Dr. Christian E. BUTZKE Enology Professor Indiana Wine Grape Council. (765) FS Room

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1 Dr. Christian E. BUTZKE Enology Professor Indiana Wine Grape Council (765) FS Room

2 Filtrosophy Filtration Systems Pad/DE Membrane Cross Flow Particle Filtration Reverse Osmosis Filterability Testing

3

4 How to Unfilter? No Un-Filtration No Routine Filtration

5 Personal Philtration Preference

6 Pad Filtration

7 Oxygen Pick-up?

8 Pad Filtration

9 Pad Filtration

10 Pad Sanitation W/out counter pressure!

11 Pad Sanitation With counter pressure!

12 Filter Gauges & Sanitation

13 Proper Cork Storage

14 Proper (TCA-free) Storage

15 EK Prefilter plus Membrane

16 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

17 Diatomaceous Earth DE Layers

18 Diatomaceous Earth

19 Diatomaceous Earth

20 DE/Rotary Drum Vacuum Filter

21 0.45µm

22 Pad/DE vs. Membrane Depth Surface

23 Membrane Filtration Electron Microscope Image by Bill Clarkson University

24 Membrane Filtration Electron Microscope Image by Bill Clarkson University

25 Membrane Filtration Surface Filtration Perpendicular Removal of Microbes µm Pores Integrity Tests

26 Sterile Filtration 1. Cellulose 2. Membrane 1.20 µm 3. Membrane 0.45 µm 4. Cellulose perpendicular Depth Surface

27 Mount Integrity Test Sterilize Bottle Re-Test Membrane Filtration Bubble Point flood membrane with water pressurize to 80% with N 2 gas increase pressure by 2 psi/min note pressure when bubbling starts compare to filter specifications

28 Integrity Tests Bubble Point Forward Flow Pressure Hold

29 Membrane Filtration Bubble Point Integrity Test Liquid Gas

30 Bubble Point Integrity Test Bubble Release largest pore diameter pressure differential surface tension (Water vs. Wine!) "steady stream of bubbles" Result: membrane integrity correct filter size correct mounting Note: 4 to 6 psi variation NOT tested: sterility downstream

31 Membrane Pore Sizes Bubble Point smallest pore size (µm)( largest

32 Mannoprotein

33 Pore vs. Protein Size 0.45 µm 0.13 Mannoprotein Size: µm ( kda) Pore Size Sterile Filter: µm

34 Shriveled Bacteria? 0.45 O.oeni O.oeni Oenococus oeni: 1.0 µm Pore Size Sterile Filter: 0.45 µm viable but non-culturable

35 Always do your Bubble Test!

36 Sources of Re-Contamination Hoses, Lines, Gauges Valves Gaskets Bottles Rinse Water Filler Bowl Inert Gas Vacuum Line Corks Filtered Air Hopper Vacuum Line Corker Jaws Conveyors Condensate Filler Heads Winemaker Millipore Corp. in PW&V 1989

37 Fouling

38 Filter Fouling undesirable accumulation of materials on the surface of the filter Yeast/Bacteria Cells (alive or dead) Biofilm Formation (Polysaccharides) Colloidal Materials (Pectine, Protein etc.) Fining Agent Residue (Bentonite etc.)

39 Cross Flow Permeate = Filtered Wine Wine Retentate Permeate = Filtered Wine

40 Cross Flow

41 Cross Flow

42 Cross Flow OUT IN OUT

43 Cross Flow

44 Cross Flow

45 0.45nm

46 Reverse Osmosis Permeate Wine Retentate Permeate = Filtered Wine

47 Reverse Osmosis Removal Alcohol Volatile Acidity (+ Ion Exchange) 4-Ethylphenol/guaiacol? Oxidative Aroma (Aldehydes)? Reduced Aroma (Sulfides)?

48 Cross Flow/Reverse Osmosis Issues Product heating/churning Aroma loss Product loss Storage/inspection/cleaning Permeate use/dsp license

49 Reverse Osmosis No absolute cut-off! smallest pore size (nm) largest

50 Reverse Osmosis Molecular Weights: Ethyldecadienoate 196 Oak Lactone 156 Vanillin Ethylphenol Phenylethanol 122 Methoxypyrazine 110 Ethylacetate 88 Molecular SO 2 64 Acetic acid 60 Ethanol 46 CO 2 44 Water 18

51 Osmotic Distillation Microporous Hollow Fiber Membrane 2 Liquid Phases: Wine vs. Water EtOH/CO 2 /SO 2 /H 2 S Evaporates Through Membrane Room Temperature and Low Pressure

52 Filterability Testing How many pads do we need? Will it go through the membrane? How much wine can we filter? Can we keep up with the bottling line? How long will it take? Suggested reading:

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