Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm...

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Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY [email protected] (765) 49-46500 www.butzke.com

Transcript of Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm...

Page 1: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Dr. Christian E. BUTZKEEnology Professor

PURDUE UNIVERSITY

[email protected] (765) 49-46500 www.butzke.com

Page 2: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size
Page 3: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

• Filtrosophy

• Filtration Systems• Pad/Cartridge/DE

• Membrane

• Cross Flow• Particle Filtration

• Reverse Osmosis

• Filterability Testing

Page 4: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

1 µm 10 µm100 nm10 nm

Page 5: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

10 µm10 µm

1 µm1 µm 100 nm100 nm

10 nm10 nmParticle Size

Page 6: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

• No Un-Filtration

• No Routine Filtration

How to Unfilter?

Page 7: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Personal Philtration Preferences

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Preferences

Parker

Laube

Dr. Dave

Kramer

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1 µm

K100

.3 µm

EK

9 µm

K900

Pad Filtration

Page 10: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

10 µm10 µm

1 µm1 µm 100 nm100 nm

10 nm10 nm

.45 µm.45 µm .2 µm.2 µm

Particle Size

Page 11: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Pad Filtration

Page 12: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Oxygen Pick-up ?

Page 13: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Pad Filtration

Page 14: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Pad Filtration

Page 15: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Pad Sanitation

w/out counter pressure!

Page 16: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

With counter pressure!

Pad Sanitation

Page 17: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Filter Gauges & Sanitation

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Proper Cork Storage

Page 19: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Proper (TCA-free) Storage

Page 20: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Pore Seize vs. Flow Rate

Page 21: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Modular Depth Filters

Stacked disks

Page 22: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Modular Depth Filters

Cartridge packs

Page 23: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

EK Pre-filter plus Membrane

Page 24: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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“

Page 25: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Diatomaceous Earth

DE LayersDE Layers

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Diatomaceous Earth

http://www.filtrox.ch

Page 27: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Diatomaceous Earth

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DE/Rotary Drum Vacuum Filter

Page 29: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

0.45µmMembrane Filtration

Page 30: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

10 µm10 µm

1 µm1 µm 100 nm100 nm

10 nm10 nm

.45 µm.45 µm .2 µm.2 µm

Particle Size

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Pad/DE vs. MembraneDepth Surface

Page 32: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Electron Microscope Image by Bill Plunkett @ Clarkson University

Membrane Filtration

Page 33: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Membrane Filtration

Electron Microscope Image by Bill Plunkett @ Clarkson University

Page 34: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Membrane Filtration

• Surface Filtration

• Perpendicular

• Removal of Microbes

• “0.2 - 1.2”µm Pores

• Integrity Tests

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Membrane Filtration Setup

Page 36: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Sterile Filtration

1. Cellulose2. Membrane 1.20 µm3. Membrane 0.45 µm4. Cellulose

1.2.3.4.

Depth

Surface

perpendicular

Page 37: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

• 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”

Page 38: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Integrity Tests

• Bubble Point

• Forward Flow

• Pressure Hold

Page 39: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Membrane Filtration

Bubble Point Integrity Test

LiquidLiquid

GasGas

Page 40: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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"

Page 41: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Membrane Pore Sizes

BubbleBubblePointPoint

pore size (pore size (µµm)m)smallestsmallest largestlargest

“.45 µm Nominal Pore Size”

Page 42: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

http://www.lallemand.com

Mannoproteins

Page 43: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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

Page 44: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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”

Page 45: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Always do your Bubble

Test !

Always do your Bubble

Test !

Page 46: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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

Page 47: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Fouling

Page 48: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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 ”

Page 49: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Cross Flow

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Cross Flow

Page 51: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Cross Flow

Page 52: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Cross Flow

Wine

Permeate

Retentate

Permeate = Filtered Wine

= Filtered Wine

Page 53: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Cross Flow

IN

OUT

OUT

Page 54: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Cross Flow: Automation

Page 55: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

.45 nm

Reverse Osmosis

Page 56: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Reverse Osmosis

Wine

Permeate

Retentate

Permeate = Filtered Wine

Page 57: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Reverse Osmosis

• Alcohol

• Volatile Acidity (+ Ion Exchange)

• 4-Ethylphenol/guaiacol ?

• Oxidative Aroma (Aldehydes) ?

• Reduced Aroma (Sulfides) ?

Removal

Page 58: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Cross Flow/Reverse Osmosis

• Product heating/churning ?

• Aroma loss ?

• Product loss ?

• Storage/inspection/cleaning ?

• Permeate use/DSP license ?

Questions:

Page 59: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Reverse Osmosis

pore size (nm)pore size (nm)smallestsmallest largestlargest

No absolute cut-off!

Page 60: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

Ethyldecadienoate 196Oak Lactone 156Vanillin 1524-Ethylphenol 1222-Phenylethanol 122Methoxypyrazine 110Ethylacetate 88Diacetyl 86Molecular SO2 64Acetic acid 60 Ethanol 46CO2 44Water 18

MolecularWeights:

Reverse Osmosis

Page 61: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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

Page 62: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

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

Page 63: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size

enology.butzke.com

Page 64: Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY · 10 µm10 µm 1 µm1 µm 100 nm100 nm 10 nm10 nm.45 µm.45 µm .2 µm.2 µm Particle Size