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Disintegration of agglomerates in liquid
Gabrie M.H. MeestersErik M. Bosma, Merel OostveenJ. Ruud van OmmenSheila Khodadadi
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Introduction
Instant powders
Wetting behaviour
Dispersing behaviour
AIM: • Good instant properties• Rapid and complete reconstitution• No lump formation
Reducing the reconstitution time• Understanding the rehydration behaviour• What is the rate limiting step
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Powder rehydration
(Forny, Marabi et al. 2011)
(Fang, Selomulya et al. 2007)
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Wetting of powders
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Experimental
• Prepare powder beds by sieving & pressing
• Determine the bulk density
• Place droplet on powder bed
• Record time required to sink in
Drop penetration time method
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Results
• Current model assumes Drawing Area (DA) = Penetration Area (PA)
• Experiments show widening by factor 1.5
Model adaption – penetration area
DA
PA
DA
PA
Original model Adapted model I
Adaption I decreases difference theory / experiments by factor 2.3 (Kozeny Carman)
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Micro Computed Tomography
Potato starch ɛ=075
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Results
• Current model estimates pore size ~ 10-7 m
• Experimental pore size (micro CT) ~ 10-6 m
Model adaption – pore size
Original model Adapted model II
Adaption II decreases difference theory / experiments by factor 4.2 (Washburn)
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Results
• Corresponds well to model predictions
• Instant starch behaviour dominated by maltodextrin
(Maltodextrine & Instant starch)
Drop penetration time [s]
Weights [#] Corn starch Maltodextrin Instant starch
1 2.0 0.14 0.14
3 1.5 0.11 0.13
12 2.3 0.09 0.10
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Disintegration of powders
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Disintegration
Rehydration of formulated potato starch
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Disintegration
Rehydration of formulated potato starch
Static version
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Disintegration
Disintegration
“The dissolution of the solid bridges between the primary particles followed by dispersion of the primary particles within the
liquid volume”(Richard, Toubal et al. 2012)
A B C D
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Modelling the data
Various researchers have modelled dispersion as a first order process existing of either a single or multiple exponential terms 1
𝑦 = 𝐴 1 − exp −𝑘𝐴 ∗ 𝑡 + 𝐵 1 − exp −𝑘𝐵 ∗ 𝑡
These researchers measured a property which is linked to disintegration, like the change in:• Viscosity• Conductivity• Light back scattering
1 To, Mitchell, Hill, Bardon and Matthews - 1994
Kravtchenko, Renoir, Parker, Brigand – 1999
Larsen, Gåserød and Smidsrød – 2003
Galet, Vu, Oulahna and Fages - 2004
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Questions to answer
• How can we quantify the disintegration time?
• Can the existing models be used for consumer product?
• What dependency exist for the rate constant?
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Experimental setup
Two measurements methods are used during this project to describe disintegration
• Laser light diffraction• Measure the particle size distribution and follow this over time• Changes in the D90 reflect how the particles get smaller• Applicable to powders with good wetting properties
• Spectrophotometer• Measure the change in optical density over time• Other reconstitution effects are also measured
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Laser diffraction Introduction
• Reservoir is filled with water
• Powder is added to the top
• Powder is pumped around to the laser
• The laser light is scattered by the particles
• A particle size distribution (PSD) is sought that best fits the scatter pattern
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Laser diffractionPSD
A PSD is obtained over time, giving insight how the distribution is affected
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Laser diffractionPSD
A PSD is obtained over time, giving insight how the distribution is affected
Static version
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Laser diffractionD90
Following the D90 over time gives us insight into how fast a particle disintegrates
0
100
200
300
400
500
600
700
800
0 50 100 150 200 250 300
D9
0 [
µm
]
Time [sec]
Formulated Potato Starch
D90
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Laser diffractionResults
A higher temperature will lead to a higher rate constant and thereby also a faster disintegration time
0.00
0.04
0.08
0.12
0.16
0.20
0 5 10 15 20 25 30 35
Init
ial r
ate
co
nst
ant
[1/s
]
Temperature [°C]
Formulated potato starch
0.00
10.00
20.00
30.00
40.00
50.00
0 5 10 15 20 25 30 35
Dis
inte
grat
ion
tim
e [
1/s
]
Temperature [°C]
Formulated potato starch
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Photo-spectrometryObscuration
• Powder and a magnetic stirrer are added to a cuvet
• Water is added from the top
• Light is passed through the sample
• As the particles disintegrate they block more light
• If soluble components are present they disappear over time, letting more light pass
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Spectrophotometry
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SpectrophotometryIntroduction
0.0
0.2
0.4
0.6
0.8
1.0
1.2
0 20 40 60
Ab
sorb
ance
un
it [
-]
Time [sec]
Milk powder
• Peaks at the beginning are caused by the initial addition of the powder
• Disintegration follows a exponential function
• Variations in the final value are caused by different concentrations
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SpectrophotometryChanging temperature
0
25
50
75
100
125
150
0 20 40 60 80
Tim
e [
sec]
Temperature [°C]
Disintegration time
Cocoa powder - Nesquik
Cocoa powder - Benco
Coffee creamer
0.01
0.10
1.00
0 20 40 60 80
Tim
e [
sec]
Temperature [°C]
Rate constant
Cocoa powder - Nesquik
Cocoa powder - Benco
Milk powder
Same behaviour is observed as for laser diffraction
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The questions
• How can we quantify the disintegration time? Laser diffraction and photo-spectrometry seem to work
• Can the existing models be used for consumer product? Literature models that described dispersion/dissolution rate
can also be applied to describe the disintegration of different powders. TO BE PROVEN YET
• What dependency exist for the rate constant? Temperature effect on both measurement methods are in
agreement with each other and with literature 1
1 Larsen, Gåserød and Smidsrød – 2003
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Issues
• Difficult to study disintegration on its own, e.g. when wetting is already critical
• Determination of time constants for the four stages will tell us where to opimise our formulations
• Model description of disintegration still to be proven
• Sinkability also difficult to determine. Will be dealt with in next research