Bulk density, Tapped Density PH 311 Laboratory Schedule & Manual

4 Experiment 3 – Carr’s Index, Hausner ratio, and Angle of Repose Determination

Aim: To determine the bulk density (BD), tapped density (TD), and angle of repose of given
powder and calculate its Carr’s index and Hausner’s ratio.

References:
 U.S. Pharmacopoeia, Chapter 616.
 The Theory and Practise of Industrial Pharmacy by Lachman and Liebermann, 3 rd Edition,
Chapter 11.
 Martin’s Physical Pharmacy and Pharmaceutical Sciences, 6th Edition, Chapter 18.

Requirements:
Apparatus: Weighing balance, glass/polypropylene funnel, glass/polypropylene measuring
cylinder (10mL/25mL), tapped density apparatus, beaker stand.

Chemicals: Granules

Theory:
The density of particles or powders is an important property affecting the processability
(powder flowability and compressibility into tablets) of powder samples. Density is defined as
weight per unit volume. In case of powders constituted with particles of different size ranges,
three types of densities can be defined.
a) True Density: The density of material itself, exclusive of the voids and intraparticle pores
larger than the molecular or atomic dimensions in the crystal lattices.
b) Granule Density: Determined by the displacement of mercury, which doesn’t not penetrate
the pores smaller than about 10µm at ordinary pressures.
c) Bulk density: Refers to the density of the powder determined by its bulk volume. Bulk
volume constitutes the true volume of the powder as well as the intra and inter-particle
voids.

Bulk density (ρb) is a characteristic of a volume of divided material such as powders, grains,
and granules. It includes the volume of solid material, open and closed pores, and the
interparticle voids. Bulk density largely depends on particle shape. As the particles become
more spherical in shape, the bulk density is increased. In addition, as the particle size increases,
the bulk density decreases. The smaller particles can form a close, more intimate packing than
larger granules. The total volume of interparticle voids can change with packing, thus leading
to the concept of tapped density, which measures the volume of a mass of sample after inducing

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Bulk density, Tapped Density PH 311 Laboratory Schedule & Manual

a closer packing of particles by tapping the container. Tapped density is the ratio of weight of
powder to the tapped volume. Tapped volume is the volume occupied by certain weight of
powder after standard number of tappings.

( )
𝐵𝑢𝑙𝑘 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 (ρ ) = (1)
( )

( )
𝑇𝑎𝑝𝑝𝑒𝑑 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 (ρ ) = (2)
( )

The interparticulate interactions influencing the bulk properties of a powder also interfere with
the powder flow. A comparison of the bulk and tapped densities can give an indirect measure
of the relative importance of these interactions in given powder. Such a comparison is often
used as an index of the ability of the powder to flow, for example, the compressibility index
(or Carr’s index) or the Hausner ratio. The compressibility index and Hausner ratios are
measures of the propensity of a powder to be compressed.

𝐶𝑎𝑟𝑟 𝑠 𝐼𝑛𝑑𝑒𝑥 = × 100 (3)

𝐻𝑎𝑢𝑠𝑛𝑒𝑟 𝑟𝑎𝑡𝑖𝑜 = (4)

Table: Correlation of powder flowability with Hausner ratio, carr’s index, angle of repose
Flow Property Hausner Ratio Carr’s Index Angle of repose
Excellent 1.00 – 1.11 <10 25 – 30
Good 1.12 – 1.18 11 – 15 31 – 35
Fair 1.19 – 1.25 16 – 20 36 – 40
Passable 1.26 – 1.34 21 – 25 41 – 45
Poor 1.35 – 1.45 26 – 31 46 – 55
Very Poor 1.46 – 1.59 32 – 37 56 – 65
Very very poor >38 >1.60 >66

The ability of a powder to flow is one of the factors involving in mixing different materials to
form a powder blend. There are many types of forces that can act between the solid particles
such as frictional forces, surface tension forces, mechanical forces caused by interlocking of
particles of irregular shape, electrostatic forces, and cohesive/van der Waals forces. These
forces can affect flow properties of a solid. Poorly flowing powders or granules present many
difficulties to the pharmaceutical industry. The production of uniform tablet dosage units has
been shown to depend on several granular properties. The frictional forces in a loose powder

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Bulk density, Tapped Density PH 311 Laboratory Schedule & Manual

can be measured by angle of repose (Φ). Angle of repose is the maximum possible angle
between the surface of a pile of powder and the horizontal plane. If more material is added to
the pile, it slides down the sides until the mutual friction of the particles, producing a surface
at an angle Φ, is in equilibrium with the gravitational forces. The tangent of the angle of repose
is equal to the coefficient of friction (µ) between the particles. Thus, the height of the pile and
diameter can provide a suitable information regarding the coefficient of friction of particles.

𝑡𝑎𝑛𝛷 = µ (5)

𝑡𝑎𝑛𝛷 = (6)

𝛷 = 𝑡𝑎𝑛 (7)

Where, 𝛷 is angle of repose, h is height of the powder pile (in cm) and r is the radius of the
base of the powder pile (in cm).

The rougher and more irregular the surface of the particles, the higher will be the angle of
repose.

Procedure:
A. For Bulk Density
1. Pass the given powder sample through a sieve of mesh 40.
2. Weigh 10g of the sieved powder and transfer gently to a 25mL measuring cylinder.
3. Carefully level the powder without compacting and read the volume of powder to the
nearest graduated unit.
4. Calculate the bulk density of the powder sample in grams/mL using equation (1).

B. For Tapped Density

1. The previously sieved powder sample is weighed (10g) and transferred to a 25mL
measuring cylinder.
2. The measuring cylinder is fixed onto the tapped density apparatus and tapped mechanically
for 100 times.
3. Note down the volume of the powder after 100 tapping which is referred to as tapped
volume.
4. Calculate the tapped density of the powder in grams/mL using equation (2).
5. Further calculate the Carr’s index (CI) and Hausner’s ratio (HR) from tapped and bulk
density data using equation (3) and (4), respectively.

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Bulk density, Tapped Density PH 311 Laboratory Schedule & Manual

Table 1: Volume and density measurements

For #20 Sieve Granules

Bulk Tapped Bulk Tapped Carr’s Hausner

Mass
Trial Volume Volume Density Density Index Ratio
(M)
(V1) (V2) (M/V1) (M/V2) (%)

Final Results (Average ± SD)

For #40 Sieve Granules

Bulk Tapped Bulk Tapped Carr’s Hausner

Mass
Trial Volume Volume Density Density Index Ratio
(M)
(V1) (V2) (M/V1) (M/V2) (%)

Final Results (Average ± SD)

C. For Angle of Repose

1. Take a funnel and place it upright on the burette stand. Adjust the height of the funnel such
that the exit orifice is just about 2.0 to 2.5 cm above the platform.
2. Keep a graph paper on the platform just below the orifice of the funnel.
3. Weigh 5g of the sieved powder sample and transfer to the funnel carefully by obstructing
the exit orifice of funnel completely with a thumb.
4. After transferring the whole quantity, remove the thumb from the orifice to let the powder
flow onto the paper placed beneath to form a pile of definite height and diameter.
5. Without disturbing the powder pile, measure the height (in cm) of the powder using a
measuring scale and trace the base of the powder pile using pencil.
6. Measure the diameter (in cm) of the pile base using a measuring scale (atleast 3 diameter
readings from one pile). Take average of the readings.

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Bulk density, Tapped Density PH 311 Laboratory Schedule & Manual

7. Repeat the experiment with same powder same thrice.

8. Calculate the angle of repose of the powder using equation (7).
9. Report the values and provide a comment its flowability based on the results.

For #20 Sieve Granules

Trial Height of Diameter (d) Davg Radius Angle of

(D1+D2+D3/3) (r =
pile (h) repose
Davg/2)
D1 =
1 D2 =
D3 =
D1 =
2 D2 =
D3 =
D1 =
3 D2 =
D3 =

Final Results (Average ± SD)

For #40 Sieve Granules

Height of Davg Radius Angle of

Trial Diameter (d) (r =
pile (h) (D1+D2+D3/3) repose
Davg/2)
D1 =
1 D2 =
D3 =
D1 =
2 D2 =
D3 =
D1 =
3 D2 =
D3 =

Final Results (Average ± SD)

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Bulk density, Tapped Density PH 311 Laboratory Schedule & Manual

Report:

1. The bulk and tapped density of the samples were found to be

a) #20 sieve granules =
b) #40 sieve granules =
2. The Carr’s index and Hausner’s ratio were found to be
a) #20 sieve granules =
b) #40 sieve granules =
3. The angle of repose of the granules before adding glidant
a) #20 sieve granules =
b) #40 sieve granules =
4. The angle of repose of the granules after adding ___% glidant
a) #20 sieve granules =
b) #40 sieve granules =

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