2017 PWGT Spring Workshop. Christian BUTZKE Professor of Enology Purdue Wine Grape Team

Transcription

1 2017 PWGT Spring Workshop Christian BUTZKE Professor of Enology Purdue Wine Grape Team

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

3 10 nm 100 nm 1 µm 10 µm

4 Particle Size 10 nm 10 µm 1 µm 100 nm

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

6 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:

7 Personal Philtration Philosophy

8 Home Depot-style Filtration

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 Centrifuge

12 Pad Filtration

13 Small Scale Pad Filtration

14 Maxi Pad Filtration

15 Oxygen Filtration

16 Pad Filtration Setup

17 Pad Filtration

18 Pad Sanitation w/out counter pressure!

19 Pad Sanitation With counter pressure!

20 Filter Gauges & Sanitation

21 Proper (TCA-free) Storage

22 Pore Seizes

23 Pore Seize vs. Flow Rate

24 Modular Depth Filters Stacked disks

25 Modular Depth Filters Cartridge packs

26 EK Pre-filter plus Membrane

27 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

28 Diatomaceous Earth DE Layers

29 6 2 Diatomaceous Earth

30 Diatomaceous Earth

31 Diatomaceous Earth

32 Diatomaceous Earth

33 DE/Rotary Drum Vacuum Filter

34 Membrane Filtration 0.45µm

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

36 Pad/DE vs. Membrane Depth Surface

37 Membrane Filtration Electron Microscope Image by Bill Clarkson University

38 Membrane Filtration Electron Microscope Image by Bill Clarkson University

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

40 Membrane Filtration Setup

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

42 Mount Integrity Test Sterilize Bottle Re-Test Membrane Filtration Bubble Point Flood membrane with water Pressurize to 80% with N 2 gas Increase pressure slowly Note pressure when bubbling starts Compare to filter specifications

43 Integrity Tests Bubble Point Forward Flow Pressure Hold

44 Membrane Filtration Bubble Point Integrity Test Liquid Gas

45 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

46 Downstream Sterility?

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

48 Mannoproteins

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

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

51 Always do your Bubble Test!

52 Pressure Hold Test

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

54 Fouling

55 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.)

56 Cross Flow

57 Cross Flow: Automation

58 Cross Flow Applications Clarifications: solids bacteria Stop yeast fermentation to retain R.S. Stop malolactic fermentation? Starting at 250 gal/hour for $30k

59 Shared Equipment? or Mobile Services

60 Cross Flow

61 Cross Flow

62 Cross Flow Permeate = Filtered Wine Wine Retentate Permeate = Filtered Wine

63 Cross Flow OUT IN OUT

64 Cross Flow/Reverse Osmosis Questions to ask: Storage/inspection/cleaning? Integrity testing? Aroma/colloidal-mouthfeel loss? Product heating/churning/ox? Product loss?

65 .45 nm Reverse Osmosis

66 Reverse Osmosis Permeate Wine Retentate Permeate = Filtered Wine

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

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

69 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

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

71 Questions?