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u www.tugraz.at
Determination of Latex and Starch
Penetration via Serial Sectioning in
Combination with Fluorescence
Micro...
Presentation Overview
 Binder Penetration/Migration
 Establishment of a New Method to Analyze Binder
Penetration
 Seria...
Binder Penetration/Migration
17.11.2015
EFPRO European Paper Week 2015
3
Binder migration
 Binder follows the evaporated
...
Establishment of a New Method to analyze
Binder Penetration
 Starch
 Reactive staining with 5-([4,6-Dichlorotriazin-2-
y...
Establishment of a New Method to analyze
Binder Penetration
17.11.2015
EFPRO European Paper Week 2015
5
Staining the
binde...
Establishment of a New Method to analyze
Binder Penetration
17.11.2015
EFPRO European Paper Week 2015
6
Staining the
binde...
Establishment of a New Method to analyze
Binder Penetration
17.11.2015
EFPRO European Paper Week 2015
7
Staining the
binde...
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
Sta...
The Influence of Base Paper Properties on
Latex Penetration
17.11.2015
EFPRO European Paper Week 2015
10
0,0
5,0
10,0
15,0...
The Influence of Solids Content on Starch
Penetration
17.11.2015
EFPRO European Paper Week 2015
11
Recipe [%] ST 70 ST 60
...
Double staining to localize Latex and Starch
17.11.2015
EFPRO European Paper Week 2015
12
Latex Latex + Starch Starch
Evaluation of SSFM via CLSM
17.11.2015
EFPRO European Paper Week 2015
13
R² = 0,8755
0
5
10
15
20
25
30
35
40
45
50
0 5 10...
Conclusion and Outlook
 SSFM is an appropriate method to localize the binder after
the coating process
 3D-data evaluati...
17.11.2015
EFPRO European Paper Week 2015
15
Thank you for your attention!
Contact:
Karin Hofer
University assistant
Insti...
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Determination of Latex and Starch Penetration via Serial Sectioning in Combination with Fluorescence Microscopy

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By Karin Hofer, Technical University of Graz. This was presented during the New Ideas for the Paper Industry: Young Researchers' Presentations session, organised as part of European Paper Week 2015. More at http://www.cepi.org/epw

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Determination of Latex and Starch Penetration via Serial Sectioning in Combination with Fluorescence Microscopy

  1. 1. u www.tugraz.at 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
  2. 2. 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 17.11.2015 EFPRO European Paper Week 2015 2
  3. 3. Binder Penetration/Migration 17.11.2015 EFPRO European Paper Week 2015 3 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
  4. 4. 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 17.11.2015 EFPRO European Paper Week 2015 4 Staining the binder Coating Embedding Image Processing 3D Data Calculations Serial Sectioning Staining the binder Fluorescein Dichlorotriazin Reactive group Covalent bond 8mm 25mm
  5. 5. Establishment of a New Method to analyze Binder Penetration 17.11.2015 EFPRO European Paper Week 2015 5 Staining the binder Coating Embedding Serial Sectioning Image Processing 3D Data Calculations Paper sampleMicroscope view Cutting process Filter cubes Lenses 10/20/50x Diamond knife Microscope unit Microtome unit Rotary microtome Sample holder Serial Sectioning
  6. 6. Establishment of a New Method to analyze Binder Penetration 17.11.2015 EFPRO European Paper Week 2015 6 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
  7. 7. Establishment of a New Method to analyze Binder Penetration 17.11.2015 EFPRO European Paper Week 2015 7 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
  8. 8. u www.tugraz.at RESULTS 8
  9. 9. 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 17.11.2015 EFPRO European Paper Week 2015 9 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
  10. 10. The Influence of Base Paper Properties on Latex Penetration 17.11.2015 EFPRO European Paper Week 2015 10 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 Penetrationdepth[µm] Coat weight [g/m²] Base Paper A Base Paper B Base Paper C Base Paper D 0 5 10 15 20 25 30 35 0,010,1110 incrementalspecificintrusion[µl/g] pore diameter [µm] 2000rpm PFI 6000rpm PFI 2000rpm PFI + filler 2000rpm PFI calendered Results of SSFM Mercury Porosimetry base paper
  11. 11. The Influence of Solids Content on Starch Penetration 17.11.2015 EFPRO European Paper Week 2015 11 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 lowshearviscosityBF100[mPas] Penetration depth [µm] Blade Sumet ST 70 ST 60 ST 60 Depletion of starch at the coating surface
  12. 12. Double staining to localize Latex and Starch 17.11.2015 EFPRO European Paper Week 2015 12 Latex Latex + Starch Starch
  13. 13. Evaluation of SSFM via CLSM 17.11.2015 EFPRO European Paper Week 2015 13 R² = 0,8755 0 5 10 15 20 25 30 35 40 45 50 0 5 10 15 20 25 30 35 40 45 CLSMPenetrationdepth[µm] SSFM Penetration depth [µm]
  14. 14. 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 17.11.2015 EFPRO European Paper Week 2015 14
  15. 15. 17.11.2015 EFPRO European Paper Week 2015 15 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: karin.hofer@tugraz.at Web: www.ipz.tugraz.at Thanks for the support of…

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