dr. christian e. butzke enology professor purdue university · 10 µm10 µm 1 µm1 µm 100 nm100 nm...

Dr. Christian E. BUTZKEEnology Professor

PURDUE UNIVERSITY

butzke@purdue.edu (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