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QC test for Powder
• 7th semester
• Madina college of Pharmacy
Hajra Iqbal: RPh
Lecturer Pharmaceutical
chemistry
October 2024
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POWDER
A powder is defined as a dry, solid substance, consisting of a large number
of finely divided particles (varying 10nm-1000μm), and typically obtained by
crushing, or grinding.
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Advantages
Powders are one of the oldest dosage forms and are used both internally
and externally.
Powders are more stable than liquid dosage form.
The changes of incompatibility are less as compared to liquid dosage
form.
Powders are more easy to transport then the liquid dosage form.
The onset of action of powdered drug is rapid as compared to other solid
dosage form. E.g. tablets, capsules
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Disadvantages
Drugs having bitter, nauseous and unpleasant taste can't be dispensed in
powdered form.
Deliquescent and hygroscopic drugs cant be dispensed in powder form.
Drugs which get affected by atmospheric conditions are not suitable for
dispensing in powder forms.
Not accurate dosage forms.
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CLACIFICATION OF POWDERS
1.Bulk powder for internal use.
2. Bulk powder for external use.
3. Simple and compound powder for internal use.
4. Powder enclosed in cachets and capsules.
5. Compressed powders(tablets).
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Evaluation of characteristics of granules or powders
1. Particle size and shape determination
2. Surface area
3. Density
Bulk density
True density
Granular density
4. Granule strength and friability
5. Flow properties
Angle of Repose
Percentage Compressibility Index
Hausner's ratio
6. Moisture content
7. Percentage fines
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1.PARTICLE SIZE AND SHAPE DETERMINATION
• Size affects the average weight of tablet, disintegration time, weight
variation, friability, flowability and drying rate.
• The size and shape depends upon processing requirements during
granulation.
• The methods for determining size and shape are:
a. Sieving
b. Sedimentation rate
c. Microscopy (SEM)By light Scattering
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a. Sieving
• Sieving (also referred to as screening) is
one of the most conventional and simplest
separation methods, having the advantage
of low-cost and ease of operation.
• A predetermined weight of dry powder is
passed through wire mesh screens, having
openings of different sizes, and the weight
of powder that is retained on each sieve is
measured.
• The nest of sieves is arranged from
coarser mesh opening to smaller mesh
opening, top to bottom.
• Vibration time is considered complete,
when the weight contained on any of the
sieves does not change by more than 5%.
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b. Sedimentation rate
• Sedimentation refers to the settling of a single particle in a
liquid medium under the influence of gravitational and
centrifugal forces.
• One of the most commonly used instruments for the sedi
mentation method is Andreasen pipette The apparatus is
composed of a 200 mm graduated cylinder with a pipette
located in the center. First, samples are mixed with the
liquid to form a suspension. Next, the suspension is placed
into the Andreasen pipette, sedimentation medium is
added, and the mixture is stirred by shaking the pipette.
After that, the pipette is left undisturbed for a certain period
of time. Then, 10 mL of the suspension is collected from a
position of 200 mm below the surface of the suspension,
and the weight of the solid obtained, after drying the
sample, is measured.
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c. microscopic method
Individual particles are measured by direct viewing of the particles, instead of statistically averaging
the diameter of a group of particles.
A sample size of at least 300–600 particles should be chosen, and, if the size difference between
particle to-particle is comparatively large, the sample size should be in creased to get a more
significant determination.
Light microscopy can be used to characterize particle sizes between about 1 to 150 microns in
diameter.
Both SEM and TEM can analyze par ticles having a much smaller size range than light microscopy,
typically less than 1 micron in diameter
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2. SURFACE AREA
• It is not commonly used for granules but generally used for drug substances
• if required particle size is measured and from this surface area is measured
• Mostly used methods are gas adsorption method and air permeability method.
• In gas adsorption, gas is adsorbed as monolayer on particles.This is in term calculated
and converted to surface area.
• In air permeability, the rate of air permeates a bed of powder is used to calculate surface
area of powder sample.
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3. DENSITY
• Another physical property of powders, is the ratio of mass to volume.
• Density may influence compressibility, tablet porosity and dissolution
• Dense hard granules may require higher load to produce cohesive
compact to reduce free granules seen on the surface of tablets
• Dense granules have less friability but cause a problem in releasing the
drug
• There are three methods to determine the density.
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3a. True or tapped density
• True density refers to the ratio of the mass of the particle to its actual
volume, excluding pore volume and the volume of the gap between
particles.
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• 3a. True or tapped density
Рo= M/V
Where, Pb bulk density of granules
M is mass of granules in gm
Vb is volume of granules in measuring cylinder after tapping in ml
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3b.Bulk Density
• Bulk density is defined as the ratio of powder bed mass to volume of that
powder bed, including both the pores and gap volume.
• Determination of powder bulk density is straight forward.
• The powder is filled into a cylinder, and, after vibration for a given time
period and intensity, the volume of powder bed is measured directly from
the cylinder.
• The bulk density is then calculated from the ratio of powder weight to
volume.
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3b. Bulk Density
Pb=M/Vb
Where, Pb bulk density of granules
M is mass of granules in gm
Vb is volume of granules in measuring cylinder in ml
more compressible bed of particulate - less flowable powder or granules
If less dense or compressible - more flowable powder or granules
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c. Granular density
• Particle density is defined as the ratio of particle mass to the particle
volume, including the pores within the particle, but still excluding the gaps
between particles.
• A commonly used method for determination of particle density is the
mercury intrusion method. Since mercury has a high surface tension, it
cannot pass through the small cracks or pores of the powder particles
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• c. Granular density
• It is determined by using pycnometer.
• Two methods are used to determine the granular density
• In one, intrusion fluid used - mercury, and other
• Any solvent of low surface tension e g.: benzene
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• The accuracy of these method depends upon ability of intrusion fluid to penetrate the
pores of granules
• Liquids should not masks granules solubilities in it, and having property to penetrate the
pores
• Density is then determined from volume of intrusion fluid displaced in pycnometer by
given mass of granulation
• It is calculated by using equation:
• Granular density (D) = M/ Vp-Vi
• Where, Vp - total volume of pycnometer
• Vi - volume of intrusion fluid (ml) containing Mass (M) (in gm) of granules required to fill
pycnometer.
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5. FLOW PROPERTIES
• It is an ability of the granule to flow from hopper to die cavity for tablet uniformity
• If flow property of granules are not uniform we are not getting tablet of uniform size
• Flow property of material results from many forces:
1. Frictional force
2. Surface tension force
3. Mechanical force caused by interlocking of irregular shape particles
4. Electrostatic forces
5. Cohesive/ vanderwaals forces
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• Forces also affect granule property such as particle size and shape, particle size distribution,
surface texture, roughness & surface area.
• If particle size of powder is </= 150micro meters the magnitude of frictional and vander waals force
predominate.
• When particle size increases, mechanical and physical properties become more important with
packing properties.
• Flow properties of granules are determined by measuring 3 parameters:
a. Angle of repose
b. Percentage compressibility index
c. Hausner's ratio
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5a. Angle of repose
• The angle between the free surface of the powder body and the horizontal plane is called the angle of repose
Tanϴ= h/r
h= Height of the pile
r= Radius of the pile
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Sr No Angle of repose Type of flow
1 ˂25 Excellent
2 25-30 Good
3 30-40 Passable
4 ˃40 Poor
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5b. PERCENTAGE COMPRESSIBILITY INDEX
• It is directly related to the relative flow rate cohesiveness and particle size. It is
simple, fast and popular method of presiding powder flow characters.
• It can be obtained from bulk density measurements
• % compressibility index = tapped density - bulk density /tapped density * 100
• I= (I-V/Vo) * 100
• Where I = % compressibility index
• V =volume occupied by powder/ granules after tapping
• Vo = volume of powder/ granules before tapping
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Sr No % Compressibility index Type of flow
1 5-15 Excellent
2 12-16 Very good
3 18-21 Good
4 23-25 Passable
5 33-38 Poor
6 ˃40 Very poor
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5c. HAUSNER'S RATIO
• It is related to interparticulate friction and as such could be used to predict powder flow
characteristics.
• It showed that powder with low particulate friction such as coarse sphere had ratio of
approximately 1.2, where as more is Cohesiveness - less free flowing powders such as
flakes have Hausner's ratio greater than 1.6
• Hausner's ratio = Tapped density / Bulk density
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6. Moisture content
• The amount of moisture present in the granule is called moisture content
• Generally granules contain 2% moisture. It is required for the binding of
the powder or granules during compression in die cavity.
• Percentage of moisture is calculated by using moisture balance or IR
balance.
• IR balance consist of simple balance which is placed to the casing in
which the IR bulb is attached which Produce heat inside the chamber.
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• The small amount of sample taken from oven to measure moisture content
and place in the moisture balance. Initial reading should be note down
after that we are initiating the IR bulb.
• As IR bulb is initiated the moisture is removed from the granules via
heating after that note down the reading
• % moisture content = initial weight - final weight /initial weight * 100
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7. PERCENTAGE FINES
• Fines means amount of powder remained in the granule.
• Generally the amount is 15% of fines.
• It is necessary for the tablet compression because if we are using 100%
granules then it is difficult to maintain hardness of tablet because they
have free space in the die cavity and after compression tablet will crack
due to air.
• % fines can be calculated by using sieve method.
• % fine should not be more than 15%.
