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Fig. 1.

1
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

1.

Dispersity of particulate systems,


1.1 About rocks, gravel, lumps, nuggets, corn, particles, nanoparticles and
colloids
1.2 Particle characterisation - Granulometry,
1.3 Particle size distributions,
1.4 Physical particle properties

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.1

Fig. 1.2
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Size Scale of Polydisperse (Material) Particle Systems


10-10
o

1A

10-9

10-8

10-7

10-6

1 nm

10-5

10-4

1 m

10-3

10-2

1 mm

10-1

1 cm

1
1m

visual ability of human eye


wave length of visible light:
X-rays and electron interferences

ultramicroscope

light microscope

electron microscope
capacitive und inductive sensors
dispersity

molecular-disperse

pore dispersity

microporous

dispersed
elements
one-dimensional
two-dimensional

molecules

colloiddisperse

mesoporous

high-disperse,
ultra-fine

fine-disperse

coarse-disperse

macroporous

makromolecules,
colloids

ultra-fines

fines

surface coatings, liquid films, membranes


chains of macromolecules, needles, fibres, threads

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.2

medium grain

coarse

Fig. 1.3
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering
Blatt 2

Mixtures of Polydisperse (Material) Particle Systems

dispersant

10-10
disperse
phase 1 Ao

10-9

10-8

10-7

1 nm

gas gas mixture


liquid
solid
transition l-g

10-6

10-5

1 m

10-4

10-3
1 mm

10-2
1 cm

gas

liquid

solid

gas
liquid
solid
gas
liquid
solid

aerosol, fog
aerosol, smoke
foam

solution, lyosol,
hydrosol

bubble system
micro-emulsion
emulsion
suspension
xerogel, porous membrane
rigid-foam insulation
gel
liquid filled, porous solid material
mixed crystal, solid solution, s-s alloy

monodisperse = uniform-sized elements

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.3

10-1

1
1m

Fig. 1.4
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Size Scale and Properties of Nanoparticles


Bioavailability
Quantum effects
Strongly developed
surface effects

109
0,001

0,01

0,1

106 m
1 m

10

100

1000 nm

Polymers
Proteins
Metal powders
Virus, DNS
Ceramic powders
Tobacco smoke
Atmospheric
aerosols
Nanoparticles for
life sciences
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.4

Fig. 1.5
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Expression of the Particle Size


characte- Eq./sketch
ristic size
breadth: b b + 1 b + l + t b 1 / 3
, ,
,
3
2
length: l
t
1/ 2
thickness: t
3
2lb + 2bt + 2lt
1/ l + 1/ b

, lb ,

equivalent diameter d, for b l t


equivalent length l, for rods l >> b t
equivalent area b l , for chips, plates
b l >> t
(4) equivalent mass s b l t , for extreme
shaped clusters:
(1)
(2)
(3)

Feret
diameter
Martin
diameter
sieve
diameter
volume V
equivalent
diameter
area A
equivalent
diameter
surface area
AS equiv.
diameter
physical
feature
equivalent
diameter

a1

A = A1 + A 2
1
(a 1 + a 2 ) or a 1a 2
2

a2

equivalent volume diameter


3

equivalent projection area


diameter 4A /
equivalent surface area diameter
specific surface diameter V / A S

AS /

Stokes diameter
v s 18
( s f ) a

aerodynamic diameter

vs
da =

image analysis d0
geometric anal. d0
geometric anal. d0
mass balancing d3
image analysis,
number basis d0
image analysis,
number basis d0
sieving, mass or
volume basis d3
Coulter counter
electrical method,
number basis d0
light extinction,
number basis d0

6V/

d St =

measuring method,
quantity r = 0...3
r = 0 number basis
r = 1 length
r = 2 area
r = 3 volume basis

v s 18
a

equivalent
light-scattering
diameter
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

light extinction,
number basis d0
gravitational, centrifugal sedimentation
and impactor, mass
basis d3
sedimentation, mass
or volume basis d3
low angle laser lightscattering method,
number basis d0
Figure 1.5

Fig. 1.6
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Characterisation of Granulometric Properties of


Disperse Material Systems
Characterisation of particle size distributions

direction of measurement

1. Particle size characteristics by


image analysis

2. Particle size distribution function


(cumulative distribution curve)

1
Qr(d)
dM

dS

0,5
Qr(d2)

dF

Qr(d)
d

Qr(d1)
0

dF FERET chord length


dM MARTIN chord length
dS maximum chord length

dmin

d1 d2

dmax
d

4. Example of measured particle size distribution


3. Frequency distribution of particle size
(distribution density curve)

qr(d) q (d) = dQr(d)


r
d(d)

Mode dh

du

di

di-1

di+1

particle size
fraction
di-1 ... di
in mm
- 0.16
0.16 ... 0.63
0.63 ... 1.25
1.25 ... 2.5
2.5 ... 5.0
5.0 ... 6.3
6.3 ... 10
10
... 16
d0
16
... 20
+ 20
d

mass
in kg
0.180
0.648
0.919
1.920
3.021
1.084
1.748
0.761
0.232
0.054

mass
cumulative
fraction
fraction
Q3(di)-Q3(di-1) Q3(d) in%
in %
1.7
1.7
7.8
6.1
16.5
8.7
34.6
18.1
63.2
28.6
73.5
10.3
90.1
16.6
97.3
7.2
99.5
2.2
100.0
0.5

10.567

100.0

5. Particle size distribution function Q3(d) and frequency distribution of particle size q3(d) of
the above example 4.
0.20

a)

b)

Q3(d) in %

80

q3(d) in mm-1

100
Qr(d*<di)

60
40

qr(d) Qr(di) - Qr(di-1)


di - di-1

0.15

0.1
dm,i =

di-1 + di
2

0.05

20
Median d50
0
0

12

16

20

Particle size d in mm

0
0

8
12
16
particle size d in mm

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

20

Figure 1.6

Fig. 1.7
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Typical frequency distributions and cumulative probability distributions


Normal Distribution (GAUSSIAN Distribution):
q r (x ) =

1
2

Q r (x ) =

1 x 2
exp

2

(1)

1 t 2
exp 2 dt

2 < 1

qr(x)

(2)

normalizes :
Q r (x ) =

1
2

t2
exp
2 dt

(3)

Qr(x50) = 0,5

with
u=

x x 50

(4 )

x 84 x 16
2

x16

(5)

xh = x50

x84

Mode xh = x50 Median

Four - Parameter Log - Normal Distribution:


1
1
q r (x ) =
exp
ln x 2
2

ln x ln x 50

ln

(6)

qr(x)
0.3
ln x50 = 1, ln = 1

Q r (x ) =

ln

1
2

1 ln t ln x
1
50
exp
t
ln
2

x=

d d min
d max
d max d

u=

ln x ln x 50
ln

(7)
dt

(8)

for d min d d max

(9 )

ln =

x
1
ln 84
2
x 16

0.2
ln x50 = 3, ln = 3
0.1

ln x50 = 3, ln = 1

(10)
0

10

15

WEIBULL Distribution:
for xmin = 0 and x* = x63 = 1

q r (x ) =

x x min

x x min

x x min

n 1

xx
min
exp
x
x


min

qr(x)

2.0

n = 5.5

n = 0.5

n=3

(11)

xx
min
Q r (x ) = 1 exp
x
x

min

for xmin = 0 and n = 1 follows the


Exponential Distribution if = 1
x63
Q(x) = 1 - exp(-x)

n=2
(12) 1.0

n=1

(13)

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.7

Fig. 1.8
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Graphical characterisation of selected particle size distributions


6. Three - parameter logarithmic
normal distribution (L) with upper
limit do and transformation (T)

97
90
Qr(d)

L
T

50

transformed
distribution

10
5
1
0.20
0.02
1

99.9

99,9
95

60
40

98
96
90
80
60
40

full-logarithmic net

3 - parameter
distribution

20
10
5
1
0.5

20
10
6

5 10
5
d50 do
d or
16 50 84

2 3

1 2 3 50

RRSB-net

full-logarithmic -net

log - normal
net

10

0.5
100
10-1
10-2

10

101
100
10-1

102
101
100

104
103
102

103
102
101

particle size d in m
1 Log-Normal distribution
2 RRSB-distribution
3 GGS-distribution

8. RRSB - distribution in a double - logarithmic diagram

cumulative distribution Q3(d) in %

10

7.0 7.5 8 9

AS,V,K d63 in m3/ m3

15

20

25 30
40

4.0 3.5 3.0 2.5 2.0 1.8 1.6 1.4 1.3 1.2 1.1 1.0
0.9

99.9
99
95
90

x
0.8

x
x

63.2
50

0.7

0.6

x
0.5

60
80
100
120
150
200
300
500
1000
2000
5000
10000

x
0.4

10

x
0.3
0.2

x
1

0.1

0.5
10-3

10-2

Pol -1
10

RRSB - net

99.9
99.5
cumulative distribution Q(d) in %

99.90
99.50

7. Comparison of particle size distribution functions


in a full-logarithmic, RRSB and log - normal
diagram (net)

0
100

101

102

particle size d in mm
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.8

Fig. 1.9
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Statistical Moments of Particle Size Distributions


Complete k-th Moment of Particle Size Distribution Qr(d*<d) related to Quantity r:

( d d * ) q r (d ) d (d ) =

do

du

du

do

M k, r =
d*

( d d * ) dQ r (d ) d m,r ,i d
k

i=1

r ,i

(1)

First Initial Moment (k = 1, d* = 0) or Expected Value


do

do

du

du

M 1, r = d m,r = d q r (d ) d (d ) =

d dQ (d ) d
r

i =1

m , r ,i

r ,i

(2)

Central Moment related to expectation (mean) dm,r


do

d m, r

M k , r = Z k ,r = (d d m,r ) k q r (d ) d (d )

(3)

du

Second Central Moment or Variance


do

do

du

i =1

Z 2 ,r = = (d d m,r ) q r (d ) d (d ) = (d d m,r ) 2 dQ r (d ) (d m,r ,i d m,r ) 2 r ,i


2
r

du

(4)

Variance according to Satz von Steiner


N

2r = Z 2 ,r = M 2 ,r M 12,,r d 2m,r ,i r ,i d 2m,r

(5)

i=1

Incomplete k-th Initial Moment du...d, i...n and Complete Initial Moment du...do, i...n...N
d

do

d q r (d ) d (d ) d m,r ,i r ,i
k

i=1

du

d q r (d ) d (d ) d km,r ,i r ,i

(6)

(7)

i =1

du

Conversion from given quantity r to a searched quantity t of Frequency Distribution


d t r q r (d )
M t r ,r

q t (d ) =

(8)

and Cumulative Distribution


d

Q t (d ) =

M t r ,r
M t r ,r

du
do

du
do

du

d t r q r (d ) d (d )

tr

q r (d ) d (d )

du

tr
m , r ,i

tr
m , r ,i

i =1
N
i =1

r ,i

(9)
r ,i

Conversion of cumulative distributions from number to mass basis or from mass to number
basis
d

Q 3 (d ) =

d q 0 (d ) d (d )

du
do

q 0 (d ) d (d )

du

i =1
N

d
i =1

3
m , 0 ,i

0 ,i

(10)
3
m , 0 ,i

0 ,i

Q 0 (d ) =

d 3 q 3 (d ) d (d )

du
do

q 3 (d ) d (d )

du

3
m , 3 ,i

3
m , 3 ,i

i =1
N
i =1

3 ,i

(11)
3 ,i

Conversion of k-th complete initial moment of a known quantity r in a searched quantity t


M k ,t =

M k + t r ,r
M t r ,r

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

(12)
Figure 1.9

Fig. 1.10
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Cumulative Particle Size Distribution, Mass and Number Basis


d

dU

i =1

mass basis: Q 3 (d ) = q 3 (d ) d(d ) 3,i

Verteilungsfunktion Q3(d) in %

100
90
80
70

Masseverteilung

60
50
40
30
20
10
0

0.5

10
50
100
Partikelgre in m

number basis: Q 0 (d ) =

3
d q 3 ( d ) d( d )

du
do

q 3 ( d ) d( d )

du

i =1

500

1000

3
m ,i

3 ,i

d
i =1

1000

3 ,i

d
N

500

3
m ,i

Verteilungsfunktion Q0(d) in %

100
90
80
70

Anzahlverteilung

60
50
40
30
20
10
0
0.5

10

50

100

Partikelgre in m
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.10

Fig. 1.11
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Multi-modal Frequency Distribution


1.8

frequency distribution q*(log d)

1.6
1.4

subcollective 1

1.2
1.0

subcollective 2

0.8
0.6 subcollective 3
0.4
0.2
0

1.0
10.0
particle size d in mm

0.1

SC,k(t) mass fraction of the k-th

total frequency distribution:

q3,tot (d, t) = SC,k q3,k d, do,k , d50,k , ln,k


k =1

subcollective (subpopulation)
q3,k

truncated log-normal distribution:


q3,k (d) =

do,k d
2 ln,k do,k

u2
exp
2
d

do,k

do,k d50,k
1 do,k d

ln
ln
u=

ln,k do,k d
do,k d50,k

d(log d)

median particle size of the


distribution function

ln,k

standard deviation of the


k-th subcollective

normalisation:
=

upper limit of the particle size


of the k-th subcollective

d50,k

dQ 3 (log d)

frequency distribution
of the k-th subcollective

with

q*3,tot

100.0

Q 3 (log d)

=
log d

3,i

total number of subcollectives

d
log i
di1

1
lim SC ,k Q 3,k [d, d o ,k , d 50,k , ln,k ] =
N
2
k =1

u2
exp 2 d(d) = Q3,tot (d, t )
u

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.11

Fig. 1.12
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Mass Fraction Related to the Number of Stressing Events


discrete mass balance model:

d sc ,1
n

d sc ,3
n

= S n ,1 sc ,1

= S n ,3,1 sc ,1 + S n ,3, 2 sc , 2

k =1

sc , k

=1

number of stressing events

Sk,j

kinetic constants for mass transfer from j to k subcollective

measured
3
model

mass fraction sc,k


1,0
0,8
0,6
0,4

0,2
2

0,0

k-th subcollective

3 4
2
3
0 1
number of stressing events n

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.12

Fig. 1.13
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Application of Image Analysis to Characterise Particle Size


1. Image of Microscope by CCD-camera
directlight

transmitted
light

direct-light

transmitted
light
particle

pixel number

2. Definition of Threshold Value

Definition of grey tone limits


for particle detection in a 8-bit
grey tone image
3. Conversion of Grey Tone Image in a
Binary Image (Binarisation)

grey tone distribution

(black)

255
(wite)

Binary image means: which


pixel of original image is shown
by 0 (black) or by 255 (white)
4. Classification of Particles
dF,ma

min. and maximum Feret diameter


equivalent circle diameter
d = 2 A/ ,
shape factor U = 4

dF,mi
dequ

A
U2

U = circumference, A = projection
area

Presentation of Particle Size Fractions


in a Colour Code
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.13

Fig. 1.14
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Principle of Laser Light Diffraction


large diffraction for particle size d wavelength, small diffraction for d >>
sample cell
lense system

Fourier
lense

detector
r

laser

f
focal distance

principle of laser light diffractometer

computer

light diffraction pattern


Fourier lense

radial light intensity


distribution at detector

I tot =

d max

tot

detector

q 0 (d ) I( r , d i ) d (d )

d min

particle size distribution

frequency distribution q3 in 1/mm

Intensity I

cumulative distribution Q3 in %

prinziple of Fourier lense


particle size distribution

100

50

particle size

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.14

Fig. 1.15
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

In-Line Particle Size Analysis (Sympatec)


feed opening
particle loaded air stream
inductive sensor

drive for rotating


sampling device

on-line sampling

dispersion air

laser beam

detector with
sensor array

low-angle laser
light-scattering
instrument
(LALLS)
d = 0.5 1750
m
nozzle and
sample cell

isokinetic sampling device for a split particle stream:


rotating sector
moving pipe
d

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.15

Fig. 1.16
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

In-Line Particle Size Analysis (Malvern)


isokinetic sampling

particle
stream
laser

Injektion nozzle

particle
feed back

detector

pressurized air

monitoring of size ranges:

0.5 - 200 m
1.0 - 400 m
2.25 - 850 m

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.16

Fig. 1.17
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Principle of Photon Correlation Spectrometer (PCS)


in suspensions at rest: light scattering at dispersed particles, that oscillate by Brownian
molecular motion

Laser

Optik

Probenbehlter

Korrelator

Photomultiplier
Optische Einheit

autocorrelation function RI,I()

intensity of scattered light

Determination of intensity time function of scattered light (reasons: interferences,


change of particle number concentration within the charac-teristic volume element)
and calculation of autocorrelation function:

fine particle
coarse particle

retardation time

time t

Autocorrelation function (Dp particle diffusion coefficient, K scattered light vector,


- retardation time)
T

R I, I () = lim I( t ) I( t + ) dt = e
T

2 D p K 2

kB T
d
=
with
3 Dp

EINSTEIN equation (d particle size, kB BOLTZMANN constant, T absolute


temperature, - dynamic viscosity)
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.17

Fig. 1.18
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering
page 1

1. Physical Principle
Laser diffraction technique is based on the phenominon that particles scatter light
in all directions (backscattering and diffraction) with an intensity that is dependent
on particle size

2. Measurement setup
Using two laser beams with different wavelength (red and blue light) additional
information to particles smaller 0,2 m is obtained
red light setup

Detectors

large angle
forward angle

backscatter

Laser

Fourier lens

Sample chamber

- scattering light hits only forward angle detectors


- the angle of the deflected laser beam is inverse proportional to the particle size

Detectors

blue light setup

large angle
forward angle

backscatter

Laser

Fourier lens

Sample chamber

- blue light (wavelength 466 nm) leads to a scattering signal for small particles
(isotropic scattering pattern) which can be detected from large angle- and
backscatter- detectors
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.18

Fig. 1.19
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.19

Fig. 1.20
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Principle of Acoustic Attenuation Spectroscopy


Suspension
Level sensor

Stopper motor
and digital
encoder

HF Transmitter

HF Receiver

LF Transmitter

LF Receiver

Transducer
Positioning Table

Stirrer

Discharge

Control
module
Microwave
and
DSP module

during acoustic wave penetration, amplitude and intensity attenuation (damping) of


ultrasonic frequency spectrum (1 to 100 MHz) in high concentrated particle
suspensions with sizes d = 10 nm 1 mm
RF generator
RF detector
detection of attenuation (damping) spectrum
correlation between attenuation characteristics
x <<
entrainment
and particle size distribution (K = 2/
suspension wave number, k fluid wave number,
s particle volume concentration, i = 1...n
particle size fraction, ri particle radius, Ami
reflected compression wave coefficient, ARe real
contribution, m number of acoustic dispersion
coefficient):

3 n i s ,i
K
= 1 3 3 (2m + 1)A Re A mi
2 i=1 k ri m=0
k

x >>
scattering
measuring zone

particle size distribution

100

50

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

particle size
Figure 1.20

frequency distribution q3 in 1/mm

frequency

cumulative distribution Q3 in %

damping

Fig. 1.21
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Determination of Particle Size Distribution and Zeta-Potential using


Electroacoustic Effect - Electrokinetic Sonic Amplitude (ESA)
1. Physical Principle
Alternating electric field (frequency range 1 to 20 MHz) generates particle oscillations
at velocities that depend on their size and zeta potential (O' Brien- Theory)

acoustic signal (ESA) as response

ESA = A( ) s
A()
s

p
Z

Z E
p

calibration function
volume fraction of particles
suspension density difference
particle density
acoustic impedance (complex resistance)

electrophoretic mobility (E)

2. Measurement Setup

E = = 0 r

ESA-Signal
Processing
0
r
v
E

permittivity of vacuum
permittivity
particle velocity
electric field strength
viscosity

suspension

m = E (d , , s ) q(d )d (d )

3. Data Analysis
Particle motion in an electric field
E;v

d
s
q(d)

Tim e
applied electric field

particle velocity

measured dynamic mobility


zeta-potential
particle diameter
volume fraction of particles
particle size frequency distribution

Mobility Spectrum

m
dyn. mobility

phase lag

phase lag

adjusting q(d) and zeta-potential from


the measured mobility spectrum

frequency
Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.21

Fig. 1.22
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Particle Density Measurement by HELIUM-Pycnometer


Determination of porefree particle volume by gas pressure measurement in a doublechamber system by HELIUM gas (migration access of internal pores dPore > 0,1 nm)
probe chamber

pressure

feed valve

discharge valve

Helium
filter
prep./ test valve

V Exp

overpressure
valve
VProbe

5,

35

VCell

V Exp

150

V Exp

VCell 35,
VCell 150

Pressure measurement in probe chamber: (VCell VProbe)

p1

Pressure test in probe and expansion chamber: (VCell VProbe) + VExp

p2

Calculation of probe volume and solid density, pre-measurement of particle mass ms


by balance

VPr obe = VCell

VExp
p1 / p 2 1

and

s =

ms
VPr obe

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.22

Fig. 1.23
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Measurement of Particle Surface by Gas Adsorption according to


BRUNAUER, EMMET and TELLER
Physical adsorption of gas molecules at particle surfaces in multi-layers due to VAN
DER WAALS interaction
gas supply

vacuum

dosing
valve

adsorbed gasv olume Vg

standard vessel

desorption
adsorption

BET range

0
probe chamber

sorption isotherms

0.35

relative partial pressure of gas p/p0

adsorbed
dewar vessel
p0 - test chamber gas molecules
(adsorpt)

liquid nitrogen
N2 at T = 77 K
p0 = 101 kPa

adsorptiv
particle surface
(adsorbens)

BET- line, valid for: 0.05 < p/p0 < 0.3

p / p0
1
C BET 1
=
+
p / p0
Vg (1 p / p 0 ) Vg ,mono C BET Vg ,mono C BET

p / p0
Vg (1 p / p 0 )
b=

a=

(CBET 1)
Vg ,mo n o C BET

BET- constant:
H m H multi a + b
C BET = exp
=
R T
a

H m free molar adsorption enthalpy of


mono-layer
H multi molar bonding enthalpy of n
multi-layers
Hcondensation

1
Vg ,mono C BET

Adsorpt mono-layer coverage:


1
Vg ,mono =
a+b

Particle Surface:

A S = A M ,g N A Vg ,mono / Vm ,l
AM,g

relative gas pressure p / p 0

NA
Vm,l

cross-sectional area of adsorpt


molecule
AVOGADRO-number
molar volume of condensed adsorpt

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.23

Fig. 1.24
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering
z c

Regular Packing Structures

b
y

porosity , coordination number k

x
a
lattice type

primitive

basic facecentred

face-centred

space-centred

cubic
a=b=c
= = = 90

a0
a0 0,1nm k = 6

k = 12

k=8

monodisperse
sphere
packing
d = const.

= 0,4764

= 0,3955

hexagonal
a=b=c
= = 90
= 120

k = 12

sphere
packing

octahedron
vacancy

tetrahedron
vacancy

= 0,2595

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.24

Fig. 1.25
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.25

Fig. 1.26
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Stressing and Flow of Wet Particle Dispersions


particle in liquid dispersion (suspension)
diluted

concentrated

suspension
and particle
flow pattern y

dy

dy
du
= x
dy

vx

f (. )
normal stress

d
a

a
d

a
>1
d

a
0 < d < 0.2

particle
volume
fraction

s < 0.066

0.3 < s <


6

particle
friction

i = 0

i = 0

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

particle
separation

dy

f ()

s
a -3
s,0= (1+ d )

vx

ux

moist packing

ux

shear rate

cubical cell
packing
model

liquid in particle packing

liquid saturated

ux

flow function

paste

a
=0
d

a
contact

-0.01 <

contact
a
< 0 deformation
d

s,0 =

s >
6
S<1

i 0

i > 30

6
pore saturation S = 1

Figure 1.26

Fig. 1.27
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Sampling

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.27

Fig. 1.28
Prof. Dr. J. Tomas, chair of Mechanical Process Engineering

Fig_MPE_1 Mechanical Process Engineering - Particle Technology Disperse Systems Prof. Dr. J. Tomas 31.03.2014

Figure 1.28

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