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Ana Marie L. Rubenicia, RPh March 14, 2012

Micromeritics

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By Mrs. Ana Marie Rubenicia RPh

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Page 1: Micromeritics

Ana Marie L. Rubenicia, RPhMarch 14, 2012

Page 2: Micromeritics

Micromeritics is the science of small particles. It is the study of a number of characteristics, including paticle size and size distribution, shape, angle of repose, porosity, true volume, apparent demsity nd bulkiness.

Page 3: Micromeritics

Particles are any unit of matter having defined physical dimensions.

Physical state of particles can be altered by physical

manipulation

Particle characteristics can alter therapeutic

effectiveness.

Page 4: Micromeritics

MICROMERITICSFACTORS AFFECTING FLOW PROPERTIES

1. PARTICLE SIZE AND SHAPE

250-2000m = free flowing75 – 250 m = flow freely or cause problem depending on

shapeVery fine particles (less than 10 m) = do not flow freely as

large particlesParticle shape and flow propertiesSpherical shape flow better than needle particlesElongated or flat particles tend to pack resulting to high

porosity powders

2. POROSITY AND DENSITYHigh density, low porosity = FREE FLOWING

3. SURFACE ROUGHNESS Leads to poor flow characteristics

Page 5: Micromeritics

MICROMERITICSTechniques of determining particle sizeMICROSCOPIC METHOD(OPTICAL MICROSCOPY)Uses an ordinary microscope for particle

measurement in the range of 0.2 m to 100 m.Presence of agglomeration and particles of more

than one component may be detectedThe diameter is obtained only from two

dimensions: length and breadth, the thickness/depth in not measured.

The microscopic method can include counting not fewer than 200 particles in a single plane using calibrated ocular on a microscope.

Page 6: Micromeritics

Particle SizeSIZE OF PARTICLE IN uM

MIDDLEVALUE“D”(um)

# OF PARTICLEPERGR ”N”

“ND”

40-60 50 15 750

60-80 70 25 1750

80-100 90 95 8550

100-120 110 140 15400

120-140 130 80 10400

∑n=355 ∑nd=36,800

1. Given the following data, what is the average diameter of the particles?

dav= ∑ nd / ∑n

dav = 36,850 / 355

dav = 103.8uM

Page 7: Micromeritics

PARTICLE SIZESIEVING - uses standard sieves; generally used for

grading coarser particles. May be employed for screening materials as fine as 44 m (No. 325 sieve)

POWDERS OF VEGETABLE AND ANIMAL DRUGS ARE OFFICIALLY DEFINED AS:

VERY COARSE (#8) – all particles pass through no.8 sieve and not more than 20 % through sieve no. 60.

COARSE (#20) – all particles pass through no.20 sieve and not more than 40 % through sieve no. 60.

MODERATELY COARSE (#40) - all particles pass through no.40 sieve and not more than 40 % through sieve no. 80.

FINE (#60) - all particles pass through no.60 sieve and not more than 40 % through sieve no. 100.

VERY FINE (#80) – all particles pass through a no. 80 sieve. There is no limit as to greater fineness.

 

Page 8: Micromeritics

PARTICLE SIZEPOWDERS OF CHEMICAL DRUGS ARE

OFFICIALLY DEFINED AS:COARSE (#20) – all particles pass through

no.20 sieve and not more than 40 % through sieve no. 60.

MODERATELY COARSE (#40) - all particles pass through no.40 sieve and not more than 60 % through sieve no. 60.

FINE (#80) - all particles pass through no.80 sieve and there is no limit as to greater fineness.

Page 9: Micromeritics

PARTICLE SIZE0.5 um – 10um – suspensions and fine

emulsions10 um – 50um - upper limit of subsieve range;

coarse emulsion particles; flocculated suspension particles

50 um – 100um – lower limit of sieve range; fine powder range

150 um – 1000um – coarse powder range1000 um – 3360um –average granule size

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A stack of sieve is arranged in order, the powder placed in the top sieve, the stack shaken, the quantity of powder resting on each sieve weighed, and this calculation performed:

dav= ∑(% retained)x(ave size) / 100

dav = 29.232 / 100 = 0.2923mm

Page 11: Micromeritics

PARTICLE SIZEOther ways of particle size determonation elutriation,

centrifugation, permeation, adsorption, the Coulter Counter, and light obstruction and the use of Andreasen pipet.

dst = 18 h /(i - e)gt

Angle of reposeA relative simple technique for estimating the flow properties of a powder. It can easily be determined by allowing a powder to flow though a funnel and fall feerly onto a surface. The height and diameter of the resulting cone are measured and the angle of repose calculated as:

tan Ѳ = h/r

h is the height of the powder cone and r is the radius of the powder cone

Low angle of repose – flow freely; high angle of repose – flow poorly

Page 12: Micromeritics

PARTICLE SIZECharateristics used to describe powder –

porosity, true volume, bulk volume, apparent density, true density, and bulkiness.

Void= Vbulk - V ; Porosity = Vbulk - V x 100 Vbulk Vbulk

Apparent Density pa = Weight of the sample ; Vbulk

true density p = Weight of the sample V

Bulkiness, B = 1/pa

Page 13: Micromeritics

PARTICLE SIZEEXAMPLE

A selected powder has a true density (p) of 3.5g/cc. Experimentally, 2.5 g of the powder measures 40 mL in a cylindrical graduate. Calculate the true volume, void, porosity, apparent density, and bulkiness.

Page 14: Micromeritics

PARTICLE SIZEClosest packing:rhombus-triangle – angles of 60

deg and 120 deg: void=o.26 ; porosity=20%Open type of packing:cubical – cubes packed at

90 deg angle: void=0.47; porosity=47%Importance of packing and flow:a. Affects the size of the containerb. The flow of granulationc. Efficiency of filling apparatues for making

tablets and capsules.d. Ease of working with powders.

Page 15: Micromeritics

Particle Size ReductionComminution, reduction of the particle size of a solid

substance to a finer state, is used :1. Facilitate crude drug extraction.2. Increase the dissolution rates of a drug3. Aid in the formulation of acceptable pharmaceutical

forms.4. Enhance absorption of drugs.

The reduction in the particle size of a solid is accompanied by a great increase in the specific surface area of the substance.

Page 16: Micromeritics

Particle Size ReductionEXAMPLEIncrease in number of particlesIf a powder consists of 1mm on edge and it is reduced to

paricles 10 um on edge, what is the number of particles reduced?

1. 1mm equals 1000um.2. 1000um/10um = 100 pieces produced on each edge;

that is, if the cube is sliced into 100 pieces on the x-axis,each 10um long, 100 pieces result.

3. If this repeated on the x- and y-axis, the result is 100x100x100 = 1 million particles produced, each 10um on edge, for each original particle 1mm on edge. This can also be written an 106 .

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Particle Size ReductionIncrease in surface areaWhat increase in the surface area of the powder is produced by

decreasing the particle size from 1mm to 10um?1. The 1mm cube has 6 surfaces, each 1mm on edge. Each face

has a surface area of 1 mm2. Because there are 6 surfaces, this 6 mm2 surface area per particle.

2. Each 10um cube has 6 surfaces, each 10um on edge. Each face has a surface area of 10x10 = 100 um2 . Because there are 6 faces, this is 6x100 um2 or 600 um2 surface area per particle. Since 106 particles resulted from comminuting the 1m cube, each 10um on edge, the surfaces are now is 600 um2 x 106, or 6 x 108um2 .

3. To get everything in the same units for ease of comparison, convert the 6 x 108um2 in to square mm as follows.

4. Since there are 1000um/mm, there must be 1000 2 ,or 1 million um2 / mm2 .

This is more appropriately express as 106 um2 / mm2, 6 x 108um2 = 6 x 102mm2 106 um2 / mm2

4

The surface area have been increased from

6 mm2 to 600 mm by the reduction inParticle size of cubes 1mm to cubes 100um on edge, an hundred fold inc

in surface area.

Page 18: Micromeritics

Thank you…May God Bless All Your Dreams and Endeavors…