Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY

Transcription

1 Dr. Christian E. BUTZKE Enology Professor PURDUE UNIVERSITY (765)

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

4 10 nm 100 nm 1 µm 10 µm

5 Particle Size 10 nm 10 µm 1 µm 100 nm

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

7 Personal Philtration Preferences

8 Preferences Parker Dr. Dave Laube Kramer

9 EK K100 K900 Pad Filtration.3 µm 1 µm 9 µm

10 Particle Size 10 nm 10 µm.45 µm.2 µm 1 µm 100 nm

11 Pad Filtration

12 Oxygen Pick-up?

13 Pad Filtration

14 Pad Filtration

15 Pad Sanitation w/out counter pressure!

16 Pad Sanitation With counter pressure!

17 Filter Gauges & Sanitation

18 Proper Cork Storage

19 Proper (TCA-free) Storage

20 Pore Seize vs. Flow Rate

21 Modular Depth Filters Stacked disks

22 Modular Depth Filters Cartridge packs

23 EK Pre-filter plus Membrane

24 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

25 Diatomaceous Earth DE Layers

26 Diatomaceous Earth

27 Diatomaceous Earth

28 DE/Rotary Drum Vacuum Filter

29 Membrane Filtration 0.45µm

30 Particle Size 10 nm 10 µm.45 µm.2 µm 1 µm 100 nm

31 Pad/DE vs. Membrane Depth Surface

32 Membrane Filtration Electron Microscope Image by Bill Clarkson University

33 Membrane Filtration Electron Microscope Image by Bill Clarkson University

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

35 Membrane Filtration Setup

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

37 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

38 Integrity Tests Bubble Point Forward Flow Pressure Hold

39 Membrane Filtration Bubble Point Integrity Test Liquid Gas

40 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

41 Membrane Pore Sizes.45 µm Nominal Pore Size Bubble Point smallest pore size (µm)( largest

42 Mannoproteins

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

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

45 Always do your Bubble Test!

46 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

47 Fouling

48 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.)

49 Cross Flow

50 Cross Flow

51 Cross Flow

52 Cross Flow Permeate = Filtered Wine Wine Retentate Permeate = Filtered Wine

53 Cross Flow OUT IN OUT

54 Cross Flow: Automation

55 .45 nm Reverse Osmosis

56 Reverse Osmosis Permeate Wine Retentate Permeate = Filtered Wine

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

58 Cross Flow/Reverse Osmosis Questions: Product heating/churning? Aroma loss? Product loss? Storage/inspection/cleaning? Permeate use/dsp license?

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

60 Reverse Osmosis Molecular Weights: Ethyldecadienoate 196 Oak Lactone 156 Vanillin Ethylphenol Phenylethanol 122 Methoxypyrazine 110 Ethylacetate 88 Diacetyl 86 Molecular SO 2 64 Acetic acid 60 Ethanol 46 CO 2 44 Water 18

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

62 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:

63 enology.butzke.com

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