1. WHITE WINE CLARIFICATION BY A NEW HYBRID PROCESS
Ph.D. Student: Fernando Salazar G.
Supervisor: Dr. Francisco López
February 3th, 2005, Tarragona, Spain

2. Preliminary Conclusions
CONTENT
Introduction
Objectives
Materials & Methods
Preliminary Results
Preliminary Conclusions
DEA Project: White wine clarification by a new hybrid process
2/20

3. STERILIZATION FILTRATION
INTRODUCTION
WHITE WINE MAKING
CRUSH
PRESS
CLARIFICATION
RAW MATERIAL
FERMENTATION
SETTLING
CLARIFICATION
STABILIZATION
IN THIS POINT IS FOCUS OUR RESEARCH
AGING
STERILIZATION FILTRATION
PAUSTERIZATION
WINE INDUSTRY
Proteins and polysaccharides, the colloidal fraction of wine, have a considerable influence on the basic operation carried out during winemaking (e.g clarification, filtration and cold stabilization)
BOTTLED
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4. CLARIFICATION TECHNIQUES
Settling
Centrifugation
Filtration
Cross-flow microfiltration
DEA Project: White wine clarification by a new hybrid process
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5. Fig.1 Configuration cross-flow microfiltration and fouling phenomena
CROSS-FLOW CONFIGURATION
Pressure
Concentrate
Feed
Pore blocking
Cake
Polarization concentration
Internal adsorption
Membrane
Permeate
Fig.1 Configuration cross-flow microfiltration and fouling phenomena
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6. CROSS-FLOW MICROFILTRATION
PROBLEMS
Flux decline during the microfiltration process due to fouling on the membrane
DEA Project: White wine clarification by a new hybrid process
6/20

7. HOW TO SOLVE THE PROBLEM?
Using Bentonite followed by microfiltration
Retentate
Permeate
Microfiltration
Feed
Addition bentonite
Applying a new hybrid process using zirconium oxide as adsorbent material: continuous process
Retentate
Permeate
Packed column
Hybrid process batch (used actually)
Hybrid process using the packed column as a filter (continuous process)
Feed
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8. OBJECTIVE
The main goal of this work is to increase the yield of the white wine cross-flow microfiltration using a new hybrid process
DEA Project: White wine clarification by a new hybrid process
8/20

9. SUB-OBJECTIVES
To design a new hybrid process using a packed column with zirconium oxide and cross-flow microfiltration.
To evaluate the yield of the cross-flow microfiltration with or without previous adsorption process.
To evaluate the effect of the proteins and polyphenols content on the permeate flux.
To evaluate the wine protein stabilization considering the cross-flow microfiltration and the new hybrid process.
DEA Project: White wine clarification by a new hybrid process
9/20

10. MATERIALS & METHODS Pinot Noir Sauvignon Blanc Chardonnay Malvasia
WHITE WINE SAMPLES
Pinot Noir
Sauvignon Blanc
Chardonnay
Malvasia
These samples were obtained from Mas dels Frares Winery, harvests 2003 and Tarragona, Spain.
DEA Project: White wine clarification by a new hybrid process
10/20

11. MATERIALS & METHODS CROSS-FLOW MICROFILTRATION Operation conditions:3 7 6 2 8 10 14 1 4 5 12 9 13 11
1. FEED
2. PUMP
3. TRANSMEMBRANE PRESSURE (MANOMETER)
4. VALVULE
5. VALVULE
6. PURGE
7. INPUT PRESSURE (MANOMETER)
8. TUBULAR MODULE MEMBRANE
9. PERMEATE STREAM
10. DIGITAL BALANCE
11. DATA ACQUISITION SYSTEM
12. OUTPUT PRESSURE (MANOMETER)
13. VALVULE
14. RETENTATE STREAM
Operation conditions:
Tubular module membrane: ceramic ZrO2, length 25 cm, area m2, pore size 0.2 mm
Transmembrane pressure: 1.5 bar
Cross-flow velocity: 2
Volumetric flow rate retentate: 3.7
Room temperature 25 ºC
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12. MATERIALS & METHODS ADSORPTION WITH ZIRCONIUM OXIDE IN PACKED COLUMN3 2
Packed column 4
White wine without treatment previous
White wine after of the adsorption 1
1. FEED
2. PERISTALTIC PUMP
3. ZIRCONIUM PACKED COLUMN
4. WHITE AFTER OF THE ADSORPTION WITH ZIRCONIUM OXIDE
Peristaltic pump
Operation conditions:
Zirconium oxide pellet
The packed column is of 19 cm high and internal diameter of 5.1 cm, g of ZrO2
The wine is pumped up-flow mode by a Watson Marlow 101 U/R peristaltic pump at a constant volumetric flow rate of 2 ml/min (1 h of residence time ).
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13. MATERIALS & METHODS PROTEIN ANALYSIS TOTAL PROTEIN Bradford’s Method
PROTEIN FRACTIONS
HPLC
Molecular Weight (MW)
Proteins standards:
Bovine serum albumin (BSA)
Ovalbumin (OV)
Lysozyme (LY)
PROTEIN HEAT STABILITY TEST
2 h at 80ºC and after for 2 h at 4ºC
Nephelometric turbidity units (NTU)
DEA Project: White wine clarification by a new hybrid process
13/20

14. MATERIALS & METHODS POLYPHENOLS ANALYSIS TOTAL POLYPHENOLS
Folin’s Method
POLYPHENOLIC PROFILE
HPLC
Polyphenols standards:
Gallic acid
Benzoic acid
Furfural acid, etc.
DEA Project: White wine clarification by a new hybrid process
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15. MATERIALS & METHODS PHYSICOCHEMICAL PROPERTIES pH Ash, g/L
Total acidity, g/L tartaric acid
Volatile acidity, g/L acetic acid
Fixed acidity, g/L tartaric acid
Sugar reducer, g/L
Volumetric alcoholic degree, %vol
Total dry extract, g/L
Ash, g/L
Chloride, g/L NaCl
Sulphates, g/L K2SO4
Chromatic characteristics (absorbance at 420, 520 and 620nm)
DEA Project: White wine clarification by a new hybrid process
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16. PRELIMINARY RESULTS THE PERMEATE FLUX
The permeate flux increased a 13 % using the new hybrid process.
Fig.2 Pinot Noir wine microfiltration with and without adsorption process
DEA Project: White wine clarification by a new hybrid process
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17. PRELIMINARY RESULTS The protein and polyphenols content or both? PNWT
PNB
PNC
PNBC
Pinot Noir Without treatment
Bentonite 2 g/l
Activated carbon 10 m/l
Bentonite 2 g/l and Activated Carbon 10 ml/l
DEA Project: White wine clarification by a new hybrid process
17/20

18. PRELIMINARY RESULTS The protein content Wine protein stabilisation
The polyphenol content
PNWT: wine without treatment
PNAA: wine after adsorption process
PNAHP: wine after hybrid process
PNAM: wine after microfiltration
PNB: wine after bentonite treatment
PNC: wine after activated carbon treatment
PNBC: wine after bentonite&carbon treatment
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19. PRELIMINARY RESULTS PERMEATE FLUX
Moreover to decrease the amount of proteins and polyphenols increasing the permeate flux.
Fig.3 Permeate flux of Pinot Noir wine during the microfiltration process considering the bentonite&active carbon treatment
DEA Project: White wine clarification by a new hybrid process
19/20

20. PRELIMINARY RESULTS PERMEATE FLUX
The proteins content has the highest effect on the permeate flux decline
Fig.4 Permeate flux of Pinot Noir wine during the microfiltration process considering different treatments
DEA Project: White wine clarification by a new hybrid process
19/20

21. PRELIMINARY CONCLUSIONS
Necessary to increase the residence time during the adsorption process.
According to preliminary results of Pinot Noir, the hybrid process allowed to increase the permeate flux during the microfiltration process.
Necessary to use another adsorbent material more selective with the total polyphenols.
Very important to know the behaviour of the other wines and the results by HPLC
DEA Project: White wine clarification by a new hybrid process
20/20

22. Thanks for your attention!!
Any questions?
DEA Project: White wine clarification by a new hybrid process