to stop water titration is determined wrongly as the cloudiness disappearance was not observed properly.
  • The eye level of the observer was not perpendicular to the reading scales
  • Different rate of agitation may influence the disappearance of cloudiness.
  • The apparatus used were not clean completely before the experiment was started.
  • The temperature during the experiment is not consistent.
To improve the accuracy of the result of experiment, some precautions must be taken. They include:
  •   The eye level of the observer must be perpendicular to the reading skills to avoid parallax errors.
  •  Use consistent rate of agitation for each mixture.
  • Clean the apparatus before using it. This is to ensure that the apparatus is free contamination.
  • The temperature of surrounding must be fixed.
  • Mask and gloves must be worn throughout the experiment as a protection from dangerous chemical.

      
      Questions     

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

The mixture will appear clear. Based on the triangular paper, the point is plotted on the left side of the curve therefore a clear solution can be observed.

2.  What will happen if you dilute 1 part of the mixture with 4 parts of (a) water (b) toluene (c) ethanol?

(a)  Water:
Two phases will be observed.
(b)  Toluene:
Two phases will be observed.
(c)   Ethanol:
One phase will be observed, the solution remain clear.

Conclusion            
     
Ethanol, toluene and water system is a ternary system with one pair of partially miscible liquid (toluene and water). The addition of sufficient amount of ethanol to the toluene-water system would produce a single liquid phase in which all the three components are miscible and the mixture is homogenous. The phase diagram for Ternary System is determined.

Reference        
   
1.) http://www.chm.davidson.edu/vce/phasechanges/PhaseDiagram.html



4.)http://chemwiki.ucdavis.edu/Physical_Chemistry/Physical_Properties_of_Matter/Phases_of_Matter/Phase_Transitions/Phase_Diagrams

5.) Physicochemical Principles of Pharmacy, 3rd edition (1998) . A.T. Florence and D.Attwood. Macmillan Press Ltd.

6.) Physical Pharmacy: Physical Chemistry Principles in Pharmaceutical Sciences, by Martin, A.N.