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ABSTRACT This experiment was done to find out the relationship between particle sizes with the angle

of repose. Empirical method that was used for the assessment of bulk solid properties is Fixed funnel method (the funnel was held closely above the petri dish in order to form a heap). Two different powders were used which are coarse sugar and starch. Same steps are repeated with starch added with 5% glidant which was magnesium stearate. The powders are poured into petri dish through a funnel held by a retort stand. When the petri dish is full and the powder begins to spill, then the pouring was stopped. The height of the pile was measured and angle of repose was calculated by using the formula: Tan = h / r INTRODUCTION Knowledge of the flow properties of a powder or a bulk solid is necessary to design silos and other bulk solid handling equipment so that no flow problems (flow obstructions, segregation, irregular flow, flooding, etc.) occur. Furthermore, quantitative information regarding flowability of bulk products is required, e.g. as part of comparative tests (e.g. effect of flow agents or other additions on flow behaviour) and quality control. The flow properties depend on several parameters which are particle size distribution, particle shape, chemical composition of the particles, moisture and temperature. It is not possible to determine theoretically the flow behaviour of bulk solids in dependence of all of these parameters. Even if this were possible, the expense for the determination of all parameters of influence would be very high. Thus it is necessary, and also simpler, to determine the flow properties in appropriate testing devices. The present paper deals with all kind of particulate solids, which are also called bulk solids, powders, or granulates. In the following the general expression bulk solid is used for all these products. The angle of repose (AoR) measures the angle of inclination of the free surface to the horizontal of a bulk solid pile. It is one of the primary properties of powders that indicates the interparticulate friction and has been used to characterize the flow behavior of powders and granular materials with respect to flowability, avalanching, stratification and segregation. OBJECTIVE 1. To calculate the angle of repose for powders having different particle sizes. 2. To investigate the relationship between size of different particles with angle of repose. APPARATUS/CHEMICAL/SUBSTANCE 1. Petri dish 2. Retort stand 3. Funnel 4. Sieve 5. Beaker 6. Weighing balance 7. Ruler 8. Container 9. Coarse sugar 10. Icing sugar/starch 11. Magnesium stearate

METHODOLOGY Experimental Method - Angle of Repose 1. Measure the external diameter of the petri dish supplied to you. Position the bottom of a funnel about 5 to 15 cm above the center of the upturned petri dish using ring stand. 2. Place a container under the petri dish so that you can pick up the powder and reuse the powder for all your replicates. 3. Slowly pour the powder sample into the funnel, tapping the funnel as necessary to ensure that powder flows through the hole. Continue this process until the bottom of the powder pile just begins to fall over the edge of the petri dish. 4. Measure the height of the pile using a ruler. If the powder is lumpy, sieve it prior to beginning the experiment. 5. Repeat Step 3-4 to obtain the triplicate. 6. Calculate the mean height of the powder pile and the mean angle of repose (0). 7. Repeat Steps 3-6 using fns powder. 8. Repeat Steps 3-6 usingfine powder with glidant. NB: Tan = Opposite / Adjacent. Therefore Tan = h/r. Experimental Method - Angle of Repose 1. A shutter was placed at the base of the funnel 2. Funnel was loaded with 50 g of the course powder. 3. Shutter was opened. 4. The time to completely empty the funnel (hopper) was recorded. 5. Step 4 was repeated to obtain triplicates. 6. Average time was calculated. 7. Steps 2-6 were repeated with fine powder and fine powder plus glidant. RESULT R=4.3cm Coarse sugar height(cm) time(s) 2.5 10 2.5 10 2.0 11 2.3 10.3 = tan-1 (2.3/4.3) =28.14o 50g/10.3s =4.85 g s-1 Starch height(cm) time(s) 4.7 4.8 4.7 4.73 = tan-1 (4.73/4.3) =47.73o starch + glidant height(cm) time(s) 4.5 57 4.4 55 4.4 54 4.43 55.3 = tan-1 (4.73/4.3) =47.73o

1 2 3 Mean Angle of repose tan =h/r Mass flow rate Mass/time

DISCUSSION During the practical, the result interpretations were as followed: 1. Coarse sugar has low angle of repose compared to the starch. 2. Coarse sugar has good flow property compared to the starch. 3. It means the coarse sugar has less cohesive force between the particles as compared to the starch. Determination of the result was done by following this guideline: Angle of Repose Flow property 25-30 Excellent 31-35 Good 36-40 Fair 41-45 Passable 46-55 Poor 56-65 Very poor >66 Very, very poor Mass flow rate is the time taken for the particles to move descends the funnel. The higher the mass flow rate the shorter the time taken by the powder to descend. The results show that coarse sugar takes shorter time to descend compared to starch added with glidant due to cohesive forces between the particles. A glidant is a substance that is added to a powder to improve its flowability. A glidant will only work at a certain range of concentrations. Above a certain concentration, the glidant will in fact function to inhibit flowability (Which means that there's a critical concentration to be used if increasing powder's flowability is intended with respect to the glidant and the powder properties). In tablet manufacture, glidants are usually added just prior to compression.The glidant used in this experiment was magnesium stearate In conducting this practical, there were several precautions need to be considered. The fine powder need to be poured slowly and little by little to prevent it from stuck in the funnel. This situation needed to be avoided as it may affect the time recorded for the powder to descend. The container (in this experiment, newspaper was used) should be nicely placed under the petri dish to pick and reuse any spilled powder (coarse sugar and starch). The nozzle of the funnel must be precisely set at the center of the petri dish to yield a more accurate angle of repose. CONCLUSION Measurement of angle of repose through fixed funnel method can determine the powder cohesiveness. Highly cohesive powder will produce higher angle of repose compared to less cohesive powder. Highly cohesive powder also requires longer time to descend through funnel when being poured.

REFERENCE Aulton, M. E. (2002). Pharmaceutics: The Science of Dosage Form. Churchill Livingstone, London. http://en.wikipedia.org/wiki/Glidant. Retrieved 25 October 2011 https://engineering.purdue.edu/ABE/People/Papers/klein.ileleji.1/bulkcorn. Retrieved 24 October 2011. Schulze, D. (2006).Flow Properties of Powders and Bulk Solids.


PHM 3133 Dosage Design I Practical 2

Determination of the Angle of Repose and Flow Properties of Powder