Dr. Christian E. BUTZKEEnology Professor
PURDUE UNIVERSITY
[email protected] (765) 49-46500 www.butzke.com
• Filtrosophy
• Filtration Systems• Pad/Cartridge/DE
• Membrane
• Cross Flow• Particle Filtration
• Reverse Osmosis
• Filterability Testing
1 µm 10 µm100 nm10 nm
10 µm10 µm
1 µm1 µm 100 nm100 nm
10 nm10 nmParticle Size
• No Un-Filtration
• No Routine Filtration
How to Unfilter?
Personal Philtration Preferences
Preferences
Parker
Laube
Dr. Dave
Kramer
1 µm
K100
.3 µm
EK
9 µm
K900
Pad Filtration
10 µm10 µm
1 µm1 µm 100 nm100 nm
10 nm10 nm
.45 µm.45 µm .2 µm.2 µm
Particle Size
Pad Filtration
Oxygen Pick-up ?
Pad Filtration
Pad Filtration
Pad Sanitation
w/out counter pressure!
With counter pressure!
Pad Sanitation
Filter Gauges & Sanitation
Proper Cork Storage
Proper (TCA-free) Storage
Pore Seize vs. Flow Rate
Modular Depth Filters
Stacked disks
Modular Depth Filters
Cartridge packs
EK Pre-filter plus Membrane
Diatomaceous Earth
”Diatomaceous Earth is a mineral filter aid mined from the fossilized silica shell remains of algae from the class
Bacillariaphyccae, better known as Diatoms“
Diatomaceous Earth
DE LayersDE Layers
Diatomaceous Earth
http://www.filtrox.ch
Diatomaceous Earth
DE/Rotary Drum Vacuum Filter
0.45µmMembrane Filtration
10 µm10 µm
1 µm1 µm 100 nm100 nm
10 nm10 nm
.45 µm.45 µm .2 µm.2 µm
Particle Size
Pad/DE vs. MembraneDepth Surface
Electron Microscope Image by Bill Plunkett @ Clarkson University
Membrane Filtration
Membrane Filtration
Electron Microscope Image by Bill Plunkett @ Clarkson University
Membrane Filtration
• Surface Filtration
• Perpendicular
• Removal of Microbes
• “0.2 - 1.2”µm Pores
• Integrity Tests
Membrane Filtration Setup
Sterile Filtration
1. Cellulose2. Membrane 1.20 µm3. Membrane 0.45 µm4. Cellulose
1.2.3.4.
Depth
Surface
perpendicular
• Mount• Integrity Test• Sterilize• Bottle• Re-Test
• flood membrane with water• pressurize to 80% with N2 gas• increase pressure by 2 psi/min• note pressure when bubbling starts• compare to filter specifications
Membrane Filtration
“Bubble Point”
Integrity Tests
• Bubble Point
• Forward Flow
• Pressure Hold
Membrane Filtration
Bubble Point Integrity Test
LiquidLiquid
GasGas
Bubble Point Integrity Test
• largest pore diameter
• pressure differential
• surface tension (Water vs. Wine!)
• membrane integrity • correct filter size• correct mounting• Note: 4 to 6 psi variation• NOT tested: sterility downstream
BubbleRelease
Result:
"steady stream of bubbles"
Membrane Pore Sizes
BubbleBubblePointPoint
pore size (pore size (µµm)m)smallestsmallest largestlargest
“.45 µm Nominal Pore Size”
http://www.lallemand.com
Mannoproteins
Pore vs. Protein Size
Mannoprotein Size: 0.003 - 0.135 µm (10 – 450 kDa)
Pore Size Sterile Filter: 0.450 µm
0.45 µm 0.130.13
Shriveled Bacteria?
Oenococus oeni: 1.0 µmPore Size Sterile Filter: 0.45 µm
0.45
O.oeni
O.oeni
0.45
0.45
“viable but non-culturable”
Always do your Bubble
Test !
Always do your Bubble
Test !
Sources of Re-Contamination
Winemaker
Filtered AirCorks
Corker Jaws
Hopper
Inert GasVacuum Line
ValvesGaskets
Conveyors
Filler Heads
Bottles
Filler Bowl
Vacuum Line
Condensate
Rinse Water
Hoses, Lines, Gauges
Millipore Corp. in PW&V 1989
Fouling
Filter Fouling
• Yeast/Bacteria Cells (alive or dead)
• Biofilm Formation (Polysaccharides)
• Colloidal Materials (Pectine, Protein etc.)
• Fining Agent Residue (Bentonite etc.)
“undesirable accumulation of materialson the surface of the filter ”
Cross Flow
Cross Flow
Cross Flow
Cross Flow
Wine
Permeate
Retentate
Permeate = Filtered Wine
= Filtered Wine
Cross Flow
IN
OUT
OUT
Cross Flow: Automation
.45 nm
Reverse Osmosis
Reverse Osmosis
Wine
Permeate
Retentate
Permeate = Filtered Wine
Reverse Osmosis
• Alcohol
• Volatile Acidity (+ Ion Exchange)
• 4-Ethylphenol/guaiacol ?
• Oxidative Aroma (Aldehydes) ?
• Reduced Aroma (Sulfides) ?
Removal
Cross Flow/Reverse Osmosis
• Product heating/churning ?
• Aroma loss ?
• Product loss ?
• Storage/inspection/cleaning ?
• Permeate use/DSP license ?
Questions:
Reverse Osmosis
pore size (nm)pore size (nm)smallestsmallest largestlargest
No absolute cut-off!
Ethyldecadienoate 196Oak Lactone 156Vanillin 1524-Ethylphenol 1222-Phenylethanol 122Methoxypyrazine 110Ethylacetate 88Diacetyl 86Molecular SO2 64Acetic acid 60 Ethanol 46CO2 44Water 18
MolecularWeights:
Reverse Osmosis
Osmotic Distillation
• Hollow Fiber Membrane
• 2 Liquid Phases: Wine vs. Water
• EtOH/CO2/SO2/H2S Evaporates Through Membrane
• @ Room Temperature and Low Pressure
www.liqui-cel.com
Filterability Testing
• How many pads/cartridges do we need?
• Will it go through the membrane?
• How much wine can we filter?
• Can we keep up with the bottling line?
• When can we go home?
Suggested reading: www.winerysolutions.com/filter.html
enology.butzke.com