2017 pwgt spring workshop - purdue university
TRANSCRIPT
Christian BUTZKEProfessor of Enology
Purdue Wine Grape Team
2017 PWGT Spring Workshop
• Filtrosophy
• Filtration Systems• Pad/Cartridge/DE • Membrane
• Cross Flow• Particle Filtration • Reverse Osmosis
• Filterability Testing
1 µm 10 µm100 nm10 nm
10 µm
1 µm 100 nm
10 nmParticle Size
• No Un-Filtration
• No Routine Filtration
How to Unfilter?
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
Personal Philtration Philosophy
Home Depot-style Filtration
1 µm
K100
.3 µm
EK
9 µm
K900
Pad Filtration
10 µm
1 µm 100 nm
10 nm
.45 µm .2 µm
Particle Size
Centrifuge
Pad Filtration
Small Scale Pad Filtration
Maxi Pad Filtration
Oxygen Pick-up @ Filtration
Pad Filtration Setup
Pad Filtration
Pad Sanitation
w/out counter pressure!
With counter pressure!
Pad Sanitation
Filter Gauges & Sanitation
Proper (TCA-free) Storage
PoreSeizes
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 Layers
Diatomaceous Earth
6’2”
Diatomaceous Earth
Diatomaceous Earth
http://www.filtrox.ch
Diatomaceous Earth
DE/Rotary Drum Vacuum Filter
0.45µmMembrane Filtration
10 µm
1 µm 100 nm
10 nm
.45 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 slowly• 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
Liquid
Gas
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"
Downstream Sterility ?
Membrane Pore Sizes
BubblePoint
pore size (µm)smallest largest
“.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 0.13
Shriveled Bacteria?
Oenococus oeni: 1.0 µmPore Size Sterile Filter: 0.45 µm
0.45
0.45
0.45
“viable but non-culturable”
Always do your Bubble
Test !
Pressure Hold 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: Automation
Cross Flow
• Clarifications: solids … bacteria
• Stop yeast fermentation to retain R.S.
• Stop malolactic fermentation ?
• Starting at ≈250 gal/hour for ≈$30k
Applications
http://www.winebusiness.com/wbm/?go=getArticle&dataId=43876
Shared Equipmentor Mobile Services ?
Cross Flow
Cross Flow
Cross Flow
Wine
Permeate
Retentate
Permeate = Filtered Wine
= Filtered Wine
Cross Flow
IN
OUT
OUT
Cross Flow/Reverse Osmosis
• Storage/inspection/cleaning ?
• Integrity testing ?
• Aroma/colloidal-mouthfeel loss ?
• Product heating/churning/ox ?
• Product loss ?
Questions to ask:
.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
Reverse Osmosis
pore size (nm)smallest largest
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/VA/SO2 Evaporates Through Membrane
• @ Room Temperature and Low Pressure
www.liqui-cel.com
