Tuesday, 8 December 2015

LAB 3 : Particle Size Analysis Using Sieving Method



Title :  Particle Size Analysis Using Sieving Method

Aim : To determine the particle size and  size distribution of  lactose powder and microcrystalline cellulose ( MCC)

Date : 19.11.2015
Introduction :
            A particle is a small object of any size range from microscopic scale to atomic scale . It is important to determine the size of the particle for a substance in order to obtain maximum efficacy of drug .  There are many methods that can be used for particle size analysis , including sieve method , microscope method , coulter counter and laser light diffraction method . The method chose for particle size analysis is based on criteria such as size range of analysis, wet or dry method , manual or automatic method and the speed of analysis .
In this experiment , sieve method are used to determine particle size and the distributions . Sieving is an old method commonly used to break down agglomerates , it is cheap , easy to perform and readily usable for large particle . It is usually use on dry samples only . It is not possible to perform on sprays and emulsions because it have very poor reproducibility for wet sieving .
In the sieving method , a sieve stack comprised on normally 6 to 8 sieves , with decreasing diameter is arranged from top to the bottom . Samples are loaded to the top sieve , that is the coarsest sieve and it is subjected to mechanical vibration for a fixed period of time . After that , the weight of sendiment collected at each stack is recorded and particle size analysis can be performed .
Apparatus : Sieve nest , spatula , weighing boat , electronic balance .
Material : Lactose powder , microcrystalline cellulose ( MCC ).


Procedure :
·         100g of lactose is weigh in a weighing boat using electronic balance .
·         Sieve nest is prepared in descending order from the largest diameter to the smallest diameter from top to bottom .
·         The powder is placed at the uppermost sieve and the sieving process is allow to proceed for 10 minutes .



·         Upon completion , the powder collected at every sieve is weighed .





·         The particle size distribution is plotted in the form of histogram .
·         The above process is repeated using MCC.
Result :
Particle size ( µm)
Mass of Lactose retained in the sieve (g)
% retained = (w sieve/w total )
x 100%
Cumulative percentage retained
% passing = 100% - cumulative percentage retained
>500
0.0392
0.0395
0.0395
99.9605
425-500
0.0046
0.0046
0.0441
99.9559
355-425
4.5063
4.5437
4.5878
95.4122
150-355
26.5859
26.8064
31.3942
68.6058
45-150
67.7878
68.3500
99.7442
0.2558
<45
0.2537
0.2558
100.00
0
                                                                   Table 1
               
                                                                    Figure 1




Particle size ( µm)
Mass of MCC retained in the sieve (g)
% retained = (w sieve/w total )
x 100%
Cumulative percentage retained
% passing = 100% - cumulative percentage retained
>500
0.0050
0.0051
0.0051
99.9949
425-500
0.0070
0.0071
0.0122
99.9878
355-425
0.1452
0.1473
0.1595
99.8405
150-355
6.5924
6.6879
6.8474
93.1526
45-150
88.9019
90.1897
97.0371
2.9629
<45
2.9206
2.9629
100.00
0
Table 2

Figure 2

Figure 3

Question :
·         What are the average particle size for both lactose and MCC ?
The average particle size for lactose and MCC fall between range 45-150µm.

·         What other methods can you use to determine the size of particle ?
Other method to determine size of particle is microscopy . It can be done through light microscope , transmission electron microscope and scanning electron microscope. It is operated by directly looking at the particles , thus determining not only the particle size but their shape and structure as well . The next method is coulter counter method , where powder samples must be first dispersed in an electrolyte to form very dilute suspension , it is then place in the coulter counter , the particle size is determine by the height of amplitude which correspond to the volume of particle displaced through the aperture into the aperture tube . Another method is laser light diffraction , where the detectors measure the particle size through the interaction between the particle and the laser beam .

·         What are the importance of particle size in a pharmaceutical formulation ?
    Particle size is important in the production of medicine as solid suspended in the liquid must be uniform so that there is no agglomerates and the content of the medicine is uniform . Particle size is important in pharmaceutical formulation as it affect drug release and drug dissolution . The smaller the size of the drug particle , the higher the surface of area in contact with the medium , thus it is easier to dissolve and easier to be absorbed by the body . Particle size also important in the case of administration of medicine , this is to make sure that drug injected into the body will not obstruct the blood vessels .

Discussion :
Size reduction process is also termed as communition or pulverization. The importance of particle size reduction is to aid efficient processing of solid particles by facilitating powder mixing or the production of suspensions, exposing cells prior to extraction and reducing the bulk volume of a material to improve transportation efficiency. Sieves is used to determine the particle size and the size distribution of both powders (MCC and Lactose). The method used of sieves is by putting MCC and Lactose powder in the most upper sieve. Then switch the plug and it will vibrate the sieve stack for 10 minutes. Each sieve can filter the powder to a smaller diameter. The highest diameter for the sieve is >500 µm followed by 425-500 µm, 355-425 µm, 150-355 µm, 45-150 µm and the lowest sieve diameter is <45 µm. After the sieving is finished. The result is obtained and recorded. The mass of powder for each sieve is measure by analytical balance. The mass obtained in different sieve indicates different size analysis of Lactose and MCC. The distribution of particle size of MCC and lactose is demonstrated experimentally in Figure 1, Figure 2, Figure 3.
Lactose and MCC have different material properties. This differences contribute to different on size distribution as shown in Figure 3. For Y axis for the graph is percentage of mass powder (MCC or Lactose) retained in the sieve (g) per total mass of powder inserted times 100. (% retained = (w sieve/w total) x 100%). For X axis is Particle size (µm). Based on data collected in the experiment particle size (µm) for MCC is >500 and the percentage retained is 0.0051% while for Lactose is 0.0395%. For 425-500 particle size (µm) the percentage retained is 0.0071% (MCC) while for Lactose is 0.0046%. For 355-425 the percentage retained is 0.1473% (MCC) while Lactose 4.5437%. For 150-355 is 6.6879% (MCC) while lactose 26.8064%. For         45-150 is 90.1897% (MCC) while lactose 68.3500% . For <45 is 2.9629% (MCC) while lactose 0.2558%. From comparison of  MCC and Lactose in the graph (Figure 3) we can deduced that MCC has finer and smaller particle size as compared to Lactose because the percentage retained of MCC in particle size (µm) >500, 355-425, 150-355 is lower than Lactose. This shown that particles of MCC is smaller that Lactose so that the tendency to pass through the sieves hole is higher and make the percentage retained is lower in particle size (µm)  >500, 355-425, 150-355 sieves.
      The total mass retained in sieves for Lactose is 99.1775g. The mass of lactose when put in the sieves stack is 100g. There is lack of 0.8225g in total mass retained. While handling this experiment after sieving is finished, we collect the total mass retained in each of the sieve but some of the powder is split. This lead to reduce of total Lactose mass retained in the sieve. The precaution can be made by more caution when handling this experiment to avoid error.

Conclusion:
In conclusion, we can conclude that difference substance have different of material properties such as Lactose and MCC. This difference resulting in difference of size distribution. Differences material properties required difference energy to reduce the particle size to the same size. This experiment indicates that MCC has smaller in particle size than lactose powder.


Reference:
1.      Patrick J. Sinko, Yashveer Singh. 2011. Martins Physical Pharmacy and Pharmaceutical Pharmacy Sciences. Ed. ke6. China: Lippincott Williams & Wilkins.  



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