EUROPEAN PHARMACOPOEIA 10.0 2.9.36.

Powder flow

Hausner Ratio : Table 2.9.35.-1.

V0 Classification of powders by fineness

Vf Cumulative
Descriptive term x50 (μm) distribution by
Depending on the material, the compressibility index can be volume basis, Q3(x)
determined using V10 instead of V0. If V10 is used, it is clearly
stated with the results. Coarse > 355 Q3(355) < 0.50

180 - 355 Q3(180) < 0.50 and

Moderately fine
Q3(355) ≥ 0.50

Fine 125 - 180 Q3(125) < 0.50 and

Q3(180) ≥ 0.50
04/2019:20935
Very fine ≤ 125 Q3(125) ≥ 0.50

01/2010:20936

2.9.35. POWDER FINENESS(21)

Particle-size distribution is estimated by analytical
sieving (2.9.38) or by application of other suitable methods 2.9.36. POWDER FLOW(22)
where appropriate. A simple descriptive classification of The widespread use of powders in the pharmaceutical industry
powder fineness is provided in this chapter. For practical has generated a variety of methods for characterising powder
reasons, sieves are commonly used to measure powder flow. Not surprisingly, scores of references appear in the
fineness. Sieving is most suitable where a majority of the pharmaceutical literature, attempting to correlate the various
particles are larger than about 75 μm, although it can be used measures of powder flow to manufacturing properties. The
for some powders having smaller particle sizes where the development of such a variety of test methods was inevitable ;
method can be validated. Light diffraction is also a widely used powder behavior is multifaceted and thus complicates the
technique for measuring the size of a wide range of particles. effort to characterise powder flow.
Where the cumulative distribution has been determined by The purpose of this chapter is to review the methods for
analytical sieving or by application of other methods, particle characterising powder flow that have appeared most frequently
size may be characterised in the following manner : in the pharmaceutical literature. In addition, while it is
x90 clear that no single and simple test method can adequately
= particle size corresponding to 90 per cent of the characterise the flow properties of pharmaceutical powders,
cumulative undersize distribution ; this chapter proposes the standardisation of test methods that
x50 = median particle size (i.e. 50 per cent of the particles may be valuable during pharmaceutical development.
are smaller and 50 per cent of the particles are 4 commonly reported methods for testing powder flow are :
larger) ; – angle of repose,
x10 = particle size corresponding to 10 per cent of the – compressibility index or Hausner ratio,
cumulative undersize distribution.
– flow rate through an orifice,
It is recognised that the symbol d is also widely used to – shear cell.
designate these values. Therefore, the symbols d90, d50, d10 In addition, numerous variations of each of these basic
may be used. methods are available. Given the number of test methods
The following parameters may be defined based on the and variations, standardising the test methodology, where
cumulative distribution. possible, would be advantageous.
With this goal in mind, the most frequently used methods
Qr(x) = cumulative distribution of particles with a dimension are discussed below. Important experimental considerations
less than or equal to x where the subscript r reflects the are identified and recommendations are made regarding
distribution type. standardisation of the methods. In general, any method of
r
measuring powder flow must be practical, useful, reproducible
Distribution type
and sensitive, and must yield meaningful results. It bears
0 Number repeating that no simple powder flow method will adequately
or completely characterise the wide range of flow properties
1 Length experienced in the pharmaceutical industry. An appropriate
2 Area strategy may well be the use of multiple standardised test
methods to characterise the various aspects of powder flow as
3 Volume needed by the pharmaceutical scientist.
Therefore, by definition : ANGLE OF REPOSE
Qr(x) = 0.90 when x = x90 The angle of repose has been used in several branches of
science to characterise the flow properties of solids. Angle of
Qr(x) = 0.50 when x = x50 repose is a characteristic related to interparticulate friction, or
Qr(x) = 0.10 when x = x10 resistance to movement between particles. Angle of repose test
results are reported to be very dependent upon the method
An alternative but less informative method of classifying used. Experimental difficulties arise due to segregation of
powder fineness is by use of the descriptive terms in material and consolidation or aeration of the powder as the
Table 2.9.35.-1. cone is formed. Despite its difficulties, the method continues
(21) This chapter has undergone pharmacopoeial harmonisation. See chapter 5.8. Pharmacopoeial harmonisation.
(22) This chapter has undergone pharmacopoeial harmonisation. See chapter 5.8. Pharmacopoeial harmonisation.

General Notices (1) apply to all monographs and other texts 387
2.9.36. Powder flow EUROPEAN PHARMACOPOEIA 10.0

to be used in the pharmaceutical industry, and a number of – the peak of the cone of powder can be distorted by the
examples demonstrating its value in predicting manufacturing impact of powder from above. By carefully building the
problems appear in the literature. powder cone, the distortion caused by impact can be
minimised ;
The angle of repose is the constant, three-dimensional angle
(relative to the horizontal base) assumed by a cone-like pile of – the nature of the base upon which the powder cone is
material formed by any of several different methods, described formed influences the angle of repose. It is recommended
briefly below. that the powder cone be formed on a ‘common base’, which
can be achieved by forming the cone of powder on a layer
Basic methods for angle of repose of powder. This can be done by using a base of fixed
A variety of angle of repose test methods are described in the diameter with a protruding outer edge to retain a layer of
literature. The most common methods for determining the powder upon which the cone is formed.
static angle of repose can be classified based on 2 important Recommended procedure for angle of repose
experimental variables : Form the angle of repose on a fixed base with a retaining lip
– the height of the ‘funnel’ through which the powder passes to retain a layer of powder on the base. The base must be
may be fixed relative to the base, or the height may be free of vibration. Vary the height of the funnel to carefully
varied as the pile forms ; build up a symmetrical cone of powder. Care must be
taken to prevent vibration as the funnel is moved. The
– the base upon which the pile forms may be of fixed diameter funnel height is maintained at approximately 2-4 cm from
or the diameter of the powder cone may be allowed to vary the top of the powder pile as it is being formed in order
as the pile forms. to minimise the impact of falling powder on the tip of the
Variations in angle of repose methods cone. If a symmetrical cone of powder cannot be successfully
or reproducibly prepared, this method is not appropriate.
Variations of the above methods have also been used to some Determine the angle of repose by measuring the height of the
extent in the pharmaceutical literature : cone of powder and calculating the angle of repose, α, from
– drained angle of repose : this is determined by allowing the following equation :
an excess quantity of material positioned above a fixed
height
diameter base to ‘drain’ from the container. Formation tan(α) =
of a cone of powder on the fixed diameter base allows 0.5 × base
determination of the drained angle of repose ; COMPRESSIBILITY INDEX AND HAUSNER RATIO
– dynamic angle of repose : this is determined by filling a In recent years the compressibility index and the closely
cylinder (with a clear, flat cover on one end) and rotating related Hausner ratio have become the simple, fast, and
it at a specified speed. The dynamic angle of repose is the popular methods of predicting powder flow characteristics.
angle (relative to the horizontal) formed by the flowing The compressibility index has been proposed as an indirect
powder. The internal angle of kinetic friction is defined by measure of bulk density, size and shape, surface area, moisture
the plane separating those particles sliding down the top content, and cohesiveness of materials, because all of these
layer of the powder and those particles that are rotating can influence the observed compressibility index. The
with the drum (with roughened surface). compressibility index and the Hausner ratio are determined
General scale of flowability for angle of repose by measuring both the bulk volume and tapped volume of
a powder.
While there is some variation in the qualitative description
of powder flow using the angle of repose, much of the Basic methods for compressibility index and Hausner ratio
pharmaceutical literature appears to be consistent with the While there are some variations in the method of determining
classification by Carr(23), which is shown in Table 2.9.36.-1. the compressibility index and Hausner ratio, the basic
There are examples in the literature of formulations with procedure is to measure the unsettled apparent volume, (V0),
an angle of repose in the range of 40-50 degrees that and the final tapped volume, (Vf), of the powder after tapping
manufactured satisfactorily. When the angle of repose exceeds the material until no further volume changes occur. The
50 degrees, the flow is rarely acceptable for manufacturing compressibility index and the Hausner ratio are calculated
purposes. as follows :
V0 − V f
Table 2.9.36.-1. – Flow properties and corresponding angles Compressibility Index = 100 ×
of repose(23) V0
Flow property Angle of repose (degrees) V0
Hausner Ratio =
Excellent 25-30 Vf
Good 31-35 Alternatively, the compressibility index and Hausner ratio may
be calculated using measured values of bulk density (ρbulk) and
Fair (aid not needed) 36-40
tapped density (ρtapped) as follows :
Passable (may hang up) 41-45
ρtapped - ρbulk
Poor (must agitate, vibrate) 46-55 Compressibility Index = 100 ´
ρtapped
Very poor 56-65
ρtapped
Very, very poor > 66
Hausner Ratio =
ρbulk
Experimental considerations for angle of repose
In a variation of these methods, the rate of consolidation is
Angle of repose is not an intrinsic property of the powder, sometimes measured rather than, or in addition to, the change
that is to say, it is very much dependent upon the method in volume that occurs on tapping. For the compressibility
used to form the cone of powder. On this subject, the existing index and the Hausner ratio, the generally accepted scale of
literature raises these important considerations : flowability is given in Table 2.9.36.-2.
(23) Carr RL. Evaluating flow properties of solids. Chem. Eng 1965 ; 72:163-168.

388 See the information section on general monographs (cover pages)

EUROPEAN PHARMACOPOEIA 10.0 2.9.36. Powder flow

Table 2.9.36.-2. – Scale of flowability(23) Variations in methods for flow through an orifice
Compressibility Flow character Hausner ratio Either mass flow rate or volume flow rate can be determined.
index (per cent) Mass flow rate is the easier of the methods, but it biases the
1-10 Excellent 1.00-1.11 results in favour of high-density materials. Since die fill is
11-15 Good 1.12-1.18 volumetric, determining volume flow rate may be preferable.
A vibrator is occasionally attached to facilitate flow from the
16-20 Fair 1.19-1.25 container, however, this appears to complicate interpretation
21-25 Passable 1.26-1.34 of results. A moving orifice device has been proposed to
more closely simulate rotary press conditions. The minimum
26-31 Poor 1.35-1.45 diameter orifice through which powder flows can also be
32-37 Very poor 1.46-1.59 identified.
General scale of flowability for flow through an orifice
> 38 Very, very poor > 1.60
No general scale is available because flow rate is critically
Experimental considerations for the compressibility index dependent on the method used to measure it. Comparison
and Hausner ratio between published results is difficult.
Compressibility index and Hausner ratio are not intrinsic Experimental considerations for flow through an orifice
properties of the powder, that is to say, they are dependent Flow rate through an orifice is not an intrinsic property of the
upon the methodology used. The existing literature points out powder. It is very much dependent upon the methodology
several important considerations affecting the determination used. The existing literature points out several important
of the unsettled apparent volume, V0, of the final tapped considerations affecting these methods :
volume, Vf, of the bulk density, ρbulk, and of the tapped density, – the diameter and shape of the orifice,
ρtapped :
– the type of container material (metal, glass, plastic),
– the diameter of the cylinder used,
– the number of times the powder is tapped to achieve the – the diameter and height of the powder bed.
tapped density, Recommended procedure for flow through an orifice
– the mass of material used in the test, Flow rate through an orifice can be used only for materials
– rotation of the sample during tapping. that have some capacity to flow. It is not useful for cohesive
materials. Provided that the height of the powder bed (the
Recommended procedure for compressibility index and ‘head’ of powder) is much greater than the diameter of the
Hausner ratio orifice, the flow rate is virtually independent of the powder
Use a 250 mL volumetric cylinder with a test sample mass head. It is advisable to use a cylinder as the container, because
of 100 g. Smaller amounts and volumes may be used, but the walls of the container must have little effect on flow. This
variations in the method must be described with the results. configuration results in flow rate being determined by the
An average of 3 determinations is recommended. movement of powder over powder, rather than powder along
FLOW THROUGH AN ORIFICE the wall of the container. Powder flow rate often increases
when the height of the powder column is less than twice the
The flow rate of a material depends upon many factors, some diameter of the column. The orifice must be circular and the
of which are particle-related and some related to the process. cylinder must be free of vibration. General guidelines for
Monitoring the rate of flow of material through an orifice dimensions of the cylinder are as follows :
has been proposed as a better measure of powder flowability.
– diameter of the opening greater than 6 times the diameter
Of particular significance is the utility of monitoring flow
of the particles,
continuously, since pulsating flow patterns have been observed
even for free-flowing materials. Changes in flow rate as the – diameter of the cylinder greater than twice the diameter of
container empties can also be observed. Empirical equations the opening.
relating flow rate to the diameter of the opening, particle Use of a hopper as the container may be appropriate and
size, and particle density have been determined. However, representative of flow in a production situation. It is not
determining the flow rate through an orifice is useful only advisable to use a funnel, particularly one with a stem, because
with free-flowing materials. flow rate will be determined by the size and length of the stem
The flow rate through an orifice is generally measured as as well as the friction between the stem and the powder. A
the mass per time flowing from any of a number of types of truncated cone may be appropriate, but flow will be influenced
containers (cylinders, funnels, hoppers). Measurement of the by the powder-wall friction coefficient, thus, selection of an
flow rate can be in discrete increments or continuous. appropriate construction material is important.
Basic methods for flow through an orifice For the opening in the cylinder, use a flat-faced bottom
plate with the option to vary orifice diameter to provide
There are a variety of methods described in the literature. The
maximum flexibility and better ensure a powder-over-powder
most common for determining the flow rate through an orifice
flow pattern. Rate measurement can be either discrete or
can be classified based on 3 important experimental variables :
continuous. Continuous measurement using an electronic
– the type of container used to contain the powder. Common balance can more effectively detect momentary flow rate
containers are cylinders, funnels, and hoppers from variations.
production equipment ;
– the size and shape of the orifice used. The orifice diameter SHEAR CELL METHODS
and shape are critical factors in determining powder flow In an effort to put powder flow studies and hopper design on a
rate ; more fundamental basis, a variety of powder shear testers and
– the method of measuring powder flow rate. Flow rate can methods that permit more thorough and precisely defined
be measured continuously using an electronic balance assessment of powder flow properties have been developed.
with some sort of recording device (strip chart recorder, Shear cell methodology has been used extensively in the study
computer). It can also be measured in discrete samples of pharmaceutical materials. From these methods, a wide
(for example, the time it takes for 100 g of powder to pass variety of parameters can be obtained, including the yield loci
through the orifice to the nearest tenth of a second or the representing the shear stress-shear strain relationship, the
amount of powder passing through the orifice in 10 s to angle of internal friction, the unconfined yield strength, the
the nearest tenth of a gram). tensile strength, and a variety of derived parameters such as

General Notices (1) apply to all monographs and other texts 389
2.9.37. Optical microscopy EUROPEAN PHARMACOPOEIA 10.0

the flow factor and other flowability indices. Because of the are used with achromatic objectives, and are preferable
ability to control experimental parameters more precisely, with apochromats ; they are required for appropriate colour
flow properties can also be determined as a function of rendition in photomicrography. Condensers, corrected at least
consolidation load, time, and other environmental conditions. for spherical aberration are used in the microscope substage
These methods have been successfully used to determine and with the lamp. The numerical aperture of the substage
critical hopper and bin parameters. condenser matches that of the objective under the conditions
Basic methods for shear cell of use ; this is affected by the actual aperture of the condenser
diaphragm and the presence of immersion oils.
One type of shear cell is the cylindrical shear cell which is
split horizontally, forming a shear plane between the lower Adjustment. The precise alignment of all elements of
stationary base and the upper moveable portion of the shear the optical system and proper focusing are essential. The
cell ring. After powder bed consolidation in the shear cell focusing of the elements is done in accordance with the
(using a well-defined procedure), the force necessary to shear recommendations of the microscope manufacturer. Critical
the powder bed by moving the upper ring is determined. axial alignment is recommended.
Annular shear cell designs offer some advantages over the Illumination. A requirement for good illumination is a
cylindrical shear cell design, including the need for less uniform and adjustable intensity of light over the entire field
material. A disadvantage, however, is that because of its of view ; Köhler illumination is preferred. With coloured
design, the powder bed is not sheared as uniformly because particles, choose the colour of the filters so as to control the
material on the outside of the annulus is sheared more contrast and detail of the image.
than material in the inner region. A third type of shear cell
(plate-type) consists of a thin sandwich of powder between a Visual characterisation. The magnification and numerical
lower stationary rough surface and an upper rough surface aperture must be sufficiently high to allow adequate resolution
that is moveable. of the images of the particles to be characterised. Determine
All of the shear cell methods have their advantages and the actual magnification using a calibrated stage micrometer
disadvantages, but a detailed review is beyond the scope of to calibrate an ocular micrometer. Errors can be minimised if
this chapter. As with the other methods for characterising the magnification is sufficient that the image of the particle is
powder flow, many variations are described in the literature. at least 10 ocular divisions. Each objective must be calibrated
A significant advantage of shear cell methodology in general separately. To calibrate the ocular scale, the stage micrometer
is a greater degree of experimental control. The methodology scale and the ocular scale must be aligned. In this way, a
generally is rather time-consuming and requires significant precise determination of the distance between ocular stage
amounts of material and a well-trained operator. divisions can be made. Several different magnifications may
be necessary to characterise materials having a wide particle
Recommendations for shear cell size distribution.
The many existing shear cell configurations and test methods Photographic characterisation. If particle size is to be
provide a wealth of data and can be used very effectively determined by photographic methods, take care to ensure
to characterise powder flow. They are also helpful in the that the object is sharply focused at the plane of the
design of equipment such as hoppers and bins. Because of the photographic emulsion. Determine the actual magnification
diversity of available equipment and experimental procedures, by photographing a calibrated stage micrometer, using
no specific recommendations regarding methodology are photographic film of sufficient speed, resolving power, and
presented in this chapter. It is recommended that the results contrast. Exposure and processing must be identical for
of powder flow characterisation using shear cell methodology photographs of both the test sample and the determination
include a complete description of equipment and methodology of magnification. The apparent size of a photographic image
used. is influenced by the exposure, development, and printing
processes as well as by the resolving power of the microscope.
01/2010:20937 Preparation of the mount. The mounting medium will
vary according to the physical properties of the test sample.
Sufficient, but not excessive, contrast between the sample and
the mounting medium is required to ensure adequate detail
of the sample edge. The particles must rest in one plane and
2.9.37. OPTICAL MICROSCOPY(24) be adequately dispersed to distinguish individual particles of
interest. Furthermore, the particles must be representative
Optical microscopy for particle characterisation can generally of the distribution of sizes in the material and must not be
be applied to particles of 1 μm and greater. The lower limit altered during preparation of the mount. Care must be taken
is imposed by the resolving power of the microscope. The to ensure that this important requirement is met. Selection of
upper limit is less definite and is determined by the increased the mounting medium must include a consideration of the
difficulty associated with the characterisation of larger analyte solubility.
particles. Various alternative techniques are available for
particle characterisation outside the applicable range of optical Crystallinity characterisation. The crystallinity of a material
microscopy. Optical microscopy is particularly useful for may be characterised to determine compliance with the
characterising particles that are not spherical. This method crystallinity requirement where stated in the individual
may also serve as a base for the calibration of faster and more monograph of a drug substance. Unless otherwise specified
routine methods that may be developed. in the individual monograph, mount a few particles of the
Apparatus. Use a microscope that is stable and protected sample in mineral oil on a clean glass slide. Examine the
from vibration. The microscope magnification (product of the mixture using a polarising microscope : the particles show
objective magnification, ocular magnification, and additional birefringence (interference colors) and extinction positions
magnifying components) must be sufficient to allow adequate when the microscope stage is revolved.
characterisation of the smallest particles to be classified in the Limit test of particle size by microscopy. Weigh a suitable
test sample. The greatest numerical aperture of the objective quantity of the powder to be examined (for example,
is sought for each magnification range. Polarising filters may 10-100 mg), and suspend it in 10 mL of a suitable medium
be used in conjunction with suitable analysers and retardation in which the powder does not dissolve, adding, if necessary,
plates. Colour filters of relatively narrow spectral transmission a wetting agent. A homogeneous suspension of particles
(24) This chapter has undergone pharmacopoeial harmonisation. See chapter 5.8. Pharmacopoeial harmonisation.

390 See the information section on general monographs (cover pages)