Managing Oxygen for Wine
Composition and Stability
EXAMINATION OF THE
BOTTLING PROCESS AND ITS
EFFECT ON TOTAL PACKAGE
OXYGEN
Hend Letaief, PhD
Davis, May 13, 2016
OUTLINE
•Why should we care?
•Bottling audits
•Initial DO, tank blanketing and transfer
•Filling
•Corking/capping
•Conclusion
2
OXYGEN AND WINE FAULTS
Data of the international wine challenge of London
(Good and Harrop, 2008)
3
1
BOTTLING AND OXYGEN UPTAKE
Oxygen uptake during various winemaking operations (mg/L)
Friedel, 2007
4
THERE ARE SEVERAL AREAS OF CONCERN FOR
EXCESS OXYGEN PICKUP DURING BOTTLING
5
IS IT POSSIBLE TO SUCCESSFULLY MANAGE OXYGEN
AT BOTTLING?
YES!!
Knowing the impact of
bottling on oxygen levels
in wine and wine quality
Controlling the factors
affecting oxygen solubility
and consumption
6
2
HOW?
Mesure your DO and HSO!
White wine DO<0.5 mg/L
Red wine DO<1 mg/L
Mesure and adjust your pH and SO2
4 mg of SO2 removes 1 mg of oxygen
ph<3.4
Molecular [SO2] >0.15 mg/L
7
HOW?
Check other parameters
Acetaldehyde on finished wine <10mg/L
[Cu] <0.2 mg/L
[Fe] <5 mg/L
Catechins<40 mg/L
Light
Temperature <15oC
Use stabilizers
ENARTIS TAN SLI
ENARTIS STAB SLI
CLARIL SLI-HM
8
OUTLINE
•Why should we care?
•Bottling audits
•Initial DO, tank blanketing and transfer
•Filling
•Corking/capping
•Conclusion
9
3
BOTTLING AUDITS
9 red wines
8 white wines
17 wineries from
California
Different closures
Natural cork
Nomacorc
synthetic
agglomerated
cork
Screwcap
5,000 gallons per year
 120,000 gallons per
year
10
FACTORS EXAMINED
Inerting the
tank and inline
Filling
technology
Use of inert gas
before and
after filling
hose length and
diameter
Use of vacuum
at corking
Tank volume
525
Gallons bottled
27,000
8
22
#Filler spouts
Speed Bot/min
550
100
11
SAMPLING FOR DO AND TPO
NomaSense O2 P300
n= 3 bottles
HSO
DO throughout the run
+
DO
=
TPO
n= # filling spouts
TPO in the middle of the run
12
4
TPO VARIATION MID-BOTTLING PROCESS
13
TPO VARIATION MID-BOTTLING PROCESS
7 audits failed to achieve TPO
levels < 1.5 mg/L
14
OUTLINE
•Why should we care?
•Bottling audits
•Initial DO, U-curve, tank blanketing and
transfer
•Filling
•Corking/capping
•Conclusion
15
5
IMPORTANCE OF REDUCING INITIAL DO AND
U-CURVE EFFECT
U-curve throughout the bottling process (n=3)
Initial DO> 1.5 mg/L
16
GOOD PRACTICES TO REDUCE THE U-CURVE
EFFECT (DO<0.5 MG/L)
Audit 11
Audit 7
Audit 4
Speed (bot/min)
176
375
150
Hose length (m)
24.5
82
46
Vacuum
Vacuum
Vacuum
Filling technology
Inerting HS in tank
N2
N2
N2
Use wine for priming
yes
yes
yes
Inert gas before the process
N2
N2
N2
Inert gas at the end of process
N2
No
N2
Whenever a wine is moved it should be protected
with inert gas
Also sparging the hoses with gas and wine during pumping could be beneficial
17
THE POTENTIAL FOR A HIGHER DO DECREASES WITH THE USE
OF INERT GAS IN THE BOTTLING TANK
18
6
FACTORS AFFECTING THE EFFICIENCY OF
SPARGING WITH INERT GAS: HENRY’S LAW
Acceptable Porosity:
Diameter 0.03 mm
Type of
gas
(density)
Inert gas
bubble size
Temperature
of the wine
Flow rates
of gas
Gas
pressure
Contact time
between the
gas and
wine
19
BLANKETING: THE KEY TO ECONOMICAL GAS
USAGE IS LAMINAR DELIVERY
Reynolds number
Re <2000
µ = Viscosity of the fluid,
V = Flow velocity,
D = Pipe diameter or length,
ρ= Density of the fluid.
Re >4000
20
ARGON BLANKETING: TURBULENT VS LAMINAR FLOW
Turbulent
flow
Laminar
flow
Data provided by C. Smith Vinovation Inc
21
7
% Oxygen at top of vessel
ARGON BLANKETING: A 2” LINE WITH A TEE AT THE
EXIT IS REQUIRED FOR ACCEPTABLE LAMINARITY
Argon Delivery @ 200 SCFH
100
90
80
70
60
50
40
30
20
10
0
1/4-inch hose
1.5-inch hose
2-inch hose w Tee
0
1
2
3
Headspace Volumes Delivered
4
Data provided by C. Smith, Vinovation Inc
22
CO 2 BLANKETING: EXAMPLE OF USE
3 to 7 volumes of CO2 at 20°C
Pressure: 1-2 bars
Flow rate: 0.1 - 0.3 L per L of wine
Time: 20min
Dharmadhikari, 1992
23
WINE TRANSFER: REDUCE TURBULENCE
FOR LOWER IMPACT ON DO
Reynolds number
µ = Viscosity of the fluid,
V = Flow velocity,
D = Pipe diameter or length,
ρ= Density of the fluid.
Frequent pumping,
centrifugal pump, high
transfer rate may dissolve
more oxygen
24
8
WINE TRANSFER CAN BE LESS IMPORTANT THAN
INITIAL DO OR HSO
The lowest and highest TPO Audits
Longer hoses do not always lead to higher TPOs
Slow bottling lines with frequent interruptions can
lead to higher TPOs
25
OUTLINE
•Why should we care?
•Bottling audits
•Initial DO, U-curve, tank blanketing and
transfer
•Filling
•Corking/capping
•Conclusion
26
DIFFERENT FILLING SYSTEMS AFFECT DO
AND HSO
Empty bottle=225 mg of O2  DO can increase by 0.3-0.7 mg/L
27
9
DIFFERENT FILLING SYSTEMS HAVE DIFFERENT
EFFECTS ON O 2 UPTAKE
Filling system
Vacuum filler, -40 mbar
O2
increase
(mg/L)
Turbulence
1.3
Pressure
Normal pressure filler, short tube
2
Normal pressure filler, long tube
0.5
Pressure filler, 1.5 bar (air, short tube)
3
Pressure filler, 1.5 bar (evacuation of
bottle and filling height correction with
CO2, short tube)
<0.5
Vacuum
Inert gas
McClellan, 1992
28
FILLING AFFECTS BOTTLE-TO-BOTTLE VARIATION
4 audits with Considerable
bottle-to-bottle variation
29
THE KEY COMPONENT REGARDING FILLING
RELATE PRIMARILY TO TURBULENCE
Cases where vacuum and Inert gas did not reduce bottle-to-bottle variations
Winery 17
Winery 5
Winery 13
128 bot/min
80 bot/min
500-600 bot/min
Screwcap
Natural cork
Nomacorc
32 spouts
24 spouts
80 spouts
Filling: vacuum
Filling and corking: vacuum
Filling: gravity
N2: Inerting bottles
N2: Inerting bottles
 Proper maintenance of
filler spouts
30
10
INERTING BEFORE FILLING GENERALLY REDUCES
OXYGEN UPTAKE (UP TO 0.5 PPM)
Recommended volume of gas: 7-8 times volume of bottle
Data provided by Nomacorc
31
OUTLINE
•Why should we care?
•Bottling audits
•Initial DO, U-curve, tank blanketing and
transfer
•Filling
•Corking/capping
•Conclusion
32
CLOSURE EFFECT ON HSO
Screwcap
Agglomerated cork
2.5
Natural cork
HSO mg/L
2
1.5
Nomacorc
1
0.5
0
A8
A1
A3
A5
A9 A10 A11 A16 A18 A6
A7 A12 A13 A15 A2
A4 A14 A17
Audit Number
33
11
COMPENSATE FOR TEMPERATURE DIFFERENCES
TO MAINTAIN PRESSURE ≤0.1 BAR (2 PSI) AT 68OF
Leakage, oxidation, spoilage
Adjust vacuum
Vacuum in HS should
be maintained between
300 mbar (-4.35 psi)
and 300 mbar.
Not possible with
screwcap
Adjust fill level
Cork: 10-15 mm ± 0.55 mm
for every degree F ± 68o F
Screwcap: 20 to 30 mm
34
VACUUM REDUCES PRESSURE BUT MORE EFFICIENT
WITH INERT GAS
No Vacuum
400.000
Pick-up = 3ppm
300.000
Oxygène dégarni (hPa)
HSO in hPa
350.000
250.000
Vacuum:
Pick-up= 1.4 ppm
Vacuum + CO2
200.000
Pick-up = 0.2 ppm
150.000
100.000
50.000
0.000
Data provided by Nomacorc
35
N2 and CO2 are the gases of choice before
and after filling
CO2 less pressure than N2 but can lead to reduction or
« spriz » reduce doses: Cork (1-1.2 mg/L); SC (0.6-0.7 mg/L)
Argon increases pressure when
wine temperature increases
Pressure
36
12
APPLYING INERT GAS WITH SCREWCAP
Interchange can occur
between the gas inside
the empty cap and that
in the HS
Liquid nitrogen
dosing is preferred
Gas purging is never
100% efficient
Cryogenic liquid (-320oF)
vaporizes due to
temperature change
No turbulence and no
air mixing!
37
ALLOW LIQUID N2 TO FULLY EVAPORATE BEFORE THE
CAP IS SEALED TO AVOID PRESSURE BUILDUP IN THE
BOTTLE!
Wine temperature
Pressure
Wine volume can increase of
0.166mL per degree Fahrenheit
Dose-droplet size
One part of liquid nitrogen
turns into 700 parts of gas
38
Gaseous nitrogen volume per
bottle (ml)
DIFFERENT DROPLET (NOZZLE) SIZES LEAD TO
DIFFERENT LIQUID TO GAS VOLUMETRIC RATIOS
175
160
145
130
115
100
85
70
55
40
25
0.03
.04" Nozzle
.05" Nozzle
.06" Nozzle
0.08
0.13
0.18
LN2 Dose Volume Per Bottle (mL)
Data provided by CHART Industries
0.23
39
13
IMPORTANT FACTORS WHEN DOSING
LIQUID NITROGEN
Dose Duration (mSec)
Common Data
Nozzle Size (inch
0.04; 0.05; 0.06
diam)
Line Speed (bpm)
50 to 150
Dose Duration (mSec)
30 to 60
.04" Nozzle
65
60
0.080
55
0.074
50
45
40
35
30
0.098
25
0.035
Data provided by CHART Industries
0.086
0.074
0.085
0.202
0.123
0.183
0.110
0.054
0.047
.06" Nozzle
0.220
0.135
0.067
0.060
0.040
.05" Nozzle
0.147
0.165
0.147
0.128
0.110
0.135
0.185
0.235
LN2 Dose Volume per Bottle (mL)
40
OUTLINE
•Why should we care?
•Bottling audits
•Initial DO, U-curve, tank blanketing and
transfer
•Filling
•Corking/capping
•Conclusion
41
BEST PRACTICES TO REDUCE TPO
Start with a low DO (good pH, SO2, stabilizer..)
Proper purging of inert gas in the tank and during wine transfer
Reduce turbulence
Reduce maintenance interruptions
Optimize conditions to closure/bottle combination: speed, fill height,
pressure, vacuum
Injection of nitrogen in the headspace of the bottle or liquid dosing for
screwcaps
MORE??
Hend Letaief, Key points of the bottling process. Study at 17
wineries identifies impacts on total package oxygen. PRACTICAL
WINERY AND VNEYARD JOURNAL, MAY 2016.
42
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ACKNOWLEDGMENTS
This work was funded by Nomacorc
Supported by the California wine industry
Bertille Goyard from AgroSup Dijon
Pauline Martinaggi from ESA Angers
The Wine Science Forum advisory board
Ashley Heisey, winemaker and wine consultant
43
Thank you!
[email protected]
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