The Field Guide to

Food Powder
Characterization
E-Book
Next-Generation
Food Powder Analysis
With Anton Paar’s portfolio of analytical instrumentation, deepen your understanding of food
powders with next-generation analysis techniques. Develop the right formulation, overcome
transportation and storage issues, and offer better, more enjoyable foods for consumers.

This e-book contains detailed measurement data including determination of density, particle
size, powder flow, cohesion strength, compressibility, and permeability.

1 FORMULATION AND R&D 3 PACKAGING AND STORAGE

1.1 Particle size analysis of food powders 3.1 Tapped and true density of food powders
1.2 X-ray diffraction for identifying crystalline 3.2 Oxidation stability of food powders
phases in food powders

14—16
4—8

4 FINAL PRODUCT ANALYSIS AND CUSTOMER

2 TRANSPORTATION AND POWDER FLOW EXPERIENCE
RHEOLOGY

4.1 Dissolution rate of food powders

2.1 Recognition of changes in powder flow 4.2 Viscosity and mouthfeel of food powders
properties 4.3 Food safety
2.2 Investigation of powder flow behavior as
a function of external parameters such as 17—21
relative humidity

9—13

5 ANTON PAAR SOLUTIONS

22—23
1 Formulation and R&D

Finding the right formulation is of utmost importance Particle analysis of chocolate powder
not only to ensure the desired product quality, but Cocoa mass needs to be ground down into smaller
also to save on manufacturing costs. Optimizing particle sizes to enable as much cocoa butter to be
food powder parameters such as particle size and released as possible. On the other hand, very small
particle size distribution enables the manufacturer particles lead to higher surface area meaning that more
to lower production costs and for the consumer of the expensive cocoa butter is needed to coat the
to enjoy higher quality products. Improving particles. The particle size thus has to be optimized in
formulations based on particle size reduces the order to reduce the need for viscosity modifiers [1][2][3].
amount of viscosity modifiers or carrying material Furthermore, because the human tongue is capable of
needed. detecting differences in particle size as small as 3 µm,
larger particles (larger than 30 µm) feel gritty in the mouth,
Additional parameters of interest when formulating making homogeneous particle sizes within a formulation
food powders are the crystalline phases, crystallite desirable [3].
size, and percent amorphous content ... An in-
depth understanding of these parameters enables The samples described herein are couverture chocolate
precise control over macroscopic properties such powder, milk chocolate powder and agglomerated
as the texture or mouthfeel of food products. chocolate powder as well as the most common additives
X-ray diffraction (XRD) can be used to identify milk powder and sugar.
and characterize these parameters – leading to
optimized processes and improved final products.

1.1 PARTICLE SIZE ANALYSIS OF VARIOUS

FOOD POWDERS
Particle size is an essential parameter when it comes to
developing and optimizing food powder formulations.
It also has further influence down the value chain in
process steps such as transport and storage. The main
method used to determine particle size and particle size
distributions of food powders is laser diffraction. The
size of the particle and the angle of the diffracted light
are inversely proportional. In other words, the angle of
diffracted light decreases when the particle size increases.
The resulting pattern of this analysis is used to gather
information on how to adjust formulations based on
particle size.
Figure 1: Particle size analysis of chocolate powders

4
As shown in Figure 1, all analyzed chocolate powders Particle analysis of sugar
have a different particle size distribution (PSD). Couverture Sugars in various forms are needed to fulfill different
and milk chocolate have bimodal size distributions with purposes. Examples are caster sugar and powdered
diameters ranging from 10 μm to 30 μm. The particle sugar, both produced by pulverizing and milling down to a
diameter of agglomerated chocolate is 300 µm on desired particle size. The close monitoring of particle size
average. during sugar manufacturing is therefore essential.

The table below illustrates the differences in particle size of

granulated and caster sugar.

SUGAR TYPE D10 (μm) D50 (μm) D90 (μm) SPAN

GRANULATED 878 ± 29 1113 ± 33 1525 ± 69 0.58 ± 0.03

CASTER 400.4 ± 20 680.6 ± 19 1083 ± 31 1.00 ± 0.06

Table 1: D10, D50 and D90 values of granulated sugar and caster sugar

The span of granulated sugar measured at a very low

value of 0.58, indicative of a very narrow, monomodal
dispersion. This suggests that the crystallization process
used for production was well controlled and produced
sugar crystals that were very homogeneous in size. The
span for caster sugar was significantly higher (1.00) and
points to a broader size distribution, suggesting that the
method used to break down sugar crystals into smaller
Figure 2: Particle size analysis of chocolate additives particles during production also introduced some level of
heterogeneity.
PSD was also measured for the most common chocolate
additives, milk powder and sugar. In Figure 2 the PSD for
these two samples is shown, with measurement returning
average diameters of 40 μm for sugar and 70 μm for milk
powder. Even though milk powder is ground during the
manufacturing process, it is still apparent that adding
it shifts the PSD of chocolate powder towards larger
diameters compared with the (milk-free) couverture
powder.

5
Particle analysis of coffee INFANT (I) AND TODDLER (T) FORMULA ( VALUES IN µm)

The particle size of ground coffee significantly influences

D10 D50 D90
the taste and has to be adapted to the brewing method.
Espresso, for instance, uses a fine coffee powder, while I 72 189 402
VENTURI
filter brewing or French press preparations use higher T 48 130 315
particle sizes. Also, very fine, outlier particles release
I 501 765 1193
unwanted bitter flavors and should be avoided. Hence, a FREE-FALL
homogeneous size distribution is desirable. For industrially T 478 746 1222
ground coffee this means that the particle size has to be
continuously monitored. Table 2: Summary of D-volume weighted data of laser diffraction for the infant (I)
and toddler (T) formula

The different size of primary particles measured in Venturi

can be directly correlated with the reconstitution and
dissolution velocity of the milk powder. The infant formula
has bigger primary particles which mean a lower surface
area than the toddler formula sample. The bigger particles
further suggest higher porosity for the infant formula.
For this reason, the infant formula reconstitutes faster in
water. Moreover, the flowability is also better than that of
the toddler milk because of the bigger agglomerate size
measured in free-fall.

INSTRUMENTS SUITABLE FOR THESE MEASUREMENTS

Figure 3: Representative volume-weighted particle size distribution of espresso PSA Series
coffee powder (grey curve) and of filter coffee powder (red curve)

Figure 3 compares the particle size distribution of an 1.2 X-RAY DIFFRACTION TO IDENTIFY
espresso powder with that of a filter coffee sample. The CRYSTALLINE PHASES IN FOOD POWDERS
espresso powder sample has a particle size below 1 mm, Sugars are commonly used powder ingredients in food
with a main peak at 600 µm. The particle size of coffee manufacturing that come in various forms. Since each type
powder used for filter coffee is much higher, with a main of sugar has a different crystal structure, sugars can easily
peak at 900 µm and a significant fraction above 1 mm. be differentiated from each other using X-ray diffraction
(XRD). XRD can be used to investigate the crystallization
The particle size distribution for both samples appears of amorphous sugars – a process that is often undesirable
homogeneous, and the apparent lack of very fine particles due to accompanying detrimental property changes,
suggests that the samples are of good quality. or for quantification of the crystalline and amorphous
components present in a powder mixture.
Particle analysis of milk powder
Different requirements apply to milk powder for infants and In the following analysis, XRD patterns of pure sugars
toddlers. Infant formula should ensure better flowability and of some sugar-containing finished food products
and faster reconstitution in water. Particle size is again the were recorded using a powder X-ray diffractometer. The
parameter of interest when optimizing these properties. crystalline sugars in the food products were then identified
from the measured diffractograms. Four pure sugars,
The upcoming measurements were conducted with two three different types of household sugar and six randomly
different dispersion modes, Venturi and free-fall. selected sugar-containing products were ground to serve
as sample materials for this study.

For further information on experimental details please read

through the comprehensive application report: Identifying
Sugars in Food Products Using X-ray Diffraction

6
Figure 4: XRD measurements of four different pure sugars. Figure 5: Diffractograms of different household sugars compared with the
diffraction pattern of pure sucrose.
Figure 4 compares the measured diffraction patterns of
pure sucrose, lactose, glucose and fructose samples. However, some small additional peaks can be found in
The different crystal structures of the four sugars result the diffractogram of preserving sugar, in particular when
in completely different diffractograms. Like for many plotting the intensities with a log scale (Figure 6). These
organic samples, the first Bragg peaks occur at small can be ascribed to pectin, which usually accounts for 1 %
scattering angles – for sucrose, lactose and glucose even to 2 % of preserving sugar, while the remaining content
at 2θ values < 10°. This emphasizes the need for a low is sucrose. This highlights the potential of XRD to identify
background at small 2θ angles. For larger 2θ angles (in trace phases in a material; this is made easier due to the
particular for 2θ > 45°), strong peak overlap occurs even low measurement background observed in the measured
for these pure, single-phase samples due to the complex data presented here.
crystal structures of the samples. Thus, the low 2θ range
is of most interest when investigating sugar-containing
samples using XRD.

For a comparison of the three types of household sugars,

the diffractograms magnified to the most relevant 2θ range
are shown in Figure 5. At first view, all three diffractograms
represent the diffractogram of pure sucrose.

Figure 6: Two magnified parts of the diffractograms showing additional peaks from
pectin in preserving sugar (red arrows)

7
Figure 7 compares the diffractograms of sucrose and is mainly caused by amorphous or weakly crystalline starch
dextrose to those of some sugar-containing food products. and oil for the banana chips, while it is mainly caused by
glucose syrup for the candy. Also, for both the banana
chips and the candy, all Bragg peaks in the diffractograms
can be ascribed to sucrose, indicating sucrose as the
main crystalline component. Small peak shifts between the
sucrose peaks of the different food product samples may
be caused by different moisture contents of the sugars.

INSTRUMENTS SUITABLE FOR THESE MEASUREMENTS

XRDynamic 500

Figure 7: Diffractograms of sugar-containing food products compared to the

diffraction patterns of pure sucrose and dextrose. Vertical lines indicate the main
Bragg peak positions of sucrose (red) and dextrose (black)

The diffractograms of ice-cream powder and instant tea

show sucrose as their main component. In both products,
significant amounts of dextrose are also observed. For
sponge cake biscuits, all observed Bragg peaks can be
ascribed to sucrose. However, the absolute sucrose peak
intensities are much lower than for pure sucrose, indicating
that major phases other than crystalline sucrose are also
present. Since the main components have an amorphous
structure, they do not produce Bragg peaks, but instead a
very wide hump of intensity is visible in the diffractogram.
This is also true for the banana chips and the candy. A
comparison to the list of ingredients shows that the hump

8
2 Transportation and
Powder Flow Rheology

Powder rheology deals with characterizing powder 2.1 RECOGNITION OF CHANGES IN POWDER
flow behavior under realistic conditions. The FLOW PROPERTIES
combination of two powder cells – powder flow Fluidization is a process were a granular material is
cell (PFC) and powder shear cell (PSC) – opens converted from a solid-like state into a dynamic fluid-like
up the possibility of applying static and dynamic state by introducing pressurized gas through the powder
measurement methods to simulate various bed. Considering different production steps, fluidization
manufacturing and storage processes. The flow can be found, for example, in fluidized bed reactors,
behavior of a powder is determined by a multitude pneumatic transport, and also during silo discharge when
of adhesive and repulsive forces, which depend on the particles are in free fall.
internal and external influences. Internal influences
include, for example, particle size, size distribution The powder flow cell helps to characterize the behavior
and density, and also factors such as surface of powders in the fluidized state, and during deaeration.
texture, surface area and porosity. External factors This so-called deaeration process occurs after the powder
comprise moisture, temperature, gas throughput has been fluidized and begins to release the trapped air
and degree of consolidation, among others. The without further compaction. In this way, it is possible to
flowability of the powder is therefore a non- simulate real life applications like pneumatic conveying,
inherent material property. Due to the multitude and and to identify de-mixing tendencies of particle blends.
complexity of the influencing factors, a theoretical
prediction of the powder behavior is difficult and The following sections provide an overview of different
requires experimental characterization. methods that can be applied to study and characterize
different flow behaviors of food powders.

Cohesion strength
Cohesion strength describes the internal resistance of a
powder to flow based on the adhesive forces between
particles. The test involves an initial fluidization followed
by a deaeration process. This aeration step is used as
sample preparation and enables operator-independent
measurements and erasing of the powder’s memory.
Due to the high repeatability and sensitivity of the test
method, even small changes in the powder bed can be
monitored. The ideal gas flow for fluidizing the powder can
Figure 8: True powder rheology methods be determined with the pressure drop test. The measuring
principle is based on a constant rotation of a two-blade
stirrer and measurement of the resulting torque. The
cohesion strength is a relative value calculated from the
measured torque and a calibration factor.

9
Some food powders, such as coffee creamer, are Determination of the wall friction angle is performed by
transported and dosed by pneumatic conveying. Here, moving a measuring system equipped with a disc over
the pressure drop method and cohesion strength the compressed bulk material. Infant formula and skim
measurement can provide important information to milk powder were tested with two different wall materials,
optimize the individual process steps and avoid incorrect namely stainless steel and polytetrafluoroethylene (PTFE,
dosing and problems during transport. Figure 9 displays Teflon®). The samples are compressed with a normal
the results of cohesion strength measurements of two stress of 3 kPa, 6 kPa and 9 kPa and the disc is rotated
different coffee creamer samples in double determination. at a constant speed on the surface of the compressed
The results show that the visually indistinguishable powder bed. As a result, the shear stress between the
samples exhibit significant differences in their flowability. wall material and the powder bed surface is measured.
The lower torque and the resulting lower cohesion strength The recorded torque is displayed for both milk powder
of coffee cream A indicates lower internal friction (or lower formulations at 9 kPa and the PTFE wall material in
bonding strength) between the particles. Higher cohesive Figure 10. From the torque signal it can be seen that the
forces were found for coffee creamer B, which can cause interaction of skim milk powder with PTFE is significantly
poorer flowability and potential problems during transport higher.
and dosing. Table 3 shows the cohesion strength value of
the two coffee creamers with the deviation obtained in the
double determination.

Figure 9: Cohesion strength results of two coffee creamer samples containing the
same ingredients. Figure 10: Results of wall friction for infant formula and skim milk powder at 9 kPa
and PTFE wall material.

MEAN COHESION STRENGTH

SAMPLE The characteristic wall shear stress for each applied
± STANDARD DEVIATION [Pa]
normal stress is plotted on a shear stress - normal stress
COFFEE CREAMER A 146 ± 1.2
diagram. The line passing through the pairs of normal
COFFEE CREAMER B 174 ± 1.2 stress and wall shear stress marks the wall yield locus. The
Table 3: Cohesion strength results ± standard deviation of the two coffee creamer wall yield locus is defined as the yield limit and specifies
samples obtained by averaging the last 20 data points of the cohesion strength the shear stress required to move the bulk material
curve. continuously across the wall surface. The mean wall
friction angle results from the trend line of the data points
Wall friction running through the origin. An example of the wall yield
Wall friction describes the friction between a bulk material point and wall friction angle plot is shown in Figure 11.
and a solid surface. The wall friction angle is not only As a general rule, the greater the wall friction angle, the
important for the design of silos, but also for the design greater the wall friction.
of chutes and other equipment where the bulk solid flows
over a solid surface. Influencing parameters are not only
the roughness and cleanliness of the wall material, but
also the material itself. Therefore, it is of great importance
to adapt the test conditions to the real-life conditions
to which the powder is subjected. In this context, the
influence of the wall material on two different milk samples
is presented.

10
 2.2. INVESTIGATION OF POWDER FLOW
BEHAVIOR AS A FUNCTION OF EXTERNAL
INFLUENCING PARAMETERS SUCH AS
RELATIVE HUMIDITY

Compressibility
Compressibility is a measure of the relative change in
volume that a sample undergoes when pressure is applied.
The term compressibility thus refers to the increase in
bulk density with increasing consolidation stress. Factors
influencing compressibility are particle size and shape,
and also water content and temperature. In this example,
the influence of moisture on the compressibility of flour is
shown in Figure 12.

Figure 11: Exemplary plot of the wall yield locus and the mean wall friction angle.

Table 4 shows the calculated mean wall friction angles

for the two milk powders, using stainless steel and PTFE
as wall material. While the wall material has only a minor
influence on infant formula, skimmed milk powder shows
a significant increase in wall friction with stainless steel
walls compared to PTFE. This indicates that PTFE-coated
containers are much better suited for the storage and Figure 12: Compressibility of flour at ambient conditions (dark grey) and after
processing of skim milk powder than stainless steel ones. conditioning the samples in the climate chamber at 35 °C and 95% RH for 1 h
(black), 2 h (red) and 24 h (light grey).

STAINLESS
STEEL [°]
PTFE [°] An increase in the water content in the flour sample leads
to a general decrease in the achievable bulk density
INFANT FORMULA 25 ± 0.2 22 ± 1.8
during compaction. Thus, the longer the flour was
SKIM MILK POWDER 57 ± 0.0 25 ± 0.8 exposed to moisture, the higher the porosity was due
Table 4: Results of mean wall friction angle for infant formula and skim milk powder to granulation and the increase in particle size. From the
with stainless steel and PTFE wall material. compression behavior, the flowability of the powder can
be calculated using the Carr index and the Hausner ratio.
INSTRUMENTS SUITABLE FOR THESE MEASUREMENTS The relationship between compression and flowability is as
MCR Evolution Series follows: The more a powder bed can be compressed, the
Powder flow cell (Fluidization only with PFC) worse its flowability.

This simple compression test can be used, for example,

to avoid ratholing and arching in silos or hoppers and also
load studies on walls and feeders can be performed.

Warren Spring cohesion

Warren-Spring cohesion is a method for directly measuring
the cohesion strength of non-fluidizable powders, such as
cohesive or very cohesive powders with the powder flow
cell.

The test procedure involves an initial compression of the

powder bed with a defined normal stress (3 kPa, 6 kPa
or 9 kPa). After removing the vertical load, a vane paddle
(Warren-Spring geometry) is lowered into the bulk material
until the upper edges of the vanes are leveled with the
surface of the bulk material. In a final step, the Warren-

11
Spring geometry begins to shear the compressed bulk test results show that exposing the flour to high relative
material by rotating at a constant speed of 0.1 rpm and humidity values for a short period of time (1 and 2 h) does
the resulting torque (M) is recorded. The Warren-Spring not significantly change the flow behavior. However, if
cohesion (SWS) is calculated according to Equation 1. the exposure time is increased to 24 hours, a significant
increase in cohesion strength is observed. This undesirable
and uncontrolled agglomeration of powders is called
"caking" and is one of the main problems during transport
and storage of powders containing salt or sugar. The
caking effect can not only cause problems during the
processing of the powder, but also affect the quality of the
Equation 1: Calculation of Warren-Spring cohesion. (R0 and Rl are defined as the final product.
outer and inner diameter of the Warren-Spring geometry)
Yield locus and time yield locus
The yield point of a consolidated bulk solid is called the
The resulting curve in Figure 13 shows the Warren-Spring yield locus function and indicates the boundary between
cohesion at the curve maximum where the consolidated "solid" and "liquid" behavior at a well-defined consolidation
powder fails and begins to flow due to the applied shear state. More information on the test procedure can be
stress. found in the application report “Introduction to Powder
Rheology”.

The powder shear cell can be used together with a

convection temperature device and a humidity generator
to condition and measure the sample under controlled
environmental conditions without the need for an additional
climate chamber. The change in flowability is observed via
an initial reference measurement and subsequent tests
after application of defined humidity and temperature
levels over a defined period of time. The effect of caking
based on humidity was observed here on a protein
Figure 13: Warren-Spring cohesion measurements of flour in triplet determination powder (Figure 15). During the test, the temperature was
at 3 kPa consolidation stress (pre-treatment: sample drying at 90 °C overnight). kept constant at 40 °C and a relative humidity of 18% RH
was selected. The protein powder was conditioned in the
The increase in cohesion strength due to water adsorption convection temperature oven for 24 h and the change of
can be studied with Warren-Spring measurements after flow behavior was monitored.
the powder has been exposed to different environmental
conditions in a climate chamber. For this purpose, the
flour was preconditioned at a relative humidity of 95% RH
and a temperature of 35 °C for different periods of time
(Figure 14).

Figure 14: Warren-Spring cohesion of flour after 0 h, 1 h, 2 h and 24 h in the

climate chamber at 95% RH and 35 °C.
Figure 15: Yield locus function (black; before sample conditioning) and time yield
The increased water content in the flour sample promotes locus at 6 kPa pre-shear (red; after exposure to 18% RH and 40 °C for 24 h) of a
the formation of capillary bridges between the particles protein powder.
and thus an increased cohesion strength value. The

12
The unconfined yield strength of a powder is obtained by To determine what environmental conditions the powder
drawing a Mohr circle through the origin and tangential to can be exposed to until the caking effect inhibits the
the yield locus function. The higher the point of intersection flow of the powder, several tests were carried out
on the x-axis, the higher the normal stress required to with increasing relative humidity. During the test, the
deform or "break" the powder as a function of the major temperature and the exposure time were kept constant
principal stress σ1 (consolidation stress). This means that compared to the previous test and only the humidity was
a powder will flow if the force acting on the powder is increased step by step. At the point where σc exceedes
greater than the unconstrained yield strength, and σc is σ1, the powder loses its flowability. Figure 16 shows that
therefore a measure of the flowability. From the relationship the protein sample starts to clump when a water activity of
between the major principle stress and the unconfined more than 0.25 is reached.
yield strength, the coefficient of flowability (ffc =σ1/σc) can
be determined. The time consolidation test results with
variable humidity are shown for the protein powder in
Table 5.

REFERENCE SHEAR SHEAR

MEASUREMENT MEASUREMENT
COEFFICIENT (BEFORE TIME (AFTER TIME
CONSOLIDATION CONSOLIDATION
STEP) STEP)

COHESION T C 786 Pa 1115 Pa

UNCONFINED YIELD
STRENGTH σ C
2782 Pa 4038 Pa

MAJOR PRINCIPLE
STRESS σ 1
9680 Pa

COEFFICIENT OF Figure 16: Evolution of time consolidation unconfined yield strength with increasing
FLOWABILITY ff c
3.48 2.40
water activity/humidity level in the temperature chamber.
Table 5: Coefficients derived from the protein powder yield locus analysis before
and after the time consolidation step (sample conditioning at 18% RH and 40 °C INSTRUMENTS SUITABLE FOR THESE MEASUREMENTS
for 24 h). MCR Evolution Series
Powder flow cell
The test shows that when the powder is exposed Powder shear cell with CTD 180 and humidity generator
to moisture, a significant increase in the yield locus
function and unconfined yield strength is observed and
consequently higher forces are required to "break" the
powder bed.

13
3 Packaging and Storage
of Food Powders

Environmental conditions, such as temperature and Measurement data and results

humidity, and mechanical forces, including gravity, Four samples of ground coffee were added to 250 mL
exert influence on how a powder behaves. graduated cylinders (readable to 2 mL) to around two-
thirds of their volumes. The weight of each was recorded.
In this unit, different measurements with Before documenting the untapped volume (bulk density),
specific purposes are proposed for food powder each coffee was shaken and visually inspected to ensure it
characterization: density and oxidation stability. had no discernable air pockets in its uncompacted state.
These measurements enable producers to optimize The ground coffee sample in the cylinder was then placed
the powder’s packaging process and storage and secured on the tapping head of the Autotap. Volumes
conditions to ensure product quality at all times. were recorded after 10, 500, and 1,250 taps. An additional
1,250 taps were used to check for any observable change
in volume.
3.1 TAPPED AND TRUE DENSITY OF FOOD
POWDERS The final results are outlined in Table 6, which clearly
Fine powders and granular materials are widely used shows that the tapped densities of the different types
in industrial processes in a variety of applications. of ground coffees increase by around 0.04 g/ml. In
The performance of the final product depends on the Image 1.2, the four analyzed ground coffees are shown
properties of the individual powdered components that in a plot of volume versus number of taps. The differently
make up the formulation. Morphology, cohesive strength, roasted coffees exhibit similar trends with similar values.
and the powder’s tapped or true density are some of the The blonde roast is the slight outlier with significantly
properties that are used in formulation optimization and higher bulk and tapped density values. Bulk and tapped
contribute to efficient packaging and transportation of density, the compressibility index, and the Hausner ratio
the final blend. Therefore, they have become standard are calculated following the formulas below.
techniques for product development. Tapped density
analysis offers the simplicity of characterization and
provides an insight into a powder’s cohesiveness and Equation 1 – Bulk density (g/mL):
m
flowability. This value is obtained by mechanically tapping where: m = weight of the sample (g)
Vi
a volumetric vessel or a graduated cylinder containing a Vi = initial volume of the sample (mL)
known amount of sample a fixed distance until no visible
change in its volume is observed.
Equation 2 – Tapped density (g/mL):
m
The material’s compressibility index and Hausner ratio can where: m = weight of the sample (g)
Vf
then be calculated. Free-flowing powders generally show Vf = final volume of the sample (mL)
little difference between the bulk and tapped densities.

Determination of a material’s true density begins with an Equation 3 – (Vi - Vf)

· 100
application of Archimedes’ principle of displacement. Carr’s Compressibility index (%): Vi
Because some samples interact with the usual where: Vi = initial volume of the sample (mL)
displacement fluid (water), gases such as helium or Vf = final volume of the sample (mL)
nitrogen are substituted. Boyle’s gas law is then applied to
ascertain a material’s true volume. The results of the two
processes are used to calculate the true density, which Equation 4 – Hausner ratio (g/mL):
Vi
can be used to directly assess the chemical composition where: Vi = initial volume of the sample (mL)
Vf
and morphology of a material in a quality control step. Vf = final volume of the sample (mL)

14
 COFFEE
BULK TAPPED COMPRESS­ HAUSNER Interpretation of results
DENSITY DENSITY IBILITY RATIO
ROASTS
(g/mL) (g/mL) INDEX (CI) % (HR) Figure 17 shows how volume decreases as the number
of taps increases. The initial volume of the same mass
DARK 0.33 0.37 12.6 1.14
of coffee is larger for dark coffee than blonde. This can
MEDIUM 0.31 0.35 13.4 1.14 be attributed to reduced exposure to heat, causing more
BLONDE 0.36 0.42 13.7 1.16 volatiles (moisture) to be retained in the coffee bean.
DECAF
DARK
0.30 0.35 12.9 1.15 Results show that the compressibility indices are
approximately 13 % and Hausner ratios are near to 1.15.
Table 6: Bulk & tapped density of coffee roasts These ground coffees exhibit good flow characteristics
according to the flowability scale (Table 7).

Conclusion
Food powder manufacturers can use the information
gleaned by tapped and skeletal density measurement
to optimize packaging and storage processes. Knowing
a material’s compressibility index and Hausner ratio can
influence container design, transport requirements, and
storage necessities.

INSTRUMENTS SUITABLE FOR THESE MEASUREMENTS

Autotap Series
Ultrapyc Series

Figure 17: Volume versus number of taps

FLOW
HAUSNER RATIO (-) CARR INDEX (%)
CHARACTER

1-1.11 10 Excellent

1.12-1.18 11-15 Good

1.19-1.25 16-20 Fair

1.26-1.34 21-25 Passable

1.35-1.45 26-31 Poor

1.46-1.59 32-37 Very poor

>1.60 >38 Very, very poor

Table 7: Scale of flowability according to Hausner ratio and the Carr index

15
3.2 OXIDATION STABILITY OF FOOD POWDERS
Food powders in the form of final product or as an
ingredient typically have a long shelf life, however it
depends on their physical and chemical properties as
well as on the packaging and storage conditions. A
conventional test method for analyzing the oxidation
stability of powder is e.g., the sensory analysis or the
determination of the peroxide value after a certain storage
time. Compared to these test methods the RapidOxy 100
provides an easy, fast, and safe determination of oxidation
and storage stability without any sample preparation.
Figure 18: Pressure drop of the two measurement runs
Measurement data and results
In contrast to the sensory analysis or the investigation Interpretation of results
of the peroxide value, the RapidOxy 100 determines As the results show in Table 9 and Figure 18, the oxidation
the oxidation stability in a fully automatic manner. The stability decreases from sample 1 to sample 4. Sample 1
measurement proceeds under accelerated conditions by indicates the highest oxidation stability because the lowest
increasing the temperature and the exposure to excess of pressure drop is observed whereas sample 4 indicates
pure oxygen. The sample in the test chamber is set under the lowest oxidation stability because the highest pressure
pressure with pure oxygen and heated up. During the drop is observed. Furthermore, the standard deviation of
measurement the temperature is kept strictly constant and each run is calculated to evaluate the quality of the test
the pressure is continuously traced. Due to the oxygen results. The small standard deviations show the measured
consumption the pressure drops accordingly. Since the test results are reliable so that different packaging, and
consumption of oxygen by a powder is a rather slow storing conditions can be evaluated.
process, the measurement is stopped after a defined time
(e.g. 20 hours). The pressure drop is sample-specific. Conclusion
The greater the amount of oxygen consumed within the Measurement of oxidation stability of food powders
set time, the less oxidatively stable is the powder. The without sample preparation is repeatable and reliable
pressure drop can simply be compared to other samples using the proposed method in order to identify the most
to investigate different batches, formulations or packages. appropriate packaging and storage conditions. Packing
The higher the pressure drop the lower is the oxidation and materials can also be evaluated as well as the shelf life that
storage stability. results from the usage under specific conditions.

A test of corn flour under the conditions below shows the INSTRUMENTS SUITABLE FOR THESE MEASUREMENTS
following data: RapidOxy 100

PARAMETER SETTING

PROGRAM Temperature-sensitive sample

TEST TEMPERATURE 60 °C

FILLING PRESSURE 700 kPA

TEST DURATION 1200 min

Table 8: Test conditions

PRESSURE PRESSURE
DROP [%] DROP [%] STANDARD REPEAT­
SAMPLE
AFTER AFTER DEVIATION ABILITY
NO.
20H: 20H: [%] [%]
RUN 1 RUN 2

1 0.7 0.6 0.05 15.4

2 1.2 1.1 0.05 8.7

3 1.7 1.8 0.05 5.7

4 2.4 2.3 0.05 4.3

Table 9: Oxidiation stability results

16
4 Final Product Analysis
and Customer Experience

One of the most critical aspects of food powder of the milk powders, low values of the BET C constant
development is ensuring that the final product is (4.14 and 7.05) were consistent with similar organic
safe and enjoyable for the consumer. When opening compositions that display weak adsorbate-adsorbent
a food powder package, there should not be any interactions.
visible clumps or moisture and the powder should
readily dissolve or mix into water or with other
ingredients. Thus, the surface area and pore size of
the final formulation must be optimized to ensure
that the final product is stable and dissolves quickly.
Additionally, along with surface area, the viscosity
of suspended or dissolved powders should be
analyzed to ensure that the product mouthfeel for
the consumer is pleasant and neither too gritty nor
too viscous. Finally, food powder products must be
tested for the presence of heavy metal and trace
element contamination to ensure that the final
product is safe for consumption.
Figure 19: Kr adsorption isotherms at 77 K for toddler (black circles) and infant
(red triangles) formula.
4.1 DISSOLUTION RATE OF FOOD POWDERS
The overall surface area and pore size of a food powder These results show clear particle size and morphologic
significantly affect its dissolution rate. Both surface area differences between the samples, leading to the
and pore size are typically measured by gas sorption conclusion that the toddler formula has a higher solubility
analysis. overall, but is prone to form clump during dissolution due
to its low permeability. This is corroborated subjectively
Surface area of milk powders through their behavior in the subsequent preparation steps
Once the solvent reaches the single particles of the in the following liquid analyses.
powder, the surface area is critical, because it defines
the area available for the interaction between the solvent INSTRUMENTS SUITABLE FOR THESE MEASUREMENTS
and the solute particles. The surface area is a function Nova Series
of particle size and shape, can differentiate porosity from
the bulk sample, and can be measured using vacuum
volumetric methods. This technique measures the amount
of an adsorbate (e.g. gas or vapor) adsorbed onto the solid
surface of an adsorbent (e.g. milk powder) at a defined
absolute temperature and pressure. Measurements of the
gas or vapor uptake amount versus pressure at a constant
temperature is known as the adsorption isotherm. This
isotherm is used to determine the accessible surface area
by applying the Brunauer Emmett Teller (BET) method.

The calculated BET-accessible surface area values for

the experimental Kr adsorption isotherm (Figure 19) were
0.041 m2/g and 0.074 m2/g for infant and toddler milk
powder formula, respectively. With the low surface areas

17
Permeability of milk powders The dependence on compression (Figure 20) shows the
Permeability is determined by how well the solvent (in this vulnerability of some powders to compaction. It can be
case water) is able to access the individual particles of the expected that the infant formula will be more likely to
powder. The higher the permeability, the more accessible produce clots after prolonged storage compared to fresh
is the sample matter. infant formula. However, the toddler formula shows worse
dissolution behavior irrespective of applied stress and thus
This parameter was measured using the combination of an will exhibit clotting either way. This was also observed
Anton Paar rheometer and a powder flow cell, by pumping subjectively in the dissolution steps.
a defined air flow across the particle bed at a fixed
pressure gradient. This indicates how much access the
water has to the product which influences the process of
PERMEABILITY PERMEABILITY PERMEABILITY
dissolution. A product with high permeability in this sense [10 -12 m²] AT [10 -12 m²] AT [10 -12 m²] AT
SAMPLE
prevents the undesired formation of knots and nodules 3 kPa CONSOL­ 6 kPa CONSOL­ 9 kPa CONSOL­
IDATION IDATION IDATION
of undissolved powder while dissolving. These lumps
of undissolved powder are the result of a barrier layer INFANT 19.8 18.1 17.4
forming when water is taken up within mostly secondary TODDLER 9.8 9.1 8.5
agglomerates, which slows down the process of
dissolution. Since formula should be prepared quickly, this Table 10: Results of the permeability measurements
is highly undesirable, making this an important parameter
in regards to the quality of the product. INSTRUMENT SUITABLE FOR THESE MEASUREMENTS
MCR Evolution Series
Figure 20 and Table 10 show the permeability results, Powder flow & shear cell
representing the powders’ air flow resistances under
different compaction forces. The infant formula is not only
notably more permeable, it is also much more dependent Vapor sorption
on the compaction, showing a significant change. Water vapor sorption is a property or phenomenon
related to a powder’s ability or propensity to absorb water
molecules from the atmosphere. Producing materials in
large quantities and shipping them to distributers for sale
can involve long storage times with significant water vapor
absorption, which producers must ensure does not affect
the substance’s quality. Appropriate packaging is essential
to avoid influences from outside environmental conditions.
But before the product is packaged into its final wrapping,
it has already interacted with the environment. In addition,
the customer may not use the whole product at once, but
rather store it after opening.

An especially influential environmental factor for powder

Figure 20: Permeability – toddler formula (black to gray curves) and infant formula properties is the relative humidity. It varies at different
(red curves) measured at compressions of 3 kPa, 6 kPa and 9 kPa (from darkest geographic locations and between different buildings and
to lightest) outdoors.

Generally, the permeability decreased with increasing Furthermore, the shelf life of materials such as milk
normal stress during compression, and the infant formula powders can be influenced by both relative humidity and
showed significantly higher permeability (by a factor of temperature.
more than two) than the toddler formula. In itself, this could
be an indication of higher particle size diversity. However, Determining the amount of water adsorbed into a material
this could also be a function of chemical composition. A such as milk powder can be measured using a static
higher amount of carbohydrates in the composition (as is volumetric vapor sorption analyzer. This type of instrument
the case with the toddler formula) would naturally change can provide specific fixed or variable temperatures and
the morphology of the particles, in this case leading to less relative humidities (RH) that mimic storage conditions
free volume and therefore lower permeability. and reveal how much water uptake or release occurs
throughout a specific time period. The vapor sorption
experiments below were carried out on dry milk powder
samples at 95% RH at temperatures of 25 °C, 35 °C,
and 45 °C. With increased exposure time to 95% RH, the

18
sample mass increased. The mass change in percent is 4.2 VISCOSITY AND MOUTHFEEL OF FOOD
depicted in Table 11. POWDERS
The final infant/toddler milk needs to meet various criteria
concerning quality. Apart from nutritional aspects, quality
TIME MILK POWDER MASS CHANGE is further reflected in the texture and stability of the milk.
24 h 21.72 % (25 °C) 24.72 % (35 °C) 24.78 % (45 °C) Additionally, its flow behavior when being filled into a
bottle and especially when it is sucked out of the bottle
by the child is of great importance when judging the
TEMPERATURE MASS INCREASE IN % experience and effort needed to draw the liquid. This, in
turn, is dependent on the particulates present within the
25 °C 24
dissolved formula which can change according to the
35 °C 24.72 nutritional needs of the child. The liquid’s flow through
45 °C 24.78 the bottle into the child’s mouth, as well as the intensity
of sucking required, differs depending on the viscosity
Table 11: Milk powders’ % mass change at 95 % relative humidity at given tem- and flow behavior of the milk product. The viscosities at
peratures shear rates which are representative of the milk flowing out
of the small hole in the feeding bottle provide important
information. Furthermore, viscosity in general plays a role
in the formula’s texture and its dispersion stability.
All samples increased by 20 % to 25 % of their original
mass after 24 hours of exposure to 95% RH at different The methods for characterization of powder and liquid
temperatures. Higher uptake amounts were achieved dispersion presented in this report will guide users to
with higher temperature, suggesting that storage of milk describe the characteristics of milk powder and its final
powders at lower temperatures reduces their likelihood of milk product. The flow curves in Figure 22 reveal different
adsorbing excess moisture. flow behavior for the two liquid milk samples. Infant milk
showed only slight shear-thinning flow behavior while the
toddler milk was significantly shear-thinning (more than an
order of magnitude decline in viscosity).

Further, the absolute viscosity values of the toddler milk

were consistently higher than those of the infant milk.

Figure 21: Water vapor adsorption isotherms of milk powders at 25 °C

Figure 22: Flow curve of infant milk (red) and toddler milk (black) at 37 °C
The full water sorption isotherms of the infant and toddler
formulas were measured at 25 °C and are shown in
Figure 21. Clear differences are seen between the two
formulas with the toddler formula adsorbing more water at
higher RH. In addition, the infant formula isotherm shows
an unusual step in the adsorption branch starting between
50% RH – 60% RH that is most probably related to a
lactose phase transition, confirming that the two formulas
have different compositions.

INSTRUMENT SUITABLE FOR THESE MEASUREMENTS

VSTAR Series

19
The almost Newtonian flow behavior of the infant milk can
be explained by the uniform particulate size distribution
in the solution. The highly shear-thinning behavior of the
toddler milk is likely due to the insoluble carbohydrate
ingredients like maltodextrin in the milk powder.

Considering the geometry of a baby bottle, the tip of the

nipple is the most sensitive part where most of the shear
rate is applied.

Considering the high shear rate applied, designing formula

to be shear-thinning (advertently or inadvertently) is a
prudent decision. Also considering the stronger muscular
development of toddlers versus infants, a higher viscosity
overall might be desirable as well.

INSTRUMENT SUITABLE FOR THESE MEASUREMENTS

ViscoQC Series
MCR Evolution Series

20
4.3 FOOD SAFETY
Acid digestion of food powders to prepare samples
prior to ICP-MS testing for metal contamination
Industrially produced food products and their primary
agricultural products are amongst the best-characterized
and continuously monitored substances of daily life.
Because of the impact of food quality on human health,
chemical analysis is required by law in most countries.
Trace element analysis, e.g., for toxic heavy metals like
lead, arsenic, cadmium, or mercury, is a routine task in
industrial and governmental food testing labs.

In order to demonstrate the excellent suitability of

Multiwave 7101/7301/7501 for sample preparation of
food and other organic samples prior to element analysis
the recovery rates of certified reference materials were
determined. The described conditions can be used as a
starting point for different kinds of organic samples.

Approximately 0.5 g of the sample were multiply weighed

into the 18 mL quartz and PTFE-TFM vials.

The vials were put into Rack 18 and 1 mL of H2O and

4 mL of conc. HNO3 (65 %) were added. After closing the
vials with the plug-on caps the rack was put into the liner
already filled with load solution (150 mL of water and 5 mL
of conc. HNO3). Table 12: NIST1566b, Results and recovery rates, n=15 Quartz:10, TFM:5

In two consecutive runs (one with quartz vials only and the
other one mixed with quartz and PTFE-TFM vials) the liner The applied digestion method is not only suitable for
was put into the Pressurized Digestion Cavity (PDC) and the digestion of the mentioned reference materials
the digestion program was started. After cooling, 1 mL of (spinach leaves and oyster tissue) but also serves as a
conc. HCl was added for stabilization of Hg. Subsequently representative starting point for any kind of organic sample,
the samples were transferred into 50 mL tubes, filled up whereas relevant parameters such as sample weight, time
and analyzed. Prior to measurement the solutions were and temperature might be adapted accordingly.
diluted 1 to 10 with distilled water.
INSTRUMENT SUITABLE FOR THIS SAMPLE PREPARATION
The measured values are well-comparable with the Multiwave 5000
certified values and the results were similar when the Multiwave GO Plus
digestions were performed in either quartz or in PTFE-TFM Multiwave 7101/7301/7501
vessels.

21
5 Anton Paar Solutions
MCR Evolution Rheometer Series Nova Series Autotap Series
The MCR Evolution series is the result These multi-station surface area These one- and two-station tapped
of consistent thinking and rethinking, and pore size analyzers provide density analyzers for powders,
of continuous development based operational simplicity and velocity granules, and small pellets are
on decades of experience, and of across the entire analysis process. automated devices that comply with
the feedback of more than 10,000 Containing four degassing stations various internationally recognized
satisfied customers. The combination and up to four analysis stations, standards. They provide high-level
of innovative and thousandfold field- this instrument delivers four five- test method control with a user-
proven technology with the modular point BETs in 20 mins, with 2 % selectable, lockable number of taps.
design represents the benchmark reproducibility. A large range of sample sizes can
in its class. With 200+ accessories, be accommodated with different
the MCR Evolution rheometer series Find out more: graduated cylinders.
gives you endless possibilities www.anton-paar.com/eb-food-nova

for rheological investigations and Find out more:

material characterization. www.anton-paar.com/eb-food-autotap
Ultrapyc Series
Find out more: Ultrapyc gas pycnometers measure
www.anton-paar.com/eb-food-mcr the true and skeletal density of XRDynamic 500
solids to track their purity and This automated multipurpose
porosity. Measurements take powder X-Ray diffractometer drives
Powder Shear and Flow Cell less than 10 minutes, so they are unbeatable XRD data quality with
The two cells for true powder perfect to control the quality of maximum efficiency. It is a versatile
rheology help you to really your solid materials throughout platform covering a wide variety of
characterize and understand your the manufacturing process. The applications with optimal solutions
powders. A wide range of dedicated PowderProtect mode enables for powder XRD, non-ambient XRD,
powder measurement methods is measurements of fine powders PDF analysis, SAXS, and more.
available putting the advantages of without instrument contamination and Intuitive to use, with fully automated
rheometers to use: fast and easy- the built-in Peltier temperature control optics and alignment routines, it
to-perform tests but also elaborate ensures superior thermal stability with allows everyone, from novices to
measurements for both quality no external temperature control bath experts, to collect top-quality XRD
control and R&D purposes. required. data quickly while minimizing errors.
XRDynamic 500: Driving XRD.
The powder shear cell is ideal for Find out more:
determining the flow behavior of www.anton-paar.com/eb-food-ultrapyc Find out more:
consolidated powders and their www.anton-paar.com/
eb-food-xrdynamic-500
time-dependent behavior. Additional
accessories provide full control over
temperature and humidity.

The powder flow cell is an innovative

and scientific approach to powder
characterization offering a wide range
of test methods. Powder behavior
can be characterized under various
processing conditions: simulating,
adjusting, and optimizing, e.g.,
manufacturing processes.

Find out more:

www.anton-paar.com/eb-food-rheology

22
Multiwave 7101/7301/7501 Multiwave GO Plus ViscoQC Series
The Multiwave 7101/7301/7501 The Multiwave GO Plus microwave ViscoQC rotational viscometers
series delivers the next level of digestion system with the patented ensure the quality of substances –
performance, working at up to Directed Multimode Cavity (DMC) from liquid to semi-solid. Eliminate the
300 °C and up to 199 bar. This provides the best of both monomode risk of measurement errors and free
ensures complete digestions of all and multimode microwaves. The up time and budget with the simplest
kinds of samples, such as food, microwave field adapts itself to the spindle exchange mechanism,
environmental, polymer, cosmetic, number of filled or empty positions automatic spindle detection,
pharmaceutical, geological, chemical, and the filling state of the vessel – automatic speed searching function
and petrochemical samples, even that’s truly innovative. Due to the for new formulations, and more. All of
in the same run. With a range of TURBO cooling process, unique these features have been developed
accessories, consumables, and cooling times as short as eight to make the operator’s life easier.
racks of up to 28 positions, sample minutes for a fully loaded twelve-
preparation has never been easier. position rotor are possible (for EPA Find out more:
methods). www.anton-paar.com/eb-food-viscoqc

Find out more:

www.anton-paar.com/­ Find out more:
eb-food-multiwave-series www.anton-paar.com/ VSTAR Series
eb-food-multiwave-go-plus
The VSTAR system goes beyond
basic water sorption to provide
Multiwave 5000 vapor and gas sorption analyses
This microwave digestion platform RapidOxy 100 over a broad range of analysis
provides digestion of a broad array Fully-automatic measurements 8x conditions. Based on the fast and
of samples (varying in difficulty or faster than other accelerated aging high-resolution vacuum-volumetric
volume), acid leaching, solvent methods, at temperature ranges of gas sorption technique, VSTAR can
extraction, evaporation, microwave- up to 180 °C. Easy cleaning in less deliver analysis results in roughly
induced O2 combustion, sample than 5 min. RapidOxy 100 is the only half the time required by classical
drying, and synthesis. Furthermore, Rapid Small-Scale Oxidation Test DVS methods. Wide chemical
it comes with a comprehensive, (RSSOT) on the market. Another compatibility allows you to measure
interactive method library, a bonus: the small 5 mL / 4 g sample adsorption/desorption isotherms and
customizable, intuitive user interface, size max. – especially helpful kinetics of many species (organics,
and modern sensor technology, when costly samples are being alcohols, amines, and more).
together with easy-to-handle investigated.
compact rotors. Find out more:
Find out more: www.anton-paar.com/eb-food-vstar

Find out more: www.anton-paar.com/eb-food-rapidoxy-100

www.anton-paar.com/
eb-food-multiwave-5000
PSA Series
With the laser diffraction technology
of the PSA series, you can determine
the particle size and particle size
distribution of both liquid dispersions
and dry powders from the nanometer
up to the millimeter range. Since
these two parameters have an
impact on processability as well as
the properties of the final product,
understanding them is essential for
product development and quality
control.

Find out more:

www.anton-paar.com/eb-food-psa

23
24
References
[1] Beckett S. T. (2001). Milling, mixing
and tempering – an engineering view of
chocolate. Journal of Process Mechanical
Engineering 215:1-8.

[2] Liang B. & R. W. Hartel (2004). Effect

of milk powders in milk chocolate. Journal
of Dairy Science 87:20-31.

[3] Afoakwa E. O., A. Paterson & M.

Fowler (2008). Relationship between
rheological, textural and melting
properties of dark chocolate as
influenced by particle size distribution and
composition. European Food Research
and Technology 227:1215-1223.

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 © 2023 Anton Paar GmbH | All rights reserved.
Specifications subject to change without notice.
XPAIA136EN-B

www.anton-paar.com