Thursday, 17 December 2015

LAB 4 PART A PARTICLE SIZE ANALYSIS USING SIEVING METHOD

TITLE
Part A: Particle Size analysis using Sieving Method

OBJECTIVES
To determine the particle size of lactose and microcrystalline cellulose (MCC).
To classify and differentiate the powder based on the diameter of the powder particles.
To identify the size distribution of lactose and microcrystalline cellulose (MCC)

DATE OF EXPERIMENT
16th November 2015

INTRODUCTION
A test sieve is an instrument which is used for the measurement of particle size. In its most common form it consists of a woven wire screen, with square apertures, rigidly mounted in a shallow cylindrical metal frame. For coarse sieving a perforated plate screen with square or round holes may be used in place of wire mesh. Square hole perforated plate sieves range down to 4mm and round hole sieves down to 1mm aperture.
A sieve test is performed by first assembling a stack of interlocking sieves. In this stack, the sieve with the largest opening is at the top. Each lower sieve will have a smaller opening than the one on the above.
The materials which are tested in this experiment are lactose and microcrystalline cellulose (MCC). The lactose is first weighed and is poured into the sieve nest before being sieved by using mechanical shaker for a fixed amount of time. At the end of the experiment, the weight of lactose is recorded and the experiment is repeated by using microcrystalline celluluose. The overall results are then presented in histograms.


LIST OF MATERIALS
Microcrystalline cellulose (MCC), Lactose


LIST OF APPARATUS
Mechanical sieve, sieve nests, large weighing boats, spatula, electronic balance, newspaper


EXPERIMENTAL METHOD
1.      100 g of lactose is weighed.


2.      The sieve nest is prepared in descending order (largest diameter to the smallest, from top to bottom).
3.      The powders are placed at the uppermost sieve and allow the sieving process to proceed for 15 minutes.




4.      Upon completion, the powder collected is weighted at every sieve and the particle size distribution is plotted in the form of histogram.
5.      The above process is repeated using MCC.



RESULTS

Lactose
Diameter of sieve nest (μm)
50
150
200
425
500
Weight (g)
38.6768
0.1488
60.9122
0.0092
0.0218





MCC
Diameter of sieve nest (μm)
<53
53
150
200
300
500
Weight (g)
17.5855
76.8885
3.3547
1.8236
0.2216
0.1261




QUESTIONS

1. What are the average particle size for lactose and MCC?
 The average particle size of lactose is between 50 µm to 200 µm and the average particle size of MCC is between 50µm to 150µm.

2. What other methods can you use to determine the size of particle?
The other methods to determine the size of particles are surface area measurement, sedimentation, electron microscope analysis, Coulter counter, laser light scattering technique, dynamic light scattering technique and optical and electrical sensing zone method.

3. What are the importances of particle size in a pharmaceutical formulation?
For the pharmaceutical industry, particle size impacts products as an influence on drug performance. Particle size of the active pharmaceutical ingredient (API) and inert excipients are to be considered in pre-formulation, design of drug delivery system as it is influencing the proceessability, stability, bioavailability and efficacy of drug delivery system. Particle size is having a pronounced effect on the absorption of drugs with low aqueous solubility for the solid dosage form. Smaller particle size has higher absorption compared to bigger particle size for the conventional solid dosage forms such as tablets that are administered orally for local and systemic action. In the other hand, the particle size of disintegrants like starch influences the disintegration time of the tablets as starch grains with large particle size are more efficient disintegrants compared to the smaller one. Furthermore, the efficacy of lubricant is also influenced by the particle size and lubricants that having a particle size of 60-100 mesh are used most often.  For insoluble drugs, the particle size of the filler influenced the dissolution rate and affect on the solubility of the drug. Syringeability and injectability properties of a parenteral suspension are closely related to the particle characteristics of the parenteral suspension. The rate of reconstitution from a drug powder to form aqueous solution/suspension is influenced by the particle size. The particle size of the dispersed phase should be below 10um in order to minimize pain and tissue irritation.

DISCUSSION

Sieving is one of the oldest methods of classifying powders and granules by particle size distribution. The sieving will sort the particle by their intermediate size dimension when sieve using a woven sieve cloth. The particles larger than 75µm is sieved with mechanical sieving whereas for smaller particles, the light weight provides insufficient force during sieving and this will cause the particles to stick together and the particles expected to pass through the sieve will be retained. Sieving is a method of choice to classify coarser grades of single powders or granules in the pharmaceutical field.
                        In this experiment, the particle size distribution of lactose and are microcrystalline cellulose (MCC) are being observed. The method used to determine their particle size distribution was sieving method or sieve analysis. A sieve nest is used to determine the article size distribution. The sieve nest is arranged in descending order from top to bottom which is from largest diameter to smallest diameter. The sieve that have diameter of aperture of 500 µm will be placed at the top followed by 425 µm, 200 µm, 150 µm, and 50 µm. The coarsest sieve was loaded with the lactose powder and it is operated for mechanical vibration for 20 minutes. The procedures are the same for the microcrystalline cellulose (MCC).

                        In this experiment, the particle size of lactose is measured based on the principle that the particle cannot pass through the sieve due to larger size particle than the sieve. Based on the results obtained, the particle size of lactose is mostly in between 200 µm and 425 µm as 60.91g of lactose is collected in this sieve followed by particle size less than 50 µm as 38.68g of lactose is collected at the most bottom sieve. In microcrystalline cellulose (MCC), the powder is mostly collected in the 53 µm sieve with 76.89g and we can assume that microcrystalline cellulose (MCC) have particle size is in between  53 µm and 150 µm follow by less than 53 µm as 17.58g of microcrystalline cellulose (MCC) is collected. Comparing both lactose and microcrystalline cellulose (MCC), we can deduct that microcrystalline cellulose (MCC)  have smaller particle size and finer than lactose.

                        The initial total weight of lactose and microcrystalline cellulose (MCC) is both 100g but by the end of experiment, the weight of lactose is 94.9g whereas microcrystalline cellulose (MCC) remains 100g. This clearly indicates that some of the lactose powder is lost during the lab and error occurs. One is when transferring of lactose and microcrystalline cellulose (MCC) from the weighing boat into the sieve and after 20 minutes of mechanical vibration, the transferring of the powder back into the weighing boat for weighing. During the process of transferring, some of the powder is still preset either in the sieve or weighing boat. This explains why the final weight of the lactose powder is not exactly 100g. The second error that occurs during the lab is the sieve nest is not covered tightly due to the machine malfunction. . Some of the powder may spill out from the container as the machine is not closed tightly. In this condition, the vibration of the machine may be irregular and this will affect the separation of powder in the sieve nest. Thus, error occurs. The powders are light weight particles. Thus, when exposed to air, it may evaporate of carried by water vapour into the air causing loss of weight. The mass will not be accurate.  Before the experiment, the sieves are cleaned using a brush to remove any powder from the previous experiment. The machine needs to be sealed tightly to prevent error.
                                                                                          
CONCLUSION
Most particles size of lactose are in the range of 0 - 49µm followed by range of 151 – 200µm. While as for MCC, most particles size are in the range of 0 - 52µm followed by 53 µm. This shows that most particles in MCC is smaller than those of lactose.

REFERENCE
Martin, A. 2011. Physcial Pharmacy: Physical Chemistry Principles in Pharmaceutical Sciences. Edisi ke-6. Philadelphia: Lippincott Williams & Wilkins.
Chang, R. & Goldsby, K. A. 2014. Chemistry. Edisi ke-11. New York: McGraw- Hill Education.

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