Determination of Latex and Starch Penetration via Serial Sectioning in Combination with Fluorescence...
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Transcript of Determination of Latex and Starch Penetration via Serial Sectioning in Combination with Fluorescence...
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Determination of Latex and Starch
Penetration via Serial Sectioning in
Combination with Fluorescence
Microscopy
Karin Hofer1, Bernhard Seidl2, Martin Kozich2, Wolfgang Bauer1
17.11.2015
EFPRO European Paper Week 2015
1
1 Institute of Paper, Pulp and Fiber Technology, Graz University of Technology, AUSTRIA
2 Agrana Research and Innovation Center, Tulln, AUSTRIA
Presentation Overview
Binder Penetration/Migration
Establishment of a New Method to Analyze Binder
Penetration
Serial Sectioning in combination with Fluorescence Microscopy
(SSFM)
Results
The Influence of Base Paper Properties on Latex Penetration
The Influence of Solids Content on Starch Penetration
Double-staining to localize Starch and Latex
Evaluation of SSFM via CLSM
Conclusion and Outlook
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Binder Penetration/Migration
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Binder migration
Binder follows the evaporated
water phase to the surface
Binder penetration
Binder follows the water into the
paper substrate
Binder
2
1
Whalen-Shaw, 1993
Localization of Binder
after the Coating Process
Establishment of a New Method to analyze
Binder Penetration
Starch
Reactive staining with 5-([4,6-Dichlorotriazin-2-
yl]amino)fluorescein
Latex
Staining by adsorption into the latex particle
with Rhodamine B
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Staining the
binder
Coating
Embedding
Image
Processing
3D Data
Calculations
Serial
Sectioning
Staining the
binder
Fluorescein
Dichlorotriazin
Reactive group Covalent bond
8mm
25mm
Establishment of a New Method to analyze
Binder Penetration
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Staining the
binder
Coating
Embedding
Serial
Sectioning
Image
Processing
3D Data
Calculations
Paper sample Microscope view
Cutting process
Filter cubes
Lenses
10/20/50x
Diamond knife Microscope unit Microtome unit
Rotary microtome
Sample holder
Serial
Sectioning
Establishment of a New Method to analyze
Binder Penetration
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Staining the
binder
Coating
Embedding
Image
Processing
3D Data
Calculations
Serial
Sectioning
Output SSFM VIS
UV
Coating layer
thickness
Fluorescent layer
thickness
Binder
Penetration Depth
Establishment of a New Method to analyze
Binder Penetration
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Staining the
binder
Coating
Embedding
Serial
Sectioning
Image
Processing
3D Data
Calculations
Serial
Sectioning
Segmentation
3D data evaluation
Image
Processing
3D Data
Calculations
CD
ZD
MD
12µm
5,4mm
100 cuts
in MD
u www.tugraz.at
RESULTS
8
The Influence of Base Paper Properties on
Latex Penetration
Recipe [%] I II III
CaCO3 100 100 100
Latex stained 8 16 6
Starch 4
NaOH set pH to 8,5 set pH to 8,5 set pH to 8,5
Target solids
content
65 65 65
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Base paper type Pulp Refining Additive
A Eucalyptus bleached 2000 PFI -
B Eucalyptus bleached 6000 PFI -
C Eucalyptus bleached 2000 PFI 20% filler (CaCO3) + Retention agent
(Percol 8383)
D Eucalyptus bleached 2000 PFI Pre-Calendering – once each side per
sheet (2000daN, room temperature)
Coating Formulation
Base Paper Type
The Influence of Base Paper Properties on
Latex Penetration
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0,0
5,0
10,0
15,0
20,0
25,0
30,0
35,0
40,0
0,0 5,0 10,0 15,0 20,0
Pe
ne
tra
tio
n d
ep
th [
µm
]
Coat weight [g/m²]
Base Paper A Base Paper B Base Paper C Base Paper D0
5
10
15
20
25
30
35
0,010,1110
incre
me
nta
l s
pe
cif
ic in
tru
sio
n [
µl/
g]
pore diameter [µm] 2000rpm PFI 6000rpm PFI 2000rpm PFI
+ filler 2000rpm PFI
calendered
Results of SSFM
Mercury Porosimetry base paper
The Influence of Solids Content on Starch
Penetration
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Recipe [%] ST 70 ST 60
CaCO3 100 100
Latex 6 6
Starch 4 4
Thickener 0,1 0,1
NaOH set pH to 8,5 set pH to 8,5
Target solids content 70 60
Coating Formulation
0
200
400
600
800
1000
1200
1400
1600
1800
0 5 10 15 20 25 30 35
low
sh
ear
vis
co
sit
y B
F100 [
mP
as]
Penetration depth [µm]
Blade Sumet
ST 70
ST 60
ST 60
Depletion
of starch
at the
coating
surface
Double staining to localize Latex and Starch
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Latex Latex + Starch Starch
Evaluation of SSFM via CLSM
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R² = 0,8755
0
5
10
15
20
25
30
35
40
45
50
0 5 10 15 20 25 30 35 40 45
CL
SM
P
en
etr
ati
on
de
pth
[µ
m]
SSFM Penetration depth [µm]
Conclusion and Outlook
SSFM is an appropriate method to localize the binder after
the coating process
3D-data evaluation can be performed and a mean
penetration depth into the base paper can be calculated
Staining procedure for starch and latex (most common
coating binders) was developed
Good correlation with CLSM
Further influences on binder penetration can be tested
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Thank you for your attention!
Contact:
Karin Hofer
University assistant
Institute of Paper Pulp and Fibre Technology
Graz University of Technology
Inffeldgasse 23
8010 Graz/ Austria
Tel: +43 316 873 30756
Mail: [email protected]
Web: www.ipz.tugraz.at
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